TWI352080B - Process and apparatus for manufacturing pure forms - Google Patents

Description

</ RTI> </ RTI> </ RTI> </ RTI> </ RTI> </ RTI> </ RTI> </ RTI> </ RTI> </ RTI> </ RTI> </ RTI> </ RTI> </ RTI> <RTIgt; The aromatic feed material is oxidized to an impure, crude product, and the aromatic carboxylic acid in an impure form is purified by treating the off-gas from the liquid phase oxidation reaction to recover the aqueous liquid, and using the aqueous liquid recovered from the oxidation reaction gas. To purify the impure aromatic carboxylic acid. BACKGROUND OF THE INVENTION Terephthalic acid and other aromatic carboxylic acids are widely used in the preparation of polyesters, usually by combining with ethylene glycol, high carbon alkylene glycol or combinations thereof. The components are converted into fibers, films, containers, bottles and other packaging materials and molded articles. In commercial practice, aromatic carboxylic acids are typically used in the presence of bromine-promoting catalysts containing cobalt and manganese, using air or another source of oxygen (which is typically gaseous oxygen) to be substituted with methyl groups in aqueous acetic acid solvents. A raw material of benzene and naphthalene wherein the position of the methyl substituent corresponds to a carboxyl group position of 20 in the desired aromatic carboxylic acid product, and is subjected to a liquid phase oxidation reaction. The oxidation reaction is exothermic and can produce aromatic carboxylic acids and by-products, including partial or intermediate oxidation products of the aromatic raw materials, and acetic acid reaction products such as methanol, methyl acetate, and bromine alkyl. Water is also produced as a by-product. The resulting aromatic carboxylic acid, which is typically produced with the oxidation by-products of the starting material, is typically dissolved or present in the liquid phase reaction mixture as a suspended solid, and is typically recovered by the separation of the crystals and solid-liquid separation techniques. The exothermic oxidation reaction is usually carried out at a suitable reaction volume (IV) at elevated temperature and pressure. The m-dimensional Wei phase reacts the mixture, and the gas phase formed by the exothermic oxidation is evaporated from the liquid phase and removed from the reactor to control the reaction temperature. The gas phase comprises water vapor, a vaporized acetic acid reaction solvent, oxygen not consumed in the oxidation reaction, gaseous by-products such as methanol, bromodecane and decyl acetate, carbon oxide and, when the oxygen source of the method is air or Another type of oxygen-containing gaseous mixture is the nitrogen, carbon oxide and other inert gaseous components of the source gas. In the manufacture of polyacetates for important applications such as fibers and bottles, it is generally preferred to use aromatic carboxylic acids in pure form, as impurities are known, such as those produced by aromatic protoplasts in the oxidation process. By-products, and more broadly, a variety of carbonyl-substituted aromatic species are known which can result in color formation of the polyester derived from the acid or in relation to its color formation, and subsequent discoloration of the product of the polyester conversion. . As is known from U.S. Patent Nos. 4,877,900, 4,772, 748, and 4,286,101, a small amount of impurities in the pure form of aromatic carboxylic acids can be obtained by: or - a plurality of progressively lower temperatures and Further oxidation at the oxygen level results from the crude product of the i-phase liquid phase oxidation reaction, and in order to convert the partial oxidation product of the feedstock to the desired acid product, the oxidation products are recovered during crystallization. Pure form of terephthalic acid and other aromatic carboxylic acids with lower impurity content, such as purified terephthalic acid or "PTA", are prepared by using precious metal catalysts in solution at elevated temperatures and pressures. Hydrogenating the acid in a low purity form, such as a crude product containing aromatic traconic acid and by-products produced by liquid phase oxidation of an aromatic starting material. In commercial practice, the liquid phase oxidation reaction of the alkyl aromatic feed material into a crude aromatic carboxylic acid and the purification of the crude product are usually carried out in a continuous integration process in which the crude product obtained from the liquid phase oxidation reaction It is used as a starting material for the purification reaction. The high temperature and high pressure gas phase produced by the liquid phase oxidation reaction in these processes are recoverable acetic acid reaction solvents, unreacted substances, reaction by-products and potential sources of energy; however, their high water content , high temperature and high pressure and technical and economic problems arising from the sequestration of components such as gaseous methyl bromide, acetic acid solvent and water for separating or recovering the components of the exhaust gas for recycling and recovering its energy content. Moreover, if the impurity S adversely affects other process aspects or product quality, even small amounts of impurities that have not been separated in the process stream can prevent reuse of the recycle stream. As described in U.S. Patent No. 5,200,557, for example, monocarboxylic acids adversely affect the hydrogenation catalyst used in the purification process, and even low levels of acetic acid residues such as those present in the crude aromatic traconic acid product recovered from the oxidation reaction liquid. Things are also considered harmful. British Patent Specification No. 1,373,230, U.S. Patent Nos. 5,3,4,676, 5,723,656, 6,143,925, 6,504,051, European Patent Specification 0 498 591 B1, and International Patent Application No. 97/27,168 A process for the preparation of aromatic tremologies, which is a liquid phase oxidation reaction of an aromatic feed from which high pressure waste gas is removed and treated to recover and recycle a portion or component thereof, And in some cases, energy is recovered. The water recovered from the high pressure oxidation reaction off-gas in these processes is then subjected to an oxidation reaction with the auto-condensed acetic acid&apos; to be recycled to the off-gas separation step for reflux or treatment in a liquid flush stream. According to the example of U.S. Patent No. 5,304,676, the oxidizing waste gas is condensed and then purified by steaming to wash the purified p-dicarboxylic acid precipitate, and according to the example of U.S. Patent No. 5,723 '656, The single-rebel acid and water vapor in the high-pressure oxidation waste are separated, and the high-pressure gas formed by the water vapor is subjected to catalytic oxidation reaction to be converted into water and carbon oxide to remove organic impurities, and the formed gas is expanded to recover energy. The treated water from the expansion and low-pressure gas condensation is used as a crystallization solvent for the purification of stearic acid. However, none of the methods such as Xuanxuan uses a liquid condensed from a high-pressure exhaust gas obtained from a liquid phase oxidation reaction as a solvent for purifying an impure aromatic acid or other aqueous liquid. Moreover, the recovery of materials and energy from the exhaust gases of such processes is usually carried out at the expense of each other, for example, if the materials are removed and the south temperature and high pressure gas phase formed by the oxidation reaction is not cooled or depressurized, Once cooled or depressurized (4) receiving material f, burning substances to control atmospheric emissions will lead to loss of energy content and other losses of oxidizing solvents, raw materials and intermediates. Impurities remaining in the recycle stream can disrupt process operations and damage to the product, such as reclaimed materials, energy, or both, and process steps that can further increase process complexity and limit or hinder its practical use. Because of the increased cost than the savings (4) and energy. The impact of lost energy and materials will increase depending on the scale of the process operation. In the world where the annual output of the product is 280 or higher, even the fractional or hundreds of ppm of raw materials and solvents: the unproductive or unstable by-products, the slight inefficiency of energy recovery and the rehydration The incremental feed of the treatment will result in a significant physical loss of the material, an increase in the consumption of fuel or electricity due to the difference in the cost and variation of the energy, the substance and the demand for the treatment of the gaseous and liquid effluent and the effluent. Unpredictable process efficiency and economics. Atmosphere content; J SUMMARY OF THE INVENTION The present invention provides a method and apparatus for preparing an aromatic carboxylic acid in a pure form, which can improve the time rate and recurrence of the substance and the energy recovery rate or both, and in more detail. The aqueous condensate can be recovered from the high pressure off-gas from the liquid phase oxidation reaction of the aromatic feed material for the purification of the aromatic carboxylic acid product from the liquid phase oxidation reaction or other aromatic form of the aromatic acid. These important features of the present invention are found in that the high pressure gas phase produced by the exhaust gas or overhead product in the liquid phase oxidation reaction in which the aromatic feed material is converted to the aromatic carboxylic acid can be treated to be in the liquid. The reaction solvent is largely removed in the material stream, and at the same time, the high-purity gas from the separation can be treated practically and efficiently under high pressure, which contains steam, and usually also contains - or a plurality of non-condensable components of the oxidation reaction waste gas, Unreacted aromatic feed and reaction by-products, with at least substantially solvent-free monocarboxylic acid 'to recover water and substantially no organic impurities derived from the oxidation reaction (such as a monocarboxylic acid solvent) and from oxidation The liquid of the reaction product of the reaction, and the liquid is suitable as a solvent for the method of purifying the impure aromatic carboxylic acid or other process liquid containing water, without additional treatment. The high-pressure gaseous overhead stream from the high-pressure gas phase separation into a rich solvent-based liquid phase-phase oxidation reaction and the high-pressure gas recovery condensate from the aqueous solution can be used in whole or in part to remove the demineralization or the known purification method. Other purified water sources. - a reaction raw material and a by-product obtained from a liquid phase oxidation reaction, which comprises the aromatic raw material substance and a by-product of the monocarboxylic acid used for the oxidation reaction, and can also be recovered according to an embodiment of the present invention. The high pressure gas phase derived from the liquid phase oxidation reaction also represents a source of recoverable energy, and the treatment of the gas phase according to embodiments of the present invention can recover energy from the pressurized gas therefrom or therefrom. Energy sources in the form of heat, work, or both can be recycled. In some such embodiments, in addition to providing a liquid suitable for purification, for example, as a solvent for use in purifying a reaction solution or in recovering a product of a pure form, or as a lotion or as a lotion In addition to the above-described advantages of the seal rinse liquid, and the other advantages described above, the present invention provides surprising flexibility to prepare a wide variety of aromatic carboxylic acids in pure form. In an integrated process for the preparation of aromatic carboxylic acids in pure form, which comprises oxidizing an aromatic feed material in a liquid phase reaction mixture to produce a crude product comprising an aromatic carboxylic acid and oxidation by-products of the feed material Purifying the crude product by hydrogenation of its solution in an aqueous liquid, the present invention can remove or reduce the need for water or pure water obtained from other sources, and can be obtained in a known method. The balance between the water produced in the liquid phase oxidation reaction and the water consumed in the purification can not be achieved, and the method of the present invention is substantially superior to the known method of δ Xuan. The high-pressure gas phase recovery from the liquid phase oxidation reaction of the aromatic feedstock to aromatic carboxylic acid and the aqueous liquid system for the purification reaction of the impure aromatic acid retardation according to the present invention The condensation of the gas is largely separated from the solvent in the high-pressure exhaust gas obtained by the liquid phase oxidation reaction, and the pressurized gas remaining after the water is recovered. Preferably, the uncondensed gas remains after the condensation. In a preferred embodiment of the invention, the liquid condensate containing aqueous and substantially solvent-free monodecanoic acid is indirectly heat exchanged by condensation of the pressurized gas to produce steam or other heated material suitable for use in other steps of the process. The heat is exchanged for recycling. The exhaust gas remaining after the condensation is subjected to pressure 'and the exhaust gas typically contains the non-coagable component of the oxidation reaction off-gas. It may also include a small amount of aromatic feed material and solvent by-products produced in the liquid phase oxidation reaction which can be converted to the high pressure oxidation overhead. Although it is generally subjected to a lower pressure than the liquid phase oxidation reaction off-gas, the condenser off-gas is subjected to high pressure and has a large energy content. Thus, in certain embodiments, the present invention recovers energy from pressurized condenser exhaust. Energy can be recovered in a combination of heat, work or a combination of them. In certain embodiments, the present invention can also be used to improve the recovery and reusability of monocarboxylic acid solvents for liquid phase oxidation reactions. In addition to the large amount of separation of the solvent-rich liquid from the oxidation reaction waste gas apparatus and the solvent-rich liquid is suitable for returning to the oxidation reaction or suitable for the oxidation reaction, the method of the invention comprises separating and purifying the aromatic compound from the purified reaction solution by refluxing. An example of a liquid containing a purified mother liquor remaining after the acid product. In such embodiments, not only deuterated by-products, such as carboxybenzaldehyde and sulfhydryl ruthenium oxide intermediates, which can be converted to the desired aromatic acid product to the dopicic acid or isophthalic acid, a solvent monocarboxylic acid, such as a solvent residue in the impure aromatic carboxylic acid product used to form the purification solution or a small amount of solvent remaining in the liquid condensate containing water condensed by the pressurized gas from the separation step, Return to the oxidation reaction. a solvent monocarboxylic acid, a reaction product thereof produced in a liquid phase oxidation reaction, an unreacted aromatic feed material derived from the oxidation reaction, or the presence of 1352080 in a high pressure gas phase derived from an oxidation reaction and continuously present in The recovery of the combination in which a large amount of the solvent monocarboxylic acid in the gas phase and the pressurized gas remaining after the water is separated can be further improved according to other examples, wherein the pressurized gas system is condensed to recover the aqueous liquid. The high pressure cold reactor exhaust gas is left to be cooled to one or more services: the gas agent is effective to remove one or more of the feed material, the solvent, and the temperature of the oxidation by-product of the solvent. The gas formed can be processed in steps to separate the feed material and/or such solvent by-products, and

In the case, the feed material, the solvent by-product or a combination thereof may be subjected to a liquid phase oxidation reaction. In one aspect, the invention provides a device for preparing an aromatic carboxylic acid. The device can improve the recovery rate of energy and avoid material loss during the manufacturing operation. In certain such embodiments, the construction of the apparatus may provide additional advantages by eliminating the corrosive nature of the lesser process gas stream, and thus the components of the apparatus and, in some cases, the components of the 'accessory or other process equipment may be With 15 suitable corrosion resistance metals and alloys such as stainless steel, steel 戍 double fine

Steelmaking (as a substitute for titanium), nickel alloy steel, and other more expensive high-resistance metals used in the manufacture of aromatic acid retardants. Briefly, 'the apparatus according to this aspect of the invention comprises a reaction vessel having an exhaust port for removing steam on top of the reaction vessel; a high pressure gaseous state containing an early 20 carboxylic acid and water separated by a stell. a C 8 monocarboxylic acid gas and water vapor in the mixture and circulated with the reaction vessel to receive t P removed from the reaction vessel

Separating device 'flowing with the separating device' is adapted to extract at least a portion of the high pressure gas from the AE 7 gorge and exchange heat with the heat sink material to extract the H primary condensing device from the high pressure gas; and to condense the high pressure gas from the Condensed, for,,,,

12

V 1352080 At least one container for purifying a member of an aromatic carboxylic acid. The preferred apparatus further includes an expander that can be circulated with the condensing unit. A preferred separation device comprises one or more high pressure distillation columns. The condenser is preferably adapted to condense as little as about 20% to about 60% to all or substantially all of the water present in the high pressure gas stream of the condenser 5 to be skinned. The condenser is optionally further adapted to return a portion of the condensate from the high pressure overhead gas stream to the separation unit. In more detail, the apparatus according to this aspect of the invention comprises a liquid phase reaction mixture suitable for a first pressure and adapted to maintain a liquid phase reaction mixture and produce a high pressure gas phase at a solvent comprising a monocarboxylic acid solvent and water. a reaction vessel for subjecting an aromatic feed material to a liquid phase oxidation reaction with gaseous oxygen, and comprising at least one vent for removing a high pressure gas phase from the reaction vessel; adapted to a second pressure, substantially not Less than the first pressure, and comprising at least one gas inlet that is circulated with the reactor to receive a high pressure gas phase removed from at least one vent of the reactor, at least one for delivering the reflux liquid to the apparatus a liquid inlet, at least one gas outlet for removing heated gas from the apparatus, at least one liquid outlet for removing a liquid stream from the apparatus, and disposed between the at least one gas inlet and the at least one gas outlet and Separating a large amount of solvent 20 monocarboxylic acid and water in the high pressure gas phase gas received in the apparatus, thereby forming a solvent-containing monocarboxylic acid and a substantially anhydrous liquid material stream a sub-saturated zone of a high-pressure gas containing water and a large amount of solvent mono-repulsive acid; containing at least one high-pressure gas removed from at least one gas outlet received from the heat exchange member of the separation device to extract high-pressure gas from the condensing device Transferring heat to the heat exchange fluid, thereby condensing the liquid condensate 13 from the high pressure gas and forming a gas inlet for the heat exchange fluid at a high temperature or a high pressure, at least one outlet for removing the high pressure exhaust gas from the condensing device, and At least one condensing device for removing the outlet of the condensate from the condensing device; and for guiding the condensate removed from the at least one outlet of the condensing device to at least one container of the aromatic acid purification device s installation. Such a device is preferably suitable for carrying out a purification process which comprises contacting a solution containing an aromatic carboxylic acid and an impurity dissolved in an aqueous liquid with hydrogen in the presence of a hydrogenation catalyst at a high temperature and a high pressure to form a purified liquid reaction mixture. And removing the solid aromatic carboxylic acid product having reduced impurities from the purified reaction mixture. A preferred apparatus for producing a purified aromatic carboxylic acid by this method comprises at least one reactor suitable for contacting a liquid purification reaction solution with hydrogen in the presence of a hydrogenation catalyst in the presence of a hydrogenation catalyst to form a purified liquid reaction mixture, preferably A product recovery vessel comprising at least one solid aromatic m acid product which can be circulated with the helium reactor to receive the purified liquid reaction mixture removed from the reactor and from which the reduced impurity content is recovered. Preferably, the apparatus further comprises _ or more, such as a filtration or other separation step for solid-purifying aromatic carboxylic acid from a liquid medium for desulfurization of a quasi-aliphatic aromatic acid buffer in a purification reaction solvent. An additional container such as a wash of the carboxylic acid product. The apparatus according to an embodiment of this aspect of the invention may also include a power recovery device circulated with the condensing unit to receive gas exiting the condenser via at least one gas outlet. The power recovery unit includes at least one inlet for receiving a gas under pressure and means for extracting work from the high pressure gas. In another aspect of the invention, there is provided a process for the preparation of an aromatic retarding acid which comprises, in a reaction zone, at a high temperature and under pressure, in the presence of a catalyst composition comprising at least one heavy metal component. The liquid phase oxidation reaction mixture of the solvent and the water causes the feed material containing at least one acid-free aromatic precursor to be contacted with gaseous oxygen, and the high temperature and high pressure can effectively maintain the liquid phase oxidation reaction mixture and form dissolved or suspended in the liquid phase. An impurity of the aromatic carboxylic acid of the liquid phase oxidation reaction mixture and an oxidation by-product containing the aromatic hydrocarbon precursor, and a high pressure gas phase containing a solvent monocarboxylic acid, water and a small amount of the aromatic precursor and by-product; The high pressure gas phase removed from the reaction zone is transferred to a liquid which has been refluxed with water and the solvent monocarboxylic acid and water in the high pressure gas phase can be largely separated to form a solvent rich monocarboxylic acid, a water-depleted liquid, and a water vapor and a high pressure gas. a separation zone; transferring the pressurized gas of the water vapor removed from the separation zone to the condensation zone, and condensing the high pressure gas to form a condensate containing water and substantially no organic impurities, and containing the high pressure The non-condensable component of the body is transferred to the condensation zone in the condensation zone under pressure; the liquid phase containing water substantially free of organic impurities is recovered from the condensation zone and is suitable for purification as an aromatic At least one aqueous liquid of the method of the carboxylic acid; and the condensate containing the water free of organic impurities on the scallops recovered from the condensation zone is sent to the method for purifying the aromatic retinoic acid, at least one step of the method comprising a) forming a purified reaction solution which has been dissolved in an aqueous liquid or a group of tickic acid and impurities which have been condensed therein; (b) under the presence of a gasification catalyst at a south temperature and a partial pressure, the aromatic containing group is slowed down. Purification reaction solution of acid and impurities in an aqueous liquid is contacted with hydrogen to form a purified liquid reaction mixture; (c) a purified liquid reaction mixture containing the aromatic carboxylic acid and impurities in an aqueous liquid recovers aromatics having a small amount of impurities a solid purified product of a carboxylic acid; and (d) a solid purified aromatic carboxylic acid product recovered from a purified liquid reaction mixture containing the aromatic carboxylic acid, impurities, and aqueous liquid by washing with at least one aqueous liquid; The aqueous liquid in at least one of the steps of the purification process comprises the condensate containing water substantially free of organic impurities. In another embodiment, a method for preparing an aromatic carboxylic acid of the present invention comprises the steps of: at least one liquid phase oxidation step comprising at least one heavy metal group in the reaction zone at π temperature and high pressure In the presence of a catalyst composition, in a liquid phase oxidation reaction mixture containing a monocarboxylic acid solvent and water, at least one substituted aromatic hydrocarbon (wherein the substituents can be oxidized to a decanoic acid group) The material is in contact with gaseous oxygen, and the high temperature and high pressure can effectively maintain the liquid phase oxidation reaction mixture, and form impurities of the aromatic carboxylic acid and reaction by-products dissolved or suspended in the liquid phase oxidation reaction mixture, and 3 water, a monocarboxylic acid, an unreacted substituted aromatic hydrocarbon, an oxygen and a by-product of the reaction by-product; and at least one purification step comprising, in the presence of a catalyst at a high temperature and higher than a catalytic metal, to cause hydrogen Contacting a purification reaction solution containing a liquid of aromatic carboxylic acid and impurities recovered from the liquid phase oxidation reaction mixture in which at least one liquid phase oxidation step has been dissolved to form a dissolved reaction solution a "deuterated liquid reaction mixture of an aromatic carboxylic acid and a hydrogenated impurity of an aqueous liquid; and at least one exhaust gas treatment step comprising a high pressure gas phase removed from a reaction zone of at least one liquid phase oxidation step Solventing monocarboxylic acid and water to form a liquid containing a solvent monocarboxylic acid and a gas, a non-reactive feed material 'reaction by-product, oxygen and a small amount of a solvent monocarboxylic acid' and directly condensing water from the high pressure gas and a condensate substantially free of organic impurities; and at least a step comprising hydrating the aqueous solution substantially free of organic impurities from the at least one waste rolling treatment step to at least a (four) step, Thereby the aqueous liquid in the purification step comprises the condensate. More specifically, at least one of the purification steps comprises at least one additional step of using an aqueous liquid: (4) the inclusion in the at least phase-of-phase oxidation step. a step of suspending or dissolving the solid product of the aromatic carboxylic acid and impurities recovered by the liquid reaction mixture in an aqueous liquid to form the purified reaction solution; (b) in an aqueous liquid a step of forming a slurry of the solid product containing the aromatic carboxylic acid and the reduced impurity content recovered from the purified liquid reaction mixture; and (4) containing a small amount of impurities recovered from the purified liquid reaction mixture by aqueous silk reduction a step of containing a solid product of the aromatic carboxylic acid. The liquid phase deuteration, purification and exhaust gas treatment steps of the method according to the embodiment of the invention are preferably integrated, whereby the liquid containing the aromatic carboxylic acid and the by-product can be separately obtained The phase oxidation product and the high pressure gas phase obtained from the single liquid phase oxidation reaction are subjected to purification and exhaust gas treatment, and the liquid condensed from the pressurized gas obtained from the exhaust gas treatment step is purified as an aqueous liquid. In another embodiment The method of the present invention comprises the steps of: (3) oxidizing a reaction mixture in a liquid phase containing a monocarboxylic acid solvent and water in the presence of a catalyst composition containing a heavy metal component in a reaction zone at a temperature of a helium temperature and a high pressure. The feed material containing the aromatic hydrocarbon precursor of the aromatic carboxylic acid is contacted with gaseous oxygen, the high temperature and high pressure can effectively maintain the liquid oxidation reaction mixture, and form dissolved or An aromatic carboxylic acid and a reaction by-product impurity in the liquid phase oxidation reaction mixture and a high pressure gas phase containing a monocarboxylic acid, water, an unreacted aromatic hydrocarbon precursor, oxygen' and a reaction by-product; b) recovering a solid product containing aromatic carboxylic acid and reaction by-product impurities from the liquid phase oxidation reaction mixture; (phantom 1352080 solid recovered from the liquid phase oxidation reaction mixture of the aromatic carboxylic acid-containing and reaction by-products magazine Suspending or dissolving the product in an aqueous liquid (at least a portion of which comprises the condensate recovered according to step (1)) to form a purified reaction solution; (d) at a high temperature and a high pressure, in the presence of a hydrogenation catalyst, the purification solution Contacting with hydrogen 5 to form a purified liquid reaction mixture; (e) recovering from the purified liquid reaction mixture a solid purified product containing an aromatic carboxylic acid having a small amount of impurities and a small amount of an oxidized aromatic hydrocarbon precursor, a hydrogenated derivative thereof or a liquid purification mother liquid composed thereof; (1) a south pressure of a solvent-containing monocarboxylic acid, water vapor, an unreacted feed precursor, oxygen, and a by-product of the liquid phase oxidation reaction from the step (4) 10 phase transfer to a separation zone which has a reflux liquid and can largely separate the monoterpene solvent and water in the high pressure gas phase; (g) a solvent monocarboxylic acid in the high pressure gas phase in the separation zone at high temperature and high pressure The acid and water are separated into a large amount into a monocarboxylic acid solvent and a water-depleted liquid, and an aqueous, aromatic feed material substantially free of a monocarboxylic acid solvent, a by-product of the oxidation step, and a small amount of a monocarboxylic acid solvent. (h) transferring the high pressure gas removed from the separation zone to the condensation zone, and transferring heat between the pressurized gas and the heat exchange fluid to condense the condensation liquid of the water substantially free of organic impurities from the high pressure gas and Forming a high pressure condensing zone exhaust; and (1) subjecting at least a portion of the condensate condensed from the pressurized gas in step (h) to step (c). More specifically, the liquid stream containing the solvent-rich monocarboxylic acid liquid n from the separation zone is moved to the reaction zone. In other embodiments, the high pressure gas transferred to the cold zone is condensed by cooling to recover a condensate containing water substantially free of organic impurities by the heat transfer from the high pressure gas to the heat exchange medium to be generated by the pressure The steam or another hot fluid is carried out; the steam or hot fluid formed under the ink can be used for heating in other steps or processes. The non-condensable component of the high-pressure gas phase obtained by condensing to recover the liquid condensate from the condensation zone under pressure and containing the high-pressure gas phase removed from the liquid phase oxidation step, and may also contain a trace amount of gaseous solvent monocarboxylic acid An acid, water, and a fatty alcohol and an ester formed by a side reaction of a solvent monocarboxylic acid due to the liquid phase oxidation reaction. Thus, in other embodiments of the invention, the condensing zone off-gas may be treated in one or more additional steps to recover unreacted feed and solvent or solvent by-products of the oxidation step. Additionally or alternatively, it may be, for example, by heat exchange to produce steam or another hot fluid for use in a process or other use, or converted to mechanical energy by a device such as an expander or other suitable device to condense substantially free of organic impurities. District waste gas pressure recovery energy. In still another embodiment of the method, providing to the separation zone to separate water from the liquid phase oxidation reaction in the high pressure gas phase and at least a portion of the solvent monocarboxylic acid, the reflux comprising liquid purification from the purification step Mother liquor. In such embodiments of the process, the purification of the solid product recovered from the liquid phase oxidation reaction preferably comprises passing the liquid containing the purified mother liquor to a liquid source that can be directed to the separation unit for reflux. BRIEF DESCRIPTION OF THE DRAWINGS The invention may be described with reference to the following drawings, in which: FIG. 1 is a schematic diagram illustrating an embodiment of an apparatus according to the present invention and used in the method of the present invention; and FIG. 2 is a view illustrating a preferred embodiment of the present invention. The method of the examples and the apparatus according to the invention, such as the apparatus of Figure 1, and the apparatus for purifying an aromatic carboxylic acid according to an embodiment of the invention. DETAILED DESCRIPTION OF THE PREFERRED EMBODIMENTS Aromatic acid protecting agents suitable for the present invention include mono- and multi-nucleating surfaces which have one or more aromatic rings and which are capable of reacting gaseous and liquid reactants in a liquid phase system. Examples of such aromatics include p-dicarboxylic acid, 1,3,5-benzenetricarboxylic acid, u, 4-benzenetricarboxylic acid, (10), isophthalic acid, benzoic acid, and naphthalene. The present invention is suitable for the preparation of a pure form of p-benzoic acid. The purification comprises terephthalic acid and the so-called intermediate purity p-dicarboxylic acid. The oxidation step of the method of the present invention is a liquid phase oxidation reaction comprising: in the presence of a catalyst composition containing a metal group, in a liquid phase reaction mixture containing a monoacid solvent and water, oxygen and A feed material having an aryl hydrocarbon oxidizable to a substituent of a carboxylic acid group is contacted. The oxidation step is carried out under conditions of high temperature and high pressure which are effective for maintaining the liquid phase reaction mixture and forming a high temperature, high pressure gas phase. The oxidation of the aromatic feed material in the liquid phase oxidation step can produce aromatic carboxylic acids as well as reaction by-products such as portions of the aromatic feed material or intermediate oxidation products and solvent by-products. The liquid phase oxidation step and associated process steps can be carried out in a batch process, a continuous process or a semi-continuous process. This oxidation step can be carried out in one or more reactors. Aromatic feed materials suitable for use in the oxidation reaction are typically included in one or more positions 'generally corresponding to the position of the carboxylic acid group of the aromatic carboxylic acid to be prepared' via at least one group which can be oxidized to a carboxylic acid group. The group replaced the aromatic smoke. The oxidizable substituent or group of substituents may be an alkyl group such as a methyl group, a propyl group or an isopropyl group or a group which already contains oxygen such as a pit group, a decyl group or a ketone group. 1352080 The substituents may be the same or different. The aromatic moiety of the starting compounds may be a benzene ring or it may be a double- or polycyclic ring such as a naphthalene ring. The number of oxidizable substituents on the aromatic moiety of the starting compound may be equal to the number of sites available on the aromatic moiety, but is generally less than all such sites, preferably from 1 to about 45 and most preferably 2 . Examples of useful feed compounds which may be used alone or together, including toluene, ethylbenzene and other alkyl substituted benzenes, o-dimethyl phenyl, p-nonyl benzene, m-nonyl benzene, anthraquinone Aldehyde, pyromellitic acid, alkylbenzyl alcohol, 1-formyl-4-methylbenzene, 1-hydroxydecyl-4-mercaptobenzene, methylacetophenone, 1,2,4-trimethyl Benzobenzene, 1-mercapto-2,4-dimercaptobenzene, 1,2,4,5-tetradecylbenzene, 10 decyl-, fluorenyl-, fluorenyl-, and methyl - substituted naphthalenes such as 2,6-didecylnaphthalene, 2,6-diethylnaphthalene, 2,7-didecylnaphthalene, 2,7-diethylnaphthalene, 2-methylindenyl-6- Mercaptophthalene, 2-mercapto-6-indenylnaphthalene, 2-mercapto-6-ethylnaphthalene, and a part of the oxidized derivative described above. For the preparation of aromatic carboxylic acids by oxidation reaction 15 of a correspondingly substituted aromatic hydrocarbon precursor of an aromatic carboxylic acid, for example, benzoic acid is prepared from monosubstituted benzene, and terephthalic acid is prepared from disubstituted benzene. Preparation of citric acid from o-disubstituted benzene, and preparation of 2,6 or 2,7 naphthalene dicarboxylic acid from 2,6- and 2,7-disubstituted naphthalene, preferably using relatively pure feed materials, More preferably, the feed material is at least about 95% by weight, more preferably at least 98% by weight or even higher, of the desired acid. A preferred aromatic hydrocarbon feed suitable for the preparation of terephthalic acid comprises para-xylene. Preferred feed materials for the preparation of benzoic acid include stupid. The solvent for the liquid phase reaction for the conversion of the aromatic feed material to the aromatic carboxylic acid product in the liquid phase oxidation step comprises a low molecular weight monocarboxylic acid, preferably 21 ((8), a monocarboxylic acid, For example, acetic acid, propionic acid, butyric acid, valeric acid and benzoic acid. Low-carbon aliphatic monocarboxylic acid and benzoic acid are preferred because of the reaction conditions for the liquid phase oxidation reaction of aromatic citric acid. The reactivity of the product to be reacted is lower than that of the high molecular weight monocarboxylic acid, and the catalytic effect of the oxidation reaction can be enhanced. The acetic acid is optimal. The solvent in the form of its aqueous solution, for example, a solution of about 80 to about 95% by weight of the acid, Most commonly used in commercial operations. Ethanol and other cosolvent materials that can be oxidized to mono-repules under such liquid phase oxidation conditions can be used as is or used with monocarboxylic acids to achieve good results. When a solvent of a mixture of a carboxylic acid and such a co-solvent is used, it is preferred to use a co-solvent which can be oxidized to the same monocarboxylic acid, so that the solvent separation step is no longer complicated. For the solvent used in the liquid phase oxidation reaction of the present invention, As used in the text The term "solvent monocarboxylic acid" as used in the component of a gaseous or liquid stream means a monocarboxylic acid having the same chemical composition as the monocarboxylic acid as the solvent for the liquid phase oxidation reaction. This usage can also distinguish such a chemical composition and other mono-acids which may be present as an oxidative brake product. By way of example, when the liquid phase oxidation mixture used in the oxidation reaction comprises an acetic acid solvent, the §5] solvent monocarboxylic acid refers to acetic acid instead of One of the k-injury or the other mono-repulsive acid species of the intermediate oxidation by-products used in accordance with the present invention, such as succinic acid and toluic acid. Moreover, as known from the text, as used herein, The phrase "solvent," but not necessarily, refers to the function of the carboxylic acid. Thus, by way of example, it is described as a solvent monocarboxylic acid as a component of a liquid phase oxidation reaction mixture. , is present as a solvent for the mixture; however, it is described as a component of the high pressure gas phase produced by the oxidation reaction or a component of the liquid phase separated from the gas phase. Solvent monocarboxylate It is not intended to indicate that the monocarboxylic acid is used as a solvent. The catalyst for the liquid oxidation reaction comprises a substance which is effective for catalyzing the oxidation reaction of the aromatic feed material to produce an aromatic carboxylic acid. It is cooled in the liquid phase reaction mixture used for the oxidation reaction because the soluble catalyst promotes contact between the catalyst, oxygen and liquid feed materials; however, heterogeneous catalyst or catalyst components can also be used. Typically, The catalyst comprises at least one heavy metal component, such as a metal having an atomic weight ranging from about 23 to about 178. Examples of suitable heavy metals include start, fierce, hunger, turn, chromium, iron, lanthanum, erbium, lanthanum or lanthanide metals. Suitable materials for such metals include, for example, acetates, hydroxides, and carbonates. Preferred catalysts include a combination of diamonds, spurs, and combinations thereof, and combinations of one or more other metals, and more preferably In the preferred embodiment, the catalyst composition for liquid phase oxidation also contains an agonist which promotes the oxidation activity of the catalytic metal, and preferably does not cause non-destructive Type or amount of byproducts. The agonist which is soluble in the liquid reaction mixture for the oxidation reaction is preferably used to promote contact between the catalyst, the agonist and the reactant. The dentate compound is often used as an agonist such as a hydrogen image, a sodium complex, a potassium salt, an ammonium halide, a south substituted hydrocarbon, a hydrocarbon halogen substituted carboxylic acid, and other functional compounds. Preferred agonists comprise at least one source of bromine. Suitable bromine sources include bromine bismuth, Br2, Ηβι·, NaBf, KBr, NH4Br, Mojiaben, &gt; stinic acetic acid, bis; r odor acetic acid, four desert smoldering, two &gt; odorous ethylene, &gt; Indifference to their combination. Other suitable agonists include aldehydes and ketones such as acetaldehyde and methyl ethyl ketone. 1352080 The reactant used in the liquid phase reaction of the oxidation step also includes a molecular oxygen-containing gas. Air is a source of oxygen. It is also possible to use oxygen-rich air, pure oxygen and other gaseous mixtures containing molecular oxygen, typically at least about 9% by volume. As can be appreciated, as the molecular oxygen content of the oxygen source increases, less compressor demand for the reactor off-gas and treatment of the inert gas can be reduced. Although air or other oxygen-containing gaseous mixture is used as the oxygen source of the process, the high pressure gas phase produced by the liquid phase reaction in the oxidation step contains nitrogen or other inert gas components of the oxygen source.

For the purposes of the present invention, the ratio of aromatic feed material, catalyst, oxygen and solvent is not critical and may vary depending on factors including the choice of reactants, solvents and catalyst compositions and the intended Details of aromatic carboxylic acid products, red design and operational factors. Range from about i: i to about 30: i solvent is better for aromatic raw materials, about 2: i to about 5: 1 is better, _ can also use more and lower ratio, even in hundreds of ratios Within the scope. The blood type upper 15 is used at least in stoichiometric amount according to the aromatic feed material, but the reaction conditions, the rate and the organic group of the horse-pressure gas phase of the m-mesh reaction are not so high that the combustible mixture is present in the gas phase. In (10) the solvent is reported as acid 'catalyst composition and operation 2 . The ratio of the material to the material; about 3 to: can effectively provide the aromatic tobacco per mole. The oxygen is most often supplied at a rate of air ===, molecular (10), and the gas phase in the reactor: the gas contains an oxidation reaction. Preferably, the solvent-free standard is from about 5% to about 8% by volume in the range of from 3 to about 5% by volume (the reaction is obtained from the reaction, and the other conditions obtained from the liquid phase oxidized 〃 fruit are removed from the reaction. Fine, the gas phase oxygen content in the lower 24 parts of the range, for example up to about 3% by volume, contributes to the preparation of an aromatic carboxylic acid having a pure form having an impurity content slightly higher than the higher gas phase oxygen content. For the liquid phase oxidation reaction of an aromatic precursor (such as p-xylene) and the purification of the formed liquid phase oxidation product according to the present invention to prepare a pure form of terephthalic acid, it is preferred to use about a gas phase oxygen content of from 0.5 to about 2.5% by volume to prepare a so-called intermediate pure product, wherein the impurity content mainly comprises 4-carboxybenzaldehyde and p-toluic acid ranging from about 100 to about 1,000 ppmw. The high gas phase oxygen content facilitates the preparation of products which can be purified to a more pure form of terephthalic acid, wherein the levels of such impurities are typically less than about 200 ppmw, based on the weight of the aromatic hydrocarbon feed and solvent, Catalysts suitable for use with catalytic metals are greater than about 1 〇 Ppmw, preferably greater than about 5 〇〇 ppmw, and less than about 1 Torr, 〇〇〇pprnw, preferably less than about 6,000 ppmw, more preferably less than about 3,000 ppmw. Preferred halogen-containing agonist and more preferably bromine-containing The agonist is present in an amount such that the atomic ratio of the element to the catalytic metal is preferably greater than about 0.1:1, preferably greater than about 〇2:1, and most preferably less than about 4:1. Less than about 3: 1. The atomic ratio of halogen to catalyst is optimally from about 0.25:1 to about 2: 1. If other conditions are the same, the concentration of the catalyst in the oxidation reaction mixture is increased in the liquid phase oxidation reaction. The reaction rate and consumption of oxygen are increased and the unreacted oxygen content in the gas phase derived from the oxidation reaction is reduced, thereby providing controllability of preparing a plurality of pure forms of aromatic carboxylic acid by the method of the present invention and Resilience. The liquid phase reaction for oxidizing an aromatic feed material to obtain a product containing an aromatic carboxylic acid is carried out in a suitable oxidation reaction zone, which typically comprises one or more oxidation reactors. Suitable oxidation reactor assembly and construction can withstand high temperatures The high pressure conditions and the septic liquid and gas phase used in the reaction zone can provide addition or mixing of the catalyst, liquid and gaseous reactants with the solvent, and the aromatic carboxylic acid product can be removed or contained therein. The liquid of the product is subjected to its recovery, and the high pressure gas phase produced by the liquid phase reaction can be removed to control the heat of reaction. The types of reactors that can be used include continuous stirred tank reactors and plug flow or reactors. The oxidation reactor comprises a columnar vessel having one or more mixing devices for mixing the liquid reactants and distributing the oxygen in the liquid phase boiling reaction mixture, the central axis of which is vertical when the vessel is used in process applications Extending. Typically, the mixing device includes one or more impellers mounted on a rotating or moving shaft. For example, the impeller can extend from the center of the center of rotation. The reactor can be made of materials designed to withstand specific temperatures, pressures, and reactive compounds used. In general, suitable oxidation reactors are made using an inert, corrosion resistant material such as titanium or at least the surface may define an internal space or volume in which the liquid reaction mixture and the reaction offgas are, such as titanium or Materials such as glass are side by side. The reaction mixture used in the liquid phase oxidation reaction is formed by combining a component comprising an aromatic feed material, a solvent and a catalyst, and adding gaseous oxygen to the mixture. In a continuous or semi-continuous process, it is preferred to combine the components in one or more mixing vessels prior to introduction to the oxidation zone; however, the reaction mixture may also form in the oxidation zone. The oxygen source can be introduced into one or more locations within the reactor, and typically introduced in a manner that promotes contact between the molecular oxygen and other reactive components, for example, by introducing compressed air or other gaseous oxygen source. In the middle part of the lower part of the internal volume of the reactor, the product in the liquid in the liquid to produce the aromatic-containing product should be oxidized to the reaction conditions, and the oxidative reaction conditions can be reversed. Effectively modulating this 0 and forming an aromatic carboxylic acid and containing the impurities of the pro-mass by-product of the 6 Xuanfangfang fe-protons dissolved or suspended in the #5 liquid reaction mixture and producing lettuce. The high (four) phase, whose gaseous component is mainly solvent Wei (that is, when the = 2 refrigerant is acetic acid, it is acetic acid) and water. The high pressure gas phase is also generally = unreduced material and oxygen in the gas phase and by-products of the liquid reduction. When the party W... is used in the operation of commercial specifications, or the source of the gas containing nitrogen or other ship gas components, the phase may also include such emotional components. . By heating the liquid phase reaction mixture, the heat generated by the oxidation is dissipated by the gas phase on top of the reaction (4). Typically, the temperature of the liquid phase reaction is maintained at about 120. (: or higher is preferably about 140 C or higher, but less than about thief and preferably less than: 23 〇 Cf. In the preparation of aromatic acid retardation products (such as terephthalic acid, benzoic acid and naphthalene) When the reaction temperature in the range of about 145t to about 2 Torr is lower than the temperature lower than about 12GC, the liquid phase oxidation reaction can be carried out under economic or gravitational force or rate or conversion rate which can adversely affect the quality of the product. The preparation of the self-p-xylene raw material at a temperature lower than about (10)^ can take more than 24 hours to be substantially completed, and the formed terephthalic acid product needs additional treatment due to the impurity content. The degree is not good 'because it may produce undesired burning phenomenon and the loss of 4 lbs. The pressure of the rib liquid reaction mixture can be read to the boiling temperature of the liquid phase 27 1352080 reaction mixture and selected to maintain a large amount of liquid Phase reaction mixture. A pressure of from about 5 to about 40 ng/cm 2 is preferred, and the preferred pressure for the particular process varies with feed and solvent composition, temperature, and other factors, and more preferably ranges from about 1〇 to about 30 kg/cm 2 . At a reaction pressure of 7 to about 21 5 kg/cm 2 , the temperature of the reaction mixture containing acetic acid as a solvent and a gas phase derived from the liquid phase reaction is from about Π〇 to about 21 〇. (: If appropriate) The residence time in the reaction vessel may vary depending on the particular throughput and conditions. For some processes, a suitable residence time is from about 20 to about 150 minutes. For certain aromatic carboxylic acid processes, such as A method of preparing terephthalic acid from a p-xylene feed material using a 10 acetic acid solvent for the reaction mixture, the solid content of the boiling liquid phase reaction mixture being as high as about 50% by weight of the liquid reaction mixture, More generally, the content is from about 10 to 35% by weight. In the process wherein the aromatic acid product is substantially soluble in the reaction solvent, the concentration of the solid in the liquid object is extremely small, as is familiar with the preparation of 15 aromatic carboxylic acids. As is known, the preferred conditions and operating parameters vary with different products and methods' and the changes can be within the above range or even beyond these ranges. The liquid phase oxidation reaction product includes self-concentration An aromatic carboxylic acid oxidized by the feed material, an impurity containing a by-product produced by the liquid phase oxidation reaction, and 20, as described above, obtained from the liquid phase reaction, which comprises boiling the liquid phase reaction mixture to remove the residue The gas phase controls the reaction temperature to be a gas phase. Specific examples of by-products of the aromatic feed material include partial or intermediate oxidation products such as toluic acid, benzaldehyde, carboxybenzaldehyde, and hydroxymethyl benzoic acid. The by-product of the liquid phase reaction also includes a solvent reaction product such as methanol and other low-carbon aliphatic alcohol oxidized from the cough 28 reaction solvent, and an ester produced by reacting the alcohol with the solvent, examples of which include Anthracene acetate, decyl propionate, butyric acid, etc. By-products are usually present in the liquid phase oxidation reaction mixture and in the gas phase formed therefrom. The carbon oxide by-products can be obtained from solvents, feed materials or their like. The oxidation reaction carried out by the by-product. In embodiments of the invention wherein the liquid phase reaction uses a bromine source as an agonist, the by-product also typically includes a lower carbosilane', such as when methyl acetate is used as the reaction solvent, the by-product is methyl bromide, which is typically The reaction of bromide ions with acetic acid is formed. As mentioned above, these bromine-containing by-products and impurities may be present in one or both of the liquid phase reaction mixture and the high pressure gas phase produced therefrom. In certain embodiments of the process of the invention, for example, wherein the solid product obtained from the liquid phase oxidation reaction is purified and the mother liquor or other recycle stream containing the purification step liquid or component thereof is transferred directly or indirectly to the liquid phase Examples of the oxidation reaction, by-products such as toluic acid which is sent to the purified liquid, and hydrogenated derivatives of various by-products obtained from the purification step may also be present in the liquid phase reaction mixture. Water is also produced as a by-product of the liquid phase reaction in the oxidation step. However, due to the addition of water, such as when using an aqueous monocarboxylic acid solvent or present in a recycle stream from other process steps, and due to the large amount of water present in the oxidation step, the liquid city may also be present in the liquid city. In the mixture, whether water system such as by-products is produced or deliberately added, since it is impossible or unnecessary to distinguish between the reaction water and the water added by reason, the phrase "the by-product of the money phase reaction" is used herein unless otherwise specified. And similar words do not refer to water. Similarly, when water or water vapor is described in the text as a component of various process liquids, gases or therapeutic gases, it is not considered unless otherwise specified or self-explanatory : No by water from by-products of the liquid phase oxidation reaction or water deliberately added to the process or both. The treatment may be carried out in a portion of the liquid reaction mixture obtained from the liquid phase oxidation using a known technique. Or a dissolved aromatic carboxylic acid reaction product for recovering the aromatic carboxylic acid reaction product contained therein. Typically, the aromatic acid which has been slurried, dissolved or polymerized and dissolved in the liquid reaction mixture and The by-products from the oxidation reaction of the aromatic feed material are removed from the reaction zone used in the liquid phase reaction and recovered by a suitable technique. Thus, in addition to the oxidation reaction step, the liquid phase oxidation according to the process of the invention The reaction may include recovering a product containing an aromatic carboxylic acid and an impurity containing a reaction by-product from the liquid phase oxidation reaction mixture. The product is preferably recovered as a solid product. The soluble product dissolved in the liquid may be recovered by crystallization. , which is usually cooled and released from the pressure of the liquid slurry or solution obtained from the oxidation reaction zone to achieve a solid product which is slurried in the liquid and a solid which is crystallized from the reaction liquid or from the crystal solvent. Separating from the liquids by centrifugation, transition or a combination thereof. The solid product recovered from the reaction liquid by such techniques comprises an aromatic carboxylic acid and impurities containing by-products of the aromatic feed material. The liquid remaining after the liquid reaction mixture recovers the solid product, also known as the oxidative mother liquor, comprising the solvent monocarboxylic acid, water, catalyst and agonist, and the liquid phase oxidation Soluble by-products, and may be derived from impurities such as recycle streams. The mother liquor typically also contains minor amounts of aromatic carboxylic acids and portions or intermediate oxidation products of aromatic feed materials that are not recovered from the liquid. Preferably, at least a portion of the mother liquor is returned to at least one reaction zone for liquid phase oxidation 'where the components useful for the liquid phase reaction, such as catalysts, agonists, solvents and by-products, can be converted to be reused In a preferred embodiment of the present invention, the liquid phase reaction mixture of the aromatic acid-containing acid and the liquid phase oxidation reaction by oxidation reaction is subjected to a crystallization reaction in one or more stages. Recycling from the liquid, such as in a single crystallization vessel or series (the temperature and pressure are continuously reduced from the previous stage to the later stage to increase product recovery), in 2 to 4 stages, for example, from range to about 14 Torr to about 25 (The temperature in the TC is in the range of from about 5 to about 40 kg/cm 2 to a final crystallization temperature in the range of from about 110 to about 15 〇X: ambient to a pressure of about 3 kg/cm 2 for crystallization reaction Crystallization large solid aromatic product. The mother liquor separated from the solid product by the crystallization reaction can be returned to the liquid phase reaction as described above. The heat is removed from the vessel used for the crystallization reaction by removing the gas phase formed by the sudden boiling or other pressure drop of the reaction liquid, and the gas phase removed from the one or more stages is preferably as follows, directly or indirectly Condensation is carried out via one or more additional recovery stages, and at least a portion is returned to the reaction zone for the liquid phase oxidation reaction. The solid product removed from the liquid phase oxidation reaction, which typically contains an aromatic oxidation product, and an intermediate oxidation product containing an oxidation by-product, such as the aromatic feed material, may be borrowed by any suitable technique. The liquid oxidized mother liquid formed by recovering the solid product is separated. Examples include centrifugation, vacuum filtration, pressure filtration, and transitions using a belt filter. Preferably, after separation, an aqueous liquid, such as pure water, or a small amount of a solvent, a monocarboxylic acid, a catalyst, an aromatic raw material, preferably directly or with other liquids (such as an oxidized mother liquor recycle or other reaction zone) The liquid product is recycled together to the oxidation by-product of the oxidation reaction or a combination of the washings of the mixture to form a solid product. The separation of the solid impure aromatic carboxylic acid recovered from the oxidizing mother liquor and the washing of the solid product are preferably carried out by solvent exchange filtration under pressure using a filter press as disclosed in U.S. Patent Nos. 5,679,846 and 5,200,557. A preferred filtration device for such separation steps is a BHS Fest filter as described in more detail in U.S. Patent No. 5,200,557. The mother liquor and washing removed from the filter cake can be transferred directly or indirectly to a liquid phase oxidation reaction. Filtering and using a multi-stage and using a pure shell-increasing lotion', for example as a liquid removed from the filter cake in the downstream stage of the previous stage of the soaking, the washing of the solid product can be replaced by a concentrated self-filter cake The solvent monocarboxylic acid provides an additional benefit in returning it to the oxidation reaction. In a more specific embodiment, the filter cake wetted by such a displacement filtered wash is sent to a drying stage from the final wash stage where it is contacted with an inert gas, typically at low levels. It is carried out under moderate pressure to remove a large amount of residual liquid from the filter cake. After washing and removing a large amount of the washing liquid from the solid product containing aromatic hydrazine and by-products, the solid formed may be dried and sent to storage or other steps, which may include preparing a reaction solution for purifying the solid product. The amount of residual solvent monocarboxylic acid sent to the purified solid product is preferably 5, 〇〇〇 ("ppmw") or less. The solid product can be dried by a flowing stream of nitrogen or other inert gas to reduce the residual solvent content. In addition to the aromatic acid retardation reaction product formed in the liquid phase reaction of the oxidation step of the process of the present invention, the process produces a solvent-containing monohydrate and a high pressure gas phase of water, and it usually also contains the liquid phase oxidation reaction. And the aromatic feed without anti-deer (4) and oxygen and, if present, the oxygen source complementary component as described above. The temperature and pressure of the gas phase present in the reaction zone correspond to the conditions of the liquid phase reaction. The exhaust gas treatment step of the present invention recovers energy, materials, and combinations thereof. The off-gas treatment step of the process of the present invention comprises separating a solvent mono-acid and a water-salt from a high-pressure gas phase stream containing at least one liquid phase oxidation step, thereby forming a monocarboxylic acid rich in at least one solvent. a liquid phase and at least a water-containing gas and typically a high-pressure gas containing a non-killing feed material, a reaction by-product, oxygen, and a small amount of solvent, and directly condensed from the high-pressure gas to contain water and substantially no _f, such as The condensate of the unreacted aromatic feed material and the oxidation by-product of the feed material in the liquid phase oxidation reaction. The high pressure gas phase is used for separation at a temperature and pressure of the temperature and pressure of the gas phase in the liquid phase oxidation (4) of the removal phase. Preferably, the step of treating the exhaust gas comprises the steps of: treating the gaseous solvent-containing solvent and water, and usually also containing the unreacted feed material, oxygen, and the by-product of the oxidation step, from at least one liquid such as the above The phase oxidation step is transferred to a separation zone which has a reflux liquid and can largely separate the fresh M and water of the high pressure gas phase towel; the high pressure gas phase towel of the sub-zone can be dissolved under high temperature and high pressure_ and water A The amount is separated into a liquid phase, which is rich in a solvent, water-poor, and contains a component having a lower volatility than the high-pressure gas phase of the solvent, and the solvent does not contain a solvent/other organic impurity. , such as an unreacted aromatic feed material and a by-product of the self-oxidation reaction, a high-pressure gas phase; moving the high-pressure gas removed from the separation device to a cold; A liquid condensate containing water substantially free of organic impurities. Preferably, the condensation is effected by transferring heat between the high-rise gas and the heat exchange fluid. In more detail, the separation of the exhaust gas treatment step according to the present invention comprises feeding the high pressure gas phase removed from the reaction vessel for performing the liquid phase oxidation reaction to the gas phase operation at a high temperature and a high pressure for mass separation The fraction in the gas phase and the separation zone of the solvent monocarboxylic acid. The high pressure gas phase can be directly moved from the reaction zone of liquid phase oxidation to the separation zone, wherein the separation device is directly installed therein or is intimately connected to the oxidation reaction vessel or other reaction zone, or indirectly by, for example, suitable for transfer. Connect with suitable conduits, valves, pumps, etc. A small portion of the high pressure and high temperature gas phase from the liquid phase oxidation reaction can be sent to other uses, such as the production of high pressure steam or heat exchange fluid. Preferably, the gas phase transferred to the separation device is maintained at a temperature and pressure high enough to thereby at least substantially retain the energy content of the gas phase entering the separation device, and the gas phase can be supplied and supplied to the gas phase. The retentive liquid in the separation zone is contacted to provide the sufficient heat for separation. Preferably, the gas phase is transferred to the separation &amp; 'the temperature of the gas phase entering the separation zone is lower than the reaction temperature in the liquid phase oxidation reaction by directly passing through the reaction zone or passing through a suitable pressure rated pipe. Not more than about 1 (TC, and the pressure of the gas phase entering the separation zone is no more than about 3 kg/cm 2 lower than the pressure in the liquid phase oxidation reaction. The reaction zone is also designed to operate at high temperatures and pressures. And preferably, operating at a temperature and a pressure lower than the temperature and pressure of the high pressure gas phase present in the reaction zone to avoid loss of energy content in the gas phase from the far reaction zone. Design of the separation zone More preferably, the gas phase can be treated at a pressure of at least about 80%, more preferably at least about 90%, and even more preferably at least about 95% of the gas phase pressure in the oxidation step. The pressure rating of the equipment in the separation zone is greater than Preferably, the gas phase is separated by at least about 80%, more preferably from about 90% to about 110%, of the oxidation reaction vessel or zone of the oxidation step of the process of the invention. Leading to the dissolution in the high exhaust phase of the separation step The single-ship and water-derived high-pressure gas from the separation step does not exceed about 10%, and more preferably does not exceed about 5%, of the solvent-supplemented acid phase. Preferably, the solvent mono-carboxylic acid content of the pressurized gaseous effluent is no more than about 2%, and more preferably no more than about 1%, of the solvent monocarboxylic acid content of the ruthenium gas phase leading to the separation zone. The separation zone for the exhaust gas treatment may comprise a solvent which is adapted to separate the solvent monocarboxylic acid and water in the high temperature and high pressure gas phase removed from the liquid phase oxidation reaction into a gas phase stream for flowing through the apparatus at a temperature and a high pressure. A liquid phase having a solvent containing a single acid and a pressurized gas as described above is obtained. Preferably, the separation device is a column or a column which is generally referred to as a distillation column and a distillation column, a dehydration column, a column, and a water column. And a high efficiency separation device designed to bring the gas phase flowing therethrough into contact with the liquid phase for mass transfer between the phases in a number of theoretical equilibrium stages, sometimes referred to as "theoretical plates" Thereby the gas phase can be separated or distributed to have various boiling point ranges a fraction, whereby a liquid phase enriched in at least one higher boiling component, such as a solvent monocarboxylic acid in the process of the invention, can be condensed from the gas phase, leaving a substantial absence of such higher boiling component and comprising one Or a gas of a plurality of low-boiling species (such as water in the oxidizing gas phase in the process of the invention). The temperature of the high-pressure gas phase removed from the oxidation reaction is sufficiently high, so that in addition to the boiling provided by the liquid phase oxidation reaction In addition to the function, no reboiling capacity is required. In order to promote the contact between the gas phase and the liquid phase in the separation device, for example, by directing the gas phase to the lower portion of the device, the reflux liquid is led to the upper portion. The reverse flow to the gas phase and the liquid phase is preferred. The contact may also be provided by an internal structure that provides a surface for solid-liquid contact. The separation device of the present invention may comprise a single device or multiple devices in series, 5 such as Tower, column or other structure. When two or more devices in series are used, the configuration, and the individual inlets and outlets thereof, can be in communication, whereby the high pressure gas phase removed from the oxidation reaction vessel can flow into the gas phase stream via the devices and therein Separating the high pressure steam and liquid (which includes the refluxing and solvent-rich monocarboxylic liquid separated from the high pressure gas phase in or between the devices) of 10 water and Cu monocarboxylic acid, whereby The first vessel in the series of devices removes the solvent rich monocarboxylic acid but water-depleted liquid, and preferably removes the high pressure gas from the aqueous vapor of the separation step and substantially free of organic impurities from the last unit in the series. The gas phase removed from the liquid phase oxidation reaction zone is directed to the separation zone and maintained at a temperature and pressure which is such that the gas phase leading to the apparatus is substantially not lower than the inlet temperature and pressure as described above. The temperature of the gas phase in the separation zone preferably ranges from about 140 to about 200 ° C, and more preferably from about 160 to about 185 ° C. The pressure is preferably from about 5 to about 40 kg/cm 2 and more preferably from about 10 to about 20 kg/cm 2 . 20 Aqueous reflux liquid is supplied to contact the high pressure steam in the separation zone. Any suitable source of liquid which is aqueous and substantially free of impurities which are detrimental to the separation step can be used. Preferred sources of reflux liquid include liquids which are condensed by the high pressure gas removed from the separation and/or condensation zone of the process of the present invention. In another preferred embodiment, which is described in more detail herein, the purified mother liquor obtained by recovering the purified aromatic carboxylic acid product from at least one of the purification liquids 36: s) 1352080 is sent to the separation zone, whereby The reflux of the separation zone contains the purified mother liquor. The reflux liquid for separation comprises such a purified mother liquor and a liquid containing water condensed by the pressurized gas removed from the separation and/or condensation zone of the present invention, either individually or in combination with one or more individual streams. This liquid is supplied to the separation zone. It is preferred to supply a reflux liquid at a rate and temperature at which the gas phase transferred from the oxidation reaction to the separation zone is subjected to heat generated by the liquid phase oxidation reaction. When the separation zone is connected to a liquid phase oxidation reaction vessel to substantially transfer the gas phase to the separation zone by a substantial autooxidation reaction, the reaction vessel can serve as a 10 reboiler. In such embodiments, the rate at which the supply liquid is refluxed to the separation zone is preferably expressed as the weight of the liquid supplied to the zone relative to the weight of the aromatic feed material that is directed to the liquid phase oxidation reaction. Preferably, a reflux liquid is provided to the separation zone in accordance with the process of the present invention, preferably at a temperature in the range of from about 120 to about 170 °C, and more preferably from about 13 Torr to about 160 °C. At these temperatures, preferably 15 is supplied to the separation zone at a rate of from about 4 to about 5 weight percent of liquid per part by weight of the aromatic precursor to the liquid phase oxidation reaction. The water contained in the high pressure steam stream removed from the liquid phase oxidation step and introduced into the separation zone is separated from the solvent monocarboxylic acid vapor, thereby condensing the solvent-rich monocarboxylic acid from the high pressure steam stream and being water-poor The liquid phase and the high-pressure gas containing water and containing no solvent, and leaving a higher boiling component. The separated liquid phase preferably comprises at least about 60% by weight solvent monocarboxylic acid and no more than about 35% by weight water. The water content of the separated liquid phase is more preferably from about 15 to about % by weight. The liquid from the separation zone typically also contains a small amount of heavier impurities, such as a small amount of aromatic carboxylic acid product and a portion or medium of the aromatic feed material. The group of materials may include other oxidation-introducing The content of the material of the silk/ring 1 oxidation reaction or the portion sent to the separation zone from other process steps is preferably not more than w% by weight. 10 15 The sulphate towel is the source of the precious solvent used in the reaction. As mentioned above, it may also include oxidation of by-products of the group and other components suitable for returning to the oxidation reaction and converting to the desired mirror. Other suitable uses of the liquid condensate include vapor-liquid or crystallization solvent and scrubbing-like replenishment for use in a liquid-liquid oxidation reaction for the liquid phase oxidation reaction of the recovered (IV) product from the oxidizing mother liquor, such as a vapor-liquid or crystallization solvent. If you want to check the oxidizing dryer air purifier. In a preferred embodiment of the method of the present invention, at least a portion, and more preferably all or substantially all of the separated liquid phase condensed by the high pressure gas phase self-directed to the separation zone is returned to the liquid phase oxidation reaction directly It is sent to a reaction vessel or a storage vessel for supplying a replenishing solvent to the reaction zone. In these embodiments, 'the water and the solvent monocarboxylic acid in the high pressure gas phase which is preferably separated into the separation zone' are thereby obtained from the liquid phase of the separation zone containing from about 15 to about 30% by weight of water, and More preferably, the water content of the separated liquid and the water which is returned to the oxidation reaction from the liquid material 20 by the other liquid material substantially offsets the water vapor removed by the oxidation reaction of the high pressure overhead gas phase and is used for recovery and separation. The liquid water removed by the aromatic carboxylic acid product of the oxidation reaction. The high pressure gas from the separation zone contains a large amount of water and is relatively free of solvent monocarboxylic acid. Preferably, the gas comprises at least about 55% by volume, and more preferably at least 38 to about 65% by volume water. The gas typically has a solvent monocarboxylic acid content of less than about 5, and more preferably less than about 3% by weight. Typically, the pressurized gas also contains unreacted aromatic feed material and 5 by-products of oxidizing the liquid phase, typically up to about 1% by weight. The pressurized gas content from the separation zone is typically up to about 4% by volume, preferably from about 1 to about 4% by volume. The inert component of the oxygen source, which typically comprises nitrogen and carbon oxide, may constitute up to about 45 vol% of the pressurized gas; when air is used as the source of oxygen, the nitrogen content of the pressurized gas typically ranges from about 30 to about 40% by volume. Generally, the pressure of the gas from the separation zone is less than the pressure in the liquid phase oxidation reaction to a gauge of about 1 kg/cm 2 in the south. The temperature of the high pressure gas from the separation zone is less than about 20 °C above the temperature of the liquid phase oxidation reaction, and preferably about 5 ° C to about 15 t. The high pressure gas from the separation zone is preferably greater than about 100 ° C, more preferably greater than about 120. (:, and less than about 250 ° C, more preferably less than about 230 ° C. The pressure of the pressurized gas remaining after separation is from about 4 to about 40 kg / cm 2 gauge. Separation of a large number of auto-oxidation reactions The high pressure gas in the high pressure gas phase and the high pressure gas removed from the separation zone after the solvent monocarboxylic acid are continuously sent to the condensation zone to condense from the gas to contain substantially no organic impurities, such as solvent monocarboxylic acid and the aromatic feed. a by-product of the oxidation reaction between the substance and the solvent, the liquid condensate of the water. The condensation zone may comprise any device capable of effectively self-conducting the high pressure gas to the condensation zone to condense water substantially free of organic impurities. Or a plurality of condensers or heat exchange devices capable of effectively providing heat transfer between the high pressure gas and the heat sink material (and preferably the heat exchange fluid). A single device or a plurality of devices connected in series may be used. Shell and tube heat The exchanger and the pot condenser are examples of preferred means l352. 80. Preferably, all or substantially all of the high pressure gas from the separation zone is directed to the condensation zone to recover a significant amount of energy and material therefrom. Can cause contracture After the liquid condensate is taken out from the condensing device, the exhaust gas remaining in the condensing zone under pressure is substantially cooled under the condition that the exhaust gas in the high-pressure gas leading to the condensing zone is cooled. The non-coagulated component of the high pressure gas, the gaseous reaction by-product, and a small amount of aromatic feed material from the separation zone, and is preferably between about 50 and about 150. (at a temperature of 5 liters at a temperature than the condensation zone) The pressure of the gas is not more than about 3 kg/cm 2 , and the difference between the gas removed from the knife-off device and the gas in the condensation zone is about 2 kg/cm 2 or less. And preferably from about 0.5 to about 1 kg/cm. 15 20, the cold gas in the straw condensation zone for heat exchange with the heat sink material can also be used to heat the shaft material. The heat sink material is preferably hot. White = body 'and the best is water. When making money as a heat exchange fluid, the disk can be = = :::: line heat exchange can be -:, its use outside part b money is added or subtracted to the method The heat exchange can be used to obtain: in the liquid application of other process steps, self-divided _ conduction =, 4 liquid. The preferred method of the invention is the exchange of the fluid between the high pressure gas and the aqueous heat exchange water. The steam under the pressure of (iv) is continuously carried out from the heat. Preferably, the temperature is different at different pressures. Operation - series of heat exchangers, in which the steam is sent to the corresponding pressure force - or a variety of process steps and the continuous colder temperature is £ &lt;The n under the force group is suitable for heating, and the liquid condensate of 3 water is produced from the pressurized gas product 40 1352080. The exhaust gas from the condensation zone can be recovered in the form of heat, work or both. Recycling the energy source as heat for use in the process reduces the fuel consumption required to produce the heat for use in the process. The power recovery source can be converted to electricity suitable for use in the method to reduce power consumption from external sources used in the method. Although a preferred embodiment of the invention includes condensing all or substantially all of the high pressure gas transferred to the condensation zone, in some embodiments of the invention, the separation is performed by extracting the thermal energy source from the gas. In addition to the condensing effect of the high pressure gas, only a portion of the water content of the gas is condensed. The heat exchange efficiency as an energy recovery method is reduced as the additional water is condensed. Thus, by avoiding the range in which the heat exchange efficiency is substantially reduced, partial condensation can be used in embodiments of the invention to increase total energy recovery, but typically its material recovery is lower than in other embodiments. The partial condensation is used for recovering a liquid condensate containing substantially pure water having a low organic impurity content, and recovering the heat energy transferred to the heat exchange fluid when the liquid condensate is condensed by cooling the high pressure gas, and also remains The lower uncondensed water is in the high-pressure condensing zone exhaust gas for further energy recovery in the form of work. In the embodiment of the invention in which the high-pressure gas system is sent to the condensation zone for condensation, whereby the 20-condensable component is not completely condensed, the partial condensation is preferably carried out, whereby the high pressure is supplied to the inlet of the condensation zone. About 50 to about 85% of the water content of the gas is condensed. In such embodiments, from about 70 to about 80% of the water content of the inlet pressurized gas is preferably removed by the condensing action. The exhaust gas in these embodiments is suitable for extracting energy in a hot form, such as heat exchange, 41 or, for example, using an expander to extract a workable form of energy. According to the present invention, it is closed, and is obtained from oxygen = should be separated. The high pressure = medium and water _ or (d) Shangcai high pressure gas system condenses by heat exchange with the body. The high-pressure gas obtained from the separation of the scent = the condensed material of the singularity or the singularity of the slag, the squeezing of the residual body after the condensing is reduced to the subsequent processing step, and the metal having only a low degree of resistance of 2 degrees can be used. Such as (iv) steel, mild steel or double refined steel, as a replacement for more expensive, highly resistant lung metals or alloys in the settings required for subsequent exhaust gas treatment steps, which may be included in the process. The total condensing effect of the solid part of the condensable component removed from the separation can also be increased (4) the volume of the liquid condensate of the water that reduces the impurity of the organic matter. The recovery of the liquid phase oxidation by-products of the aromatic feed material and the solvent remaining in the uncondensed gas after the acid is tempered or condensed can be enhanced. Condensation can be performed in a single step. It can also be carried out in multiple steps, wherein in the first stage, the gas stream containing the high pressure gas removed from the separation zone is cooled to a first temperature to produce a first stage condensate, which is then The uncondensed portion of the gas is condensed at a lower temperature to obtain a second stage condensate, and the uncondensed portion of the gas is directed to the second stage, and one or more additional steps may be selected as needed. The uncondensed portion of the stage gas is condensed at a lower temperature than in the previous stage to form a liquid condensate and a residual uncondensed gaseous portion. The heat exchange between the pressurized gas and its uncondensed portion in the staged condensers can result in heat exchange fluids at different temperatures or pressures, such as medium and low pressure steam, which can be used in other process steps or Heating outside the process. In the preferred embodiment of the invention 352080, two or more levels of steam are produced for energy recovery, preferably using condensing or other low pressure steam turbines. In such embodiments, the condensate removed at different temperatures may be sent to other operational uses having corresponding temperatures to avoid additional heating or cooling of the condensate portion, and in some cases, It is necessary to limit the accumulation of specific impurities in the step of recycling the condensate. For example, the condensate removed at a temperature ranging from about 9 Torr to about 3 〇 ° C can be preferentially sent to one or more of the purification steps, such as mixing an impure aromatic carboxylic acid in an aqueous liquid. To form a purified reaction solution or as a crystallization solvent for use in the purified aromatic carboxylic acid product. At almost no further heat input, at a relatively south temperature, for example, in the range of from about 130 to about 160 ° C, the recovered condensate itself or with an aqueous liquid obtained from other processing steps (such as in a purification step) The mother liquor remaining after recovery and/or separation of the purified aromatic carboxylic acid is well suited as a reflux for separation. When such high temperature condensate is used as a reflux for separation, due to the low content of its light components such as 15 lower alcohols and solvent monocarboxylates produced as solvent by-products in the liquid phase oxidation reaction, Additional benefits are obtained and tend to condense at higher concentrations in lower temperature condensate. Lower temperature condensate, such as this condensate in the range of about 60 to about 90 ° C, is also very suitable for use in thermal condensate applications, such as washing and liquid phase oxidation reactions for product separation, purification reactions or two A sealing rinse used in 20, and a lower temperature condensate, such as a condensate in the range of about 40 to about 50 ° C, suitable for condensate applications, such as scrubber washes. Although the condensation that can be carried out to other temperatures with suitable temperatures to different temperatures can provide a preferred method of energy management in the method of the invention 'should be understood, if necessary, for example, for other steps 43 1352080 The heat exchange process will cool or heat the condensed condensate fraction or stream at a temperature that is higher or lower than the temperature required or preferred for such other steps. According to a preferred embodiment of the present invention, the exhaust gas obtained from the condensation zone under pressure and the five households of anhydrous antimony on the shell can retain the water of the pressurized gas obtained by the separation according to the degree of condensation in the condensation step. . In addition to the water vapor in the exhaust gas, the gas may comprise a non-condensable group of liquid phase oxidizing waste gases, such as unreacted oxygen from the oxidation reaction, if present in the oxidation reaction. Nitrogen, carbon oxide and other inert gas 10 components in the source, and oxidized carbon with a small amount of the feed material and solvent monocarboxylic acid, and other oxidation by-products of the unreacted feed material, and trace amounts obtained from others The solvent monocarboxylic acid of the exhaust gas which has not been removed in the step. Even when the water in the exhaust gas is completely condensed into a liquid condensate 70, so that the uncondensed waste gas remaining after condensing does not contain water, the ink force of the exhaust gas is high enough, and especially when the liquid phase is 15 The gaseous oxygen source used in the oxidation reaction is air or another gaseous mixture having a large amount of inert gas, whereby the gas phase removed from the oxidation reaction and the pressurized gas obtained from the separation zone and the condensation zone contain a large amount of inert gas content. At this time, the volume of the condensing zone exhaust gas makes it a useful source for energy recovery. 2〇 According to some embodiments of the invention, the energy source is recovered from the pressurized exhaust gas obtained from condensation. Energy is preferably recovered in the form of work. In these embodiments, the pressurized gas stream containing the off-gas from the condensation zone is transferred directly or indirectly to the means for recovering the energy in the form of work. Preferably, the energy recovery device is an expander or a gas stream adapted to be received under pressure and equipped with blades that can be rotated by the 44 1352080 flowing gas, thereby producing work that can be used for other process steps or processes and under reduced pressure. A similar device for cooling gas. The work may be extracted from the pressurized gas to produce, for example, the power of a generator or a compressor that compresses air or a source of gaseous oxygen for liquid phase oxidation or other equipment that requires mechanical work. This extracted source can be used in other steps of the process or other methods. Alternatively, it can be stored or transferred to an electric tree for transmission to other locations. The exhaust gas remaining after recovering the energy in the form of work can be discharged, preferably subjected to additional treatment, such as condensing to remove the water present in the condensed zone exhaust gas in an appreciable amount and to perform the scrubbing gas to remove 10 Conducive to the release of bromine or other compounds in the atmosphere, after the discharge. If necessary, energy recovery can be carried out after scrubbing or treating the gas to remove the humic compound. The removal of corrosive components prior to energy recovery facilitates the fabrication of internal components of expanders or other power recovery devices from materials having lower corrosion resistance than preferred materials; however, the removal steps of such components are also The power that can be recovered from the gas 15 can be reduced. As an alternative to the high pressure exhaust gas from the condensing zone or, as a further step of recovering the energy source in the form of work as described above, the exhaust gas obtained from the condensation can be treated to remove organic and other combustible compounds and corrosive components. In certain embodiments, such treatments are particularly useful for recovering a small amount of unreacted aromatic feed material, and the reaction product of the solvent monocarboxylic acid that may remain in the exhaust gas for oxidation. The condensing action of the high pressure gas obtained from the separation includes one or more condensations at a temperature low enough to cause the water in the gas to be substantially 'and preferably at least about 8% condensed and volatile impurities The ester reaction product such as a lower alcohol and the solvent monocarboxylic acid may remain in the unreduced exhaust gas phase at a temperature which is sufficiently cooled to a temperature of preferably from about 4 Torr to about 9 Å. In the embodiment of the present invention, since the uncondensed exhaust gas obtained from the condensing action is sufficiently cold, it can be used as a liquid scrubber for recycling, thereby facilitating the separation of the impurities. In other embodiments, the treatment aids in reducing or removing organic species such as the unreacted feed material and, if not removed, solvent by-products, and from the use of a bromine source as a liquid phase oxidation catalyst. The by-product of the ruthenium bromide reaction of the liquid phase oxidation reaction of the agent, the high pressure gas phase generated in the liquid phase oxidation reaction and the subsequent removal of the high pressure gas removed from the separation and self-condensation The exhaust gas is treated. It should be understood that such treatments may affect the amount of energy recovered from the exhaust after condensation. Therefore, in the embodiment of the invention in which the exhaust gas in the condensing zone is treated before the energy in the form of work is recovered, the preferred treatment is carried out without a large loss of pressure or volume of the gas. When the condensing zone exhaust gas has an appreciable water content, it is also preferred that the water is not condensed or cooled from the gas until the recovery of the energy source in the form of work does not cause a large amount of condensation of the water. In these embodiments, the preheating of the treated gas is preferably performed prior to energy recovery. The present invention includes the treatment of a pressurized off-gas from a condensing action to remove unreacted feed material and solvent by-products produced in the liquid phase oxidation reaction, such as a lower alkyl ester of the solvent monocarboxylic acid In one example, the treatment helps to return these components to the oxidation reaction. The treatment method also reduces the presence of these impurities in the process of recurrence of the % material stream and its stable balance in the total process operation. Preferably, the uncondensed gas removed from the pressure by self-condensation is contacted with the liquid scrubber at a temperature of from about 35 to about 60 ° C to obtain a small amount of m aromatic feed, solvent or solvent. a gas-washed gas phase of the product and a reaction product containing the unreacted aromatic feed material, the solvent monocarboxylic acid or a reaction product derived from liquid phase oxidation (such as its corresponding alcohol with the solvent) a liquid product of at least one of esters. Preferably, the liquid product is returned to the reaction zone in the liquid phase oxidation step. Any suitable scrubber and gas stream for contacting the 3-6 condensing exhaust gas may be used to extract volatile components from the gas, such as unreacted feed materials, solvent monocarboxylic acids, and/or A by-product of the auto-oxidation reaction is transferred to the liquid phase. A high-pressure absorption column having an internal structure such as a disk or a packed bed having a gas for promoting the gas to be scrubbed, which is in contact with the liquid scrubber, is usually used. Suitable scrubbers are those which are liquid at the temperature of the gas to be scrubbed, and wherein the materials to be recovered have a large degree of solubility. Examples include lower alcohols and c18 carboxylic acids such as acetic acid, C. Acid, butyric acid, etc. The preferred liquid scrubber is a monocarboxylic acid which can be used as a solvent for the liquid phase oxidation reaction and a mixture thereof with water. Suitable scrubbers, apparatus and their use for the liquid phase oxidation reaction of aromatic feedstocks to aromatic carboxylic acids to recover exhaust gas components are described in further detail in US 6,143,925, which is incorporated herein by reference. Reference materials. The pressurized condenser off-gas, with or without prior treatment of the scrubbing of the untreated feed material or solvent by-product as described above, may also be treated to remove the rot or its flammable material. Although any method which can perform this removal step without a large loss of pressure and volume of shai gas can be used, it is preferred to subject the gas to an oxidation reaction and to optimally carry out a catalytic oxidation reaction to remove organic, combustible gas. ! And rot! Suspected component. These treatments are generally included in high-temperature, low-corrosive or more environmentally compatible gases that can be oxidized to organic, flammable, and rot components to a concentration of 1352080 carbon and water, and are substantially not low. The uncondensed gas under pressure is heated under the pressure of the pressurized gas pressure, and includes exhaust gas under pressure from self-condensation or scrubbing or other treatment, and gaseous oxygen in the combustion zone. Preferably, the heating of oxygen is carried out under pressure in the presence of a suitable oxidation catalyst disposed in the combustion zone so as not to interfere with the flow of the heating gas therebetween. The pressurized gas may be optionally preheated prior to oxidation. Preheating can be carried out by any suitable means, such as by heat exchange, direct steam injection, or other suitable method. The combustion treatment may also optionally include scrubbing a 10 pressure gas removed from the combustion to remove acidic, inorganic materials, such as when the bromine source is used as described above for liquid phase oxidation reactions. Bromine or hydrogen bromide produced by the oxidation of bromo alkane in the exhaust gas. Catalysts for catalytic oxidation reactions typically comprise at least one transition group element of the Periodic Table of the Elements (IUPAC). Preferred are Group VID metals, more particularly 15 platinum, palladium and combinations thereof with one or more additional or auxiliary metals. It can be used in the form of a composite such as an oxide, such a catalytic metal. Typically, the catalytic metal is disposed on a carrier or carrier material which has a low or no catalytic activity but which is strong in strength and stability to withstand the high temperature and high pressure oxidizing environment of the combustion zone. Suitable catalyst carrier materials include gold 20 genus oxides containing one or more metals, examples of which include mullite, spinel, stone less, oxidized stone, oxidation in Lu, Shi Xi Stone oxidation in Lu, titanium oxide, oxidation error. Various crystal forms of such materials can be used, such as alpha, 7&quot;, (5 and 7? oxidized, rutile, and anatase titanium oxide. The catalyst metal loading on the carrier composition is the most Preferably, a fraction of a few percent by weight, when processing a gas having a large amount of water tea vapor content (such as about 20% by volume or more), preferably uses a higher filling amount. Any convenient configuration, shape or The size of the catalyst β, for example, the catalyst may be in the form of small particles, particles, rings, spheres, etc., and preferably may form a hard blister, honeycomb, porous or pore 5-hole structural configuration or Promoting contact with the gas present in the combustion zone without hindering the flow of gas through the zone. A specific example of a catalytic oxidation catalyst for the exhaust gas removed by the condensation treatment of the exhaust gas treatment of the present invention comprises a load bearing In the embodiment of the invention in which the energy source is recovered in the form of work from the gas containing the exhaust gas removed from the condensation zone, and in the embodiment of the invention Especially when this gas pack An appreciable amount of water (e.g., at least about 5% by volume), the gas may be selectively heated to prevent the gas sent to the energy recovery from containing liquid water. This heating step may be in other processing or processing steps, such as The thermal or catalytic oxidation reaction should be carried out before, after or together. In these embodiments, the heating can be carried out by any suitable technique, such as by heat exchange or direct injection of steam or other hot gases. Heating to about 20 ( TC or higher can effectively prevent water condensation, preferably at a temperature of about 250 to about 350 ° C. Except for the condensed 20-zone exhaust gas remaining after condensation of the high-pressure gas removed from the separation H, the exhaust gas treatment step of the method of the present invention The condensing action can condense the liquid obtained from the pressurized gas. The condensate contains high-purity water. In addition to the external liquid, the condensate contains an organic impurity containing a small amount of a solvent, a single acid, and the solvent monobasic acid, and a solvent thereof. Acidic vinegar' and a small amount of low molecular weight alcohol reaction product of a portion of the aromatic feed material or intermediate oxidation by-product. 49 1352080 according to the method of the invention And the composition, the water and impurity content of the condensate may be slightly different. However, in general, the condensate has a water content of at least about 94% by weight, and preferably from 96 to about 98% by weight. The solvent has a mono-content of about 5% by weight or less, and preferably no more than about 5% to about 3% by weight. Impurities such as oxidation reaction products with or from the solvent and oxidation of the aromatic feed material The low-carbon fatty alcohol of the solvent formed by the by-product and the vinegar thereof are typically present at a level of up to about i% by weight, and preferably no more than about 5 〇〇 ppmw. The low organic impurity content allows the liquid, which does not require additional purification or other treatments that reduce the level of impurities, is suitable for other uses, including not only the wash solution for solid-liquid separation but also the separation from the liquid phase oxidation reaction. The reflux or washing of water and solvent in a high pressure gas phase, and as an aqueous liquid in the process for preparing a purified aromatic carboxylic acid. Unexpectedly, even in the commercial specification process, the 15 liquid condensate does not require additional treatment or purification, ie is not only suitable as a crystallization solvent or lotion for the recovery and separation of the aromatic carboxylic acid product in pure form. And it can be used as a solvent for a solvent reaction solution containing an aromatic carboxylic acid and an impurity which have been dissolved in an aqueous liquid. Therefore, in a preferred embodiment of the method of the present invention, a liquid condensate which is condensed from a pressurized condenser off-gas and which contains water and substantially no organic 20 impurities is sent to an aromatic carboxylic acid purification method or step, and can be used as A new or supplemental solvent that dissolves the crude or impure aromatic carboxylic acid product to be purified. In these examples, the process of the invention not only reduces or even eliminates the need for demineralization or other high purity water sources for known aromatic carboxylic acid purification processes, but also reduces the need to treat or liquid Waste Disposal Process v &lt;? 50 The volume of the effluent. In an embodiment of the invention comprising purifying or preparing a purified aromatic carboxylic acid, the at least one purification step comprises providing the aqueous and aromatic carboxylic acid at a temperature of about half and at a temperature in the presence of a hydrogenation catalyst-containing catalyst. The purified reaction solution of the liquid in which the impurities are dissolved is contacted with hydrogen to form a purified liquid reaction mixture containing the aromatic carboxylic acid and hydrogenated impurities which have been dissolved in the aqueous liquid. In a preferred embodiment, the crude solid product recovered from the liquid phase oxidation reaction is dissolved in an aqueous liquid to form a purified reaction solution containing an aromatic carboxylic acid and an oxidation reaction containing a β-aromatic feed material. Impurities of oxidation by-products. Preferably, the dry crystallization product is obtained by recovering the pure aromatic hydrocarbon product containing a small amount of impurities from the purified liquid reaction mixture, and the liquid purification mother liquid remaining after recovering the product in the pure form and/or from one or A variety of aqueous liquids, such as crystallization solvents and washings, separate the product in pure form. The at least one aqueous liquid used in the purifying step includes a condensate containing water which is substantially free of organic impurities recovered from the condensation zone in the exhaust gas treatment as described herein. According to another preferred embodiment of the present invention, the purified mother liquor obtained from at least one purification step is sent to an exhaust gas treatment, wherein the purified mother liquor is removed as a separation zone or a washing liquid is removed by a large amount of separation from the liquid phase oxidation reaction. The solvent monocarboxylic acid and water vapor in the high pressure gas phase. As described above, the aromatic carboxylic acid product obtained by the liquid phase oxidation reaction of a feed material containing an aromatic compound having an oxidizable substituent is sometimes referred to as a crude aromatic carboxylic acid product or from liquid phase oxidation. The crude product of the reaction comprises an aromatic carboxylic acid and one or more oxidation interdescent products or by-products. Although the specific chemical composition of the intermediate product and by-products may vary depending on the composition of the oxidative feed material, the oxidation reaction conditions, and other factors, and may not even be fully understood by the particular feed material, it is known to include - Or a plurality of aromatic compound-based compounds such as benzofural, carboxybenzaldehyde, ketone and hydrazine which may result in an undesired color of the desired aromatic ship product or the polyester produced therefrom or the undesired color. And the compounds can be hydrogenated to a species which is more soluble in the aqueous solution than the aromatic carbonyl compounds and aromatic carboxylic acids or which has a lesser color or tendency to color. The preferred impure aromatic carboxylic acid product to be purified according to the present invention is an aromatic carboxylic acid-containing, and the aromatic feed material is subjected to a liquid phase oxidation reaction, and the liquid phase oxidation reaction and purification step are integrated therein. The crude solid product in which the liquid phase oxidation reaction is the crude product of the by-product produced by the liquid phase oxidation reaction in a continuous process for the starting material for purification. However, it should also be understood that the starting materials for use in the purification reaction may be or include impure products containing aromatic slow acids and aromatic carbonyl impurities as described above, which are derived from the integration or non-conformity of the feed materials. The liquid phase oxidation reaction is integrated or present or produced as a by-product from other methods or sources. The invention therefore includes wherein the impure aromatic traculous acid product starting material for purification comprises aromatic phthalic acid and at least one of which can form an aqueous solution having a solubility greater than the unhydrogenated aromatic carbonyl impurity or less color or The hydrogenation of the coloration tendency, the aromatic carbonyl impurity of the aromatic product substituted by the carbonyl group. Purification is carried out by subjecting a small amount of a solvent monocarboxylic acid, which may also be present in the impure aromatic carboxylic acid product, such as residual solvent remaining in the crude product obtained from the liquid phase oxidation step. The concentration ranging from hundreds to thousands of ppmw, as is ubiquitous in products derived from commercial scale liquid phase oxidation reactions, does not adversely affect the purification of the process of the invention. The aromatic carboxylic acid product to be purified preferably has a solvent monocarboxylic acid content of not more than about 10% by weight. In more detail, a preferred purification step of the present invention comprises dissolving a solid product containing aromatic (tetra) and impurities in an aqueous liquid, at least a portion of which preferably comprises the condensation of the exhaust gas treatment described herein and includes substantial The bribe towel with no organic impurities is decontaminated into a purification reaction, and the purified solution is contacted in the presence of a hydrogenation catalyst at a high temperature and a high pressure to form a purified liquid reaction mixture, and the purified liquid reaction mixture is recovered. A solid purified product of an aromatic lysate having a small amount of impurities, and an aqueous liquid purification mother liquid containing oxidation by-products, hydrogenated products thereof, and combinations thereof is separated from the recovered solid purified product. An impure acid is used in the aqueous solution to carry out a gasification reaction of the impure aromatic ship to reduce the impurity content. The condensate which is condensed from the pressurized exhaust gas of at least one of the exhaust gas treatment steps as described in the text is used as a purifying agent. Although in order to avoid increasing the cost, complexity and additional equipment for the use, storage or handling of the condensate, it is preferred to directly supply the condensate from the condensing process without the use of by-products or other impurities. The addition or intermediate treatment, but it should be understood that such increased processing is not excluded, although it does not require the condensate to be suitable as a solvent for purification. Likewise, while it is not necessary to obtain a test medium of sufficient purity to be suitable as a purification solvent for the present invention, it should be understood that this month covers the use of a liquid condensate derived from condensation with a new demineralized water or other source of purified water. The liquid condensate recovered from the high pressure gas condensation obtained in the separation step of the present invention preferably constitutes at least about 50%' and more preferably from about 80 to about 100% of the solvent used in the purification reaction solution. 1352080

The concentration of the purification solvent of the impure aromatic carboxylic acid to be treated in the purification step is generally low enough to substantially dissolve the impure acid, and the concentration is sufficiently high for practical system operation and efficient application, It can also be used as a solvent for the liquid and after recovering the aromatic carboxylic acid in a pure 5-form form with a small amount of impurities from the purified reaction mixture, it can still be used as a purification mother liquid. The solution containing from about 5 to about 50 parts by weight of impure aromatic acid in each hundred parts by weight of the solution at the temperature of the process is suitable for providing the proper solubility required for practical operation. Preferably, the purification reaction solution contains from about 8% to about 3% by weight, and more preferably from about 20 to about 35% by weight, of the impure aromatic carboxylic acid, at a temperature for purification by the gasification reaction. 10 Catalysts suitable for purification of hydrogenation reactions comprising one or more catalytic activities required for hydrogenation of impurities in impure aromatic carboxylic acid products, such as oxidation intermediates and by-products and/or aromatic carbonyl heavys metal. The catalyst metal is preferably supported or carried on a carrier material which is insoluble in water and which does not react with the aromatic acid retardation under the purification process conditions. A suitable catalyst metal is the first difficult metal of the Periodic Table of the Elements (IUPAC version), which includes Ji, Ming, Qian, Iron X, Silver, and combinations thereof. Shouting includes the best combination of gold and heart. Carbon and charcoal having a surface area of several hundred or several thousand... and sufficient strength and abrasion resistance which are long-term use under operating conditions are preferred carriers. The metal filling is not important, but the filling amount of 疋H is preferably about 5% by weight based on the total weight of the genus and the genus of the genus or the metal group, and the conversion is present in the absorbing material ( It comprises from about 1% to about 3% by weight, and more preferably about (%)% of a bismuth metal, for the use of the medium. For these purposes, the metal preferably comprises. For use, the catalyst is preferably used in particulate form, for example, pellets, extrudates, spheres or granules, but other solid forms are also suitable. The particle size of the catalyst is selected such that the bed of catalyst particles is readily maintained in a suitable purification reactor, but the purified reaction mixture can be passed through the bed without undesired pressure drops. Preferably, the average particle size allows the catalyst particles to pass through a 2-mesh screen, but can be retained on a 24 mesh screen (1) s Sieve Series) and, more preferably, through a 4 mesh screen, but retained in a 12 mesh screen and optimally 8-mesh screen. on. The aqueous purification reaction solution is contacted with hydrogen in the presence of a catalyst under high temperature and high pressure for purification. The temperature ranges from about 2 Torr to about 37 Torr, preferably from about 225 to about 325 ° C and most preferably from about 240 to about 300. (: The pressure is sufficient to maintain the liquid phase containing the aqueous reaction solution. The total pressure is at least equal to, and preferably exceeds, the sum of the partial pressures of the hydrogen gas leading to the process and the water vapor boiling from the aqueous reaction solution at the operating temperature. Preferably, the pressure is from about 35, and more preferably from about 7 to about 105 kg/cm. The aqueous solution is subjected to hydrogenation conditions as described above in a suitable reaction vessel which can withstand the reaction temperature and pressure and the acidic character of its liquid contents. The purification reaction solvent is contacted with hydrogen. Preferably, the reactor is configured to have a substantially central axis 'when the reactor is used for operational purposes, it is upright, and the cylindrical reactor can be used in both the upflow and downflow reactors. The medium is typically maintained by a mechanical carrier to maintain the catalyst particles in the bed and can be present relatively freely in the reactor via one or more particulate fixed beds of the reaction solution. Usually one touch is preferred. a media bed, but it is also possible to use multiple beds or passes with the same or different catalysts, for example in terms of particle size, hydrogenation catalyst metal or metal filling weight, 'different catalyst layers, or A single bed of catalyst and other materials, such as a substance that can protect the catalyst, and which can benefit. A mechanical carrier in the form of an annual mesh or a surface formed from a suitable parallel metal lamella is typically used. Other suitable catalyst retention devices include, for example, a tubular Johnson or a multi-well plate. The internal components and surfaces of the reactor and the mechanical carrier are rotted by the contact with the acidic reaction solution and the reaction product mixture. The utility model is composed of a material having suitable resistance. The carrier for the catalyst bed preferably has an opening of about 丨 mm or less and is made of, for example, a steel, a chin or a nickel-hydrochloride-resistant alloy (Hastelloy) c. In a preferred embodiment of the invention, an aqueous solution of the impure aromatic carboxylic acid to be purified is added to the reactor vessel or to the upper portion of the reactor vessel at elevated temperature and pressure. a position, and the solution can flow downwardly through the catalyst bed contained in the reactor vessel in the presence of hydrogen, wherein in many cases hydrogen is used to reduce impurities to dissolve in the reaction mixture a hydrogenation product which is larger than the desired aromatic acid or has a lesser color or coloration tendency. In this preferred mode, the liquid purification reaction mixture containing the aromatic carboxylic acid and the hydrogenated impurity is from or near the reactor vessel. A portion of the reactor below the bottom or bottom is removed. The reactor for purification can be operated in several modes. In one mode, the predetermined liquid content is maintained within the reactor and at a specific reactor pressure Hydrogen is fed at a rate sufficient to maintain the predetermined liquid content. The difference between the actual reactor pressure and the vaporization/flying 1 of the vaporized purification solution present in the headspace of the reactor is the hydrogen separation of the s-top space. It can be mixed with an inert gas such as nitrogen or water vapor, in which case the reaction is 1352080. The difference between the pressure and the vapor pressure of the vaporization reaction solution present is hydrogen and the inert gas mixed therewith. Merger housing. In such cases, the argon partial pressure can be calculated from the known relative amounts of known hydrogen and the inert gas present in the mixture. 5 In another mode of operation, the reactor can be filled with an aqueous liquid reaction solution 'by which there is substantially no reactor vapor space, but there are hydrogen bubbles that expand or contract at the top or top of the reactor, thus providing The reaction thieves the volume of the top portion whereby the hydrogen added to the reactor is soluble in the input purification reaction solution. In this embodiment, the reactor is operated in a hydraulic 10 full load system where hydrogen is fed to the reactor by flow control. The concentration of hydrogen in the solution can be adjusted by adjusting the hydrogen flow rate fed to the reactor. The pseudo hydrogen partial pressure value can be calculated from the solution hydrogen concentration if necessary, which can then be corrected by the hydrogen flow rate fed to the reactor. When the operation is such that the process control can be achieved by adjusting the hydrogen partial pressure, the root 15 is based on the pressure rating of the reactor, the impurity content of the impure aromatic carboxylic acid, the activity of the catalyst, and the other known to those skilled in the art. In view of the factors, the partial pressure of hydrogen in the reactor is preferably in the range of from about 0,5 to about 15 kg/cm 2 or more. In an operating mode that includes direct adjustment of the hydrogen concentration in the feed solution, the hydrogen of the solution is not saturated and the reactor itself is hydraulically 20 fully loaded. Therefore, the adjustment of the hydrogen flow fed to the reactor provides a good control of the hydrogen concentration in the solution. During the hydrogenation reaction, the space velocity, which is expressed as the weight of the impure aromatic acid in the purified reaction solution per hour by weight of the catalyst, is typically from about 1 hour to about 25 hours-1, and preferably about 2 hours 1 to about 15 hours -1. Where 57 1352080 the residence time of the purified liquid stream in the catalyst bed may vary depending on the spatial extent. The aryl Group 5 carboxylic acid product in the pure form is removed from the liquid purification reaction mixture in a pure form lower than the crude or other impure aromatic carboxylic acid product used to kill the purified solution. The purified reaction mixture comprises an aqueous reaction solvent which has dissolved the aromatic carboxylic acid and a hydrogenated aromatic impurity having a higher solubility in the aqueous reaction liquid than the hydrogenation precursor, and is cooled to separate the pure form from the reaction mixture. The low impurity solid aromatic carboxylic acid leaves a liquid purification mother liquid having hydrogenated impurities dissolved in the liquid. The separation is usually carried out by cooling to the crystallization temperature, which is low enough so that the aromatic carboxylic acid can be crystallized to produce crystals in the liquid phase. The crystallization temperature is sufficiently high that the dissolved impurities and the reaction product derived from the hydrogenation reaction are still dissolved in the liquid phase. The crystallization temperature is usually up to 16 ° C, and preferably up to about 150 ° C. In a continuous operation, the separation step typically involves removing the liquid purification reaction mixture from the purification reactor and performing a crystallization reaction of the aromatic carboxylic acid in one or more of the 15 crystal vessels. When carried out in a series of stages or in individual crystallization vessels, the temperatures in the different stages or vessels may be the same or different, and preferably decrease from each stage or vessel to the next. The BB action typically also results in a liquid boiling from the purified liquid reaction mixture, which can be recovered by condensation and recycled to one or more purification stages 20, one or more upstream crystallization stages or, in the present invention In a preferred embodiment, the solvent monocarboxylic acid and water vapor in the high pressure gas phase derived from the liquid phase oxidation reaction are separated. Preferably, the aqueous product is added to the crystallization product recovered from the deuterated liquid reaction mixture recovered in a sequential crystallization reaction which is carried out directly or indirectly with one or more wash solutions for use in the crystallization product. Preferably, the liquid comprises a condensate comprising water which is substantially free of organic impurities recovered from the high pressure gas produced by the mixture of the monocarboxylic acid and the water vapor in the high pressure gas phase derived from the liquid phase oxidation reaction. Thereafter, the purified mother liquor, which contains hydrogenated impurities, is dissolved therein to separate the crystallized, purified aromatic carboxylic acid product. The separation of the crystallization product is usually carried out by centrifugation or filtration. A preferred method of separation includes the pressurization of an aqueous slurry of an aromatic tannic acid in a pure form and the use of an aqueous liquid as described in U.S. Patent No. 5,175,355, the entire disclosure of which is incorporated herein by reference. The wash was obtained from a filtered filter cake. The condensate condensed by the exhaust gas treatment as described herein is a preferred aqueous liquid which can be used for washing in the pure form of the aromatic carboxylic acid. The purified mother liquor remaining after recovery of the solid purified aromatic acid retardant from the purified reaction mixture contains water and a hydrogenated derivative of a by-product or impurity present in the impure aromatic citric acid starting material. The mother liquor also typically includes a minor amount of aromatic carboxylic acid remaining in the solution. Such hydrogenated derivatives include compounds which are suitable for conversion to aromatic carboxylic acids by liquid phase oxidation reactions. Thus, in preferred embodiments of the invention, these hydrogenated derivatives are directly or indirectly transferred to a liquid phase oxidation reaction. in. The residual aromatic carboxylic acid present in the mother liquor may also be directly or indirectly transferred to the liquid phase oxidation reaction after separation from these hydrogenated derivatives. Preferably, at least a portion of the purified mother liquor remaining after separation of the aromatic carboxylic acid in solid form is sent to the liquid phase oxidation step to carry out the step of transferring the derivative and the aromatic carboxylic acid to the oxidation reaction. Unless the water from the purified mother liquor sent to the oxidation reaction can be used as a stream to return to the oxidation reaction, the water content of the purified mother liquor will destroy the water balance in the oxidation reaction. Preferably, the hydrogenated impurities in the purified mother liquor are transferred to the liquid phase oxidation reaction alone or preferably together with the aromatic carboxylic acid present in the mother liquor without disrupting the water balance in the oxidation reaction. More preferably, directly or indirectly, at least a portion, and most preferably substantially all, of the liquid mother liquor remaining after solid purification of the aromatic carboxylic acid is separated from the liquid purification reaction mixture, and transferred to the oxidation reaction according to the present invention. The separation zone of the high pressure gas phase exhaust gas treatment is used as a reflux liquid therein. For example, if one or more distillations are used to separate the solvent monocarboxylic acid and water in the high pressure gas phase produced by the liquid phase oxidation reaction of the aromatic feed material, all or part of the purified mother liquor may be used as a supply or Reflow of multiple columns. The water present in the mother liquor added by reflux is substantially vaporized into the gas phase in the column, and the water remaining in the gas phase leaving the column becomes part of the pressurized gas from the separation. . a high-boiling component of the mother liquor comprising hydrogenated impurities, such as a liquid phase oxidation by-product of the oxidation reaction of the aromatic feed, and if aromatic phthalic acid is present, remains on the Bahai liquid phase It can be returned directly or indirectly to the liquid phase oxidation reaction mixture, for example as part of the liquid phase of the solvent-rich monocarboxylic acid obtained from the separation or in a separate stream removed from the separation. Purification reactors, catalyst bed configurations, operational details, crystallization, and product recovery techniques and apparatus suitable for use in the process of the present invention are described in further detail in U.S. Patent Nos. 3,584,039, 4,626,598, 4,629,715, 4,782,181, US 4, 892, 972, US 5, 175, 355, US 5, 354, 898, US 5, 362, 908, and US Pat. BRIEF DESCRIPTION OF THE DRAWINGS Figure 1 illustrates in more detail the apparatus for carrying out the process for the preparation of the aromatic carboxylic acid of the present invention in accordance with the present invention. The apparatus includes a reactor having an exhaust port for removing steam on top of the reactor; a separation device capable of separating a large amount of cU8 monoacid and water vapor in a gaseous mixture of the monocarboxylic acid and water under pressure, The separation device is a high pressure gas phase that is circulated by the reactor to receive the exhaust port from the reactor; a condensing device circulated with the separation device, adapted to condense at least a portion of the high pressure gas and heat The sink material exchanges heat from the pressurized gas extraction energy source; and the liquid condensate for condensing the high pressure gas obtained from the condensing device is sent to at least one device having an aromatic carboxylic acid purification device. This figure does not describe the preferred embodiment, wherein the apparatus also includes an expander for circulating the exhaust gas recovery energy under pressure from the condensing unit. A preferred form of apparatus 'also referred to in the illustration includes a pressure rated reactor that defines a substantially enclosed internal volume adapted to contain a liquid reaction mixture and overhead vapor and comprising at least one for directing liquid An inlet to the internal volume, at least one inlet for introducing oxygen-containing gas under pressure to the internal volume, and at least one product for removing a slurry containing liquid or solid in the liquid from the internal volume a liquid product outlet' and at least one exhaust port for removing high pressure exhaust gas from the internal volume; and a reaction for receiving high pressure exhaust gas removed from at least one exhaust port of the reactor within the apparatus Separating means for circulating, and comprising at least a column comprising at least one vapor inlet adapted to receive high pressure exhaust gas flowing through the column into the high pressure gas phase, at least one reflux liquid adapted to flow through the column a liquid inlet for receiving a reflux liquid, a device within the column and located between the vapor and the liquid inlet, which is provided in the same direction as the flow direction of the high pressure steam The crucible contacts the surface of the vapor and the liquid phase, whereby the high-pressure gas phase of the hydrous c, _8 monocarboxylic acid and water vapor received in the column can be separated into a liquid phase rich in the core 8 monocarboxylic acid but poor in water. And a high pressure gas containing water, and the S Xuan Cl -8 monochatty acid in the pressurized exhaust gas received in the column is not more than about 10%, at least one liquid outlet for removing liquid therefrom, and at least one for self The column removes an exhaust port of the aqueous high pressure gas above the liquid inlet, at least one condensing device circulated with the separating device for receiving a pressurized gas of 3 water, the condensing device comprising at least one suitable a gas inlet for receiving a pressurized helium gas, at least one exhaust port adapted to remove the pressurized exhaust gas from the condensation device, for exchanging heat between the high pressure gas and the heat transfer medium leading to the condensation device, and from the gas A heat transfer device for condensing an aqueous liquid and means for purifying the aromatic carboxylic acid by feeding the aqueous liquid recovered in the condensing device to one or more receiving vessels in the vessel. Referring to Figure 1, the oxidation reactor 1 includes a continuous cylindrical shell that defines an enclosed inner volume. In use, the lower portion of the internal volume contains liquid 2, the reaction mass, and a portion of the internal volume at the liquid level contains overhead reaction gases. The internal volume is borrowed from a liquid filling container (not shown) through a plurality of inlets, such as 12a, 12b, 12c, and 1:2d, which are connected to the outside of the reactor. Aromatic feed material 'mixture and solvent in soluble form, and compressed air or another oxygen to be used in a suitable transfer line (as indicated at 13, which is in communication with inlet 12a) and a self-retracting machine or other suitable device (not shown in the figure). The configuration of these populations is good. Liquid and gaseous components can be introduced at the liquid level in the interior of the container. The reaction vessel also includes at least one outlet for removing a liquid phase reaction mixture comprising the crude product from the interior, indicated at 14 which comprises an aromatic carboxylic acid and an oxidation by-product, which is typically also in solution It is present in the liquid or suspended or slurried in solid particles in the liquid or both dissolved and suspended in the liquid. Reactor 10 also includes at least one vent or outlet 16 for removing high pressure gas phase evaporating from the liquid reaction object from within the reactor. The location of the vent 16 is preferably equivalent to the upper portion of the reactor in an appropriate position for operational use. The preferred reactor is designed as a substantially cylindrical vessel having a central axis extending substantially vertically when the reactor is in a position suitable for operational use. The container is suitable for use, such as a stirring device having a shaft 20, indicated at 18, on which one or more liquids can be rotated in the interior of the reactor during manufacturing to agitate the liquid reaction present in the reactor. Impellers 22 and 24 of the mixture. In a preferred embodiment of the invention, at least two impellers or mixing devices are mounted on the shaft to mix the gaseous and liquid components of the liquid reaction object without adversely depositing solids in the reactor. The next part. Axial flow impellers, typically fabricated as impellers, radial flow mixers, such as flat blade disc turbines and disperser discs, ribbon mixing elements, pitch blade turbines with vane pitch for cocoa flow up or down (pitched blade) Turbine mixers, which provide primarily tangential flow, and other configurations are suitable for mixing the liquid phase oxidation reaction system, and are preferably used in various combinations to demonstrate higher levels in the area below the liquid reaction mixture. The solids content, the higher gas content in the upper zone, and other characteristics of the liquid phase reaction mixture that can vary between the liquid objects. Other designs are disclosed in U.S. Patent No. 5,198,156 and U.S. Patent No. 5, 198, 152, the disclosure of which is incorporated herein by reference to the entire entire entire entire entire entire entire entire entire entire A continuous trailing edge, a non-recessed surface, and an open outer end, and preferably used with an upright tube or a porous gas distributor to distribute the hollow blade configuration of the gas, and U.S. Patent No. 5,904,423 describes a mixer in which the agitating element is Mounted on the central rotating shaft at a downward angle' and the radially inner ends of the trailing edges of the blades are angled outwardly toward the direction of movement of the blades, the agitating elements being shaped toward the direction of movement By the liquid 'and its means can be used to direct the gas under the agitating elements into the central cavity formed by the conical disk at the end of the shaft. At least the reactor, the agitator shaft, and the components of the mixing element that causes the liquid reaction mixture to contact the overhead gas during manufacturing use are made of a substantially corrosion-resistant material. Examples include titanium metal and alloys and dual refining stainless steel. Titanium metal is preferred. * The reactor is circulated with a separation device whereby the separation device reads the gas on the high top which is removed from the gas vent 16 from the reactor. The separation device is designed to self-conduct to the high temperature of the apparatus. The water vapor in the gas on the top of the reactor is separated by a large amount of Cl. 8 «acid vapor, thereby forming a liquid phase rich in the single solution and substantially free of the acid, but rich in water vapor 1 U top _L gas. A pressure-rated column or column or a series of columns or a preferred separation device equipped with at least one of the population for receiving a pressurized gas, at least one inlet for directing a returning liquid, 1352080 at least one outlet for removing high pressure gas from the separation device, and a deionization zone containing an internal structure that provides a surface to promote mass transfer between the countercurrent gas and the liquid phase, sufficient to provide a solvent in the gas phase The separation of mono-slow acid and water is ten. Reasonable 'balance phase. The device is preferably designed to feed a population of gas to a lower portion of the column or to the gas.  One or more upper positions, and the fractionation zone is located in the middle, thereby moving upward from the gas phase • I and reflowing from the rising gas phase _ the liquid to the τ ', B) produces a countercurrent. The additional material to the column or column may include a plurality of gases or secret streams that are removed or added, such as 10 to remove the monorichic acid-rich liquid from the gas phase, the outlet or inlet. 4 The separation device may also have an H device or other suitable device for increasing the ingestion' but when the substantially high (four) phase from the liquid phase oxidation reactor is sent directly to the device, 'the device is usually not needed or Since the oxidation reactor is based on the exothermic nature of the oxidation reaction, it can be effectively used as a re- 5' crucible and thus does not require a large degree of cooling. In a preferred embodiment, the direct combination or compaction of the Weihua reactor and the separation device is by direct connection or by means of one or more exhaust ports and separation devices or gases in the reactor. A suitable pressure rating tube or other conduit between the inlets is achieved, whereby the gas phase in the liquid phase reaction conditions is removed from the reactor and introduced at the same temperature and pressure in the 2G h reaction zone at the same or real f Inside the separation device. Preferably, the 3H separation device can separate the water in the high pressure gas of the device and the combination of the water and the mixture, thereby forming at least about 6 to 85 reset solvent per 100 parts by weight of the liquid. The liquid phase and the gas per 100 parts by weight of the gas contain about 65 to 65 parts by weight of high pressure gas. To achieve this separation, the fractionation zone of the separation apparatus is equipped with several theoretical equilibrium stages, such as internal discs, structural packing, combinations of discs and packed beds, or surfaces may be provided inside the apparatus for the presence of Provided by the structure of mass transfer between the gas phase and the liquid phase in the apparatus, or a combination thereof. For this separation, it is preferably at least about 20 theoretical equilibrium stages. If the other conditions are the same, the separation efficiency increases as the theoretical equilibrium phase is increased, so there is no theoretical upper limit to the number of equilibrium stages included in the separation apparatus used in accordance with the present invention. However, for practical purposes, the separation of the solvent may be such that the solvent monocarboxylic acid content of the outlet gas is 1% by weight or less of the solvent monocarboxylic acid content of the inlet gas phase of the smectic apparatus, and at least about 2 Torr may be used. A theoretical equilibrium phase is reached and provided by about 70 such segments exceeds the degree of separation described above, making the other phases impractical or uneconomical. Preferred separation devices having structured packing have at least about 3 packed bed or packed zones&apos; and more preferably from about 4 to about 6 such beds to provide the appropriate surface and theoretical equilibrium stages required for separation. An example of a suitable filler is a structured filler obtained in the form of a sheet of crucible corrugated metal obtained from KGGP LLC, which arrangement produces a flow channel whereby the fork line can produce a mixture suitable for liquid and gas phases. distance. A preferred separation device having a disk comprises from 30 to about 9 disks, of which at least about 7% is located between the population of the separation device and the inlet of the reflux liquid from the reactor. Preferably, it is in the form of a sieve or a bubble, and has a blade efficiency of about 30 to about. The number of disks required for a particular theoretical equilibrium phase can be calculated by dividing the number of stages by the efficiency of the disk. When used in operation, the gas introduced into the separation device and present therein has a liquid phase at a high m including water, monolin and other rot residues such as/odor compounds and unbound products thereof, such as when used for the oxidation Conversely, when the catalyst comprises a source of water, the bromine hydrogen present in the gas on top of the deuteration reaction. Therefore, in a preferred embodiment of the invention, the (four) structure of the separation device that is read and (4) is contacted during the process operation and Other devices are made of a suitable metal that prevents corrosion and other damage due to this contact. For such surfaces, including the disc, packing or other structure of the fractionation zone, titanium is a preferred material for construction. The titanium surface of this structure readily aggregates solid deposits undesirably, and the solid deposits contain iron oxides derived from impurities present in various process liquids circulated through the apparatus. A method of controlling the concentration of iron oxide deposits or the amount of soluble iron impurities in a process liquid is described in commonly-assigned U.S. Patent No. 6,852,879, the disclosure of which is incorporated herein by reference. In the embodiment of the invention represented by Figure 1, the separation device is a high pressure distillation column 30 having a gas inlet 34 for receiving the oxygenation reactor 1 and a plurality of disks. 31, 33, 35 and 37 clarify. The steam column includes at least one for selectively moving liquid material stream from the column to the oxidation reactor 10 via line 60, optionally via one or more intermediate storage tanks or reservoirs (not shown). Lower exit 32. The column also includes at least one liquid inlet 36 disposed in a portion above the column relative to the liquid outlet 32, such as a suitable container for pumping liquid from a reflux reservoir or directly from a purification step via line 61. (not shown) and reflux liquid is added to all or most of the trays of the column. The column also includes at least one gas outlet 38 for removing high pressure gas from the column from the separation step. The distillation column 30 can be provided with one or more additional liquid inlets 44 for introducing a reflux liquid that is different from the reflux liquid added at the inlet 36. By-products of the aromatic hydrocarbon feed containing a specific oxidation by-product 'and particularly liquid phase oxidation reaction and/or refluxing thereof, such as a hydrogenated derivative which can be introduced into a reflux liquid containing a purified mother liquor or other recycle stream Preferably, for the liquid stream, one or more, and preferably from about 2 to about 10, theoretical equilibrium stages are employed to direct the reflux liquid to a location spaced apart from each other. Additional reflux supplied by inlet 44 may be used to prevent such by-products from entering the gas phase rising to introduction point 44, thereby reducing their presence in the high pressure gas from the separation step and from column 30. content. The separation device of the apparatus according to this aspect of the invention is in communication with the condensing means. The condensing device is adapted to receive a gas stream containing high pressure gas removed from the separation device and adapted to condense a liquid condensate containing water substantially free of organic impurities from the gas stream and leaving The high pressure condenser off-gas of the non-condensable component of the gas of the separation device, and if not substantially completely condensed to the high pressure inlet gas of the condensing device, the exhaust gas may also include water vapor. The 忒 condensing device also includes at least one outlet for removing the condensate condensed from the gas introduced therein and the uncondensed gas under pressure and for guiding the inlet gas to the lower temperature or pressure An indirect heat exchange device that transfers heat between the heat exchange fluids that are removed at higher temperatures or forces. The condensing device also includes means for delivering the condensate to the purification apparatus, the apparatus preferably being circulated with a container or liquid receiving means of the purification apparatus, which is removed by the outlet for removing the condensate. The condensate can be transferred directly to the hybrid device. The material can also be included as a device for recirculating (4). The condensing device may comprise a single or a series of heat exchanges such as a shell and tube heat exchanger, a plate and frame heat exchanger or a suitable heat exchange device, wherein the heat from the population gas is transferred to the == quality, Such as water, steam or another kind of heat transfer fluid to increase the 'm temperature or pressure. For sputum methods with different steam pressure and liquid field demand or preference, it is best to let the C&A exchange The device generates steam or other heat exchange fluid at different pressures or temperatures, and produces condensate at different temperatures. The condenser is made of a material suitable for high temperature gas flow and is used _彳 or exists in it Cooling of the towel (4) (4) Made of metal or alloy of bribe characteristics. The inner surface of the steel is not good, but other metals and human gold are also suitable. σ Refer to Figure 1 for the separation device represented by the steam lung 30. The port 38 and the combined transfer line 39 are circulated with the condensing unit 5. In the figure, the condensation = 50 is composed of two condensers 52 and 62 connected in series, each equipped with a suitable gas inlet, 54 and 56, respectively. At the exit from which the gas was removed, Optionally, 56 and 66, the condenser effluent is passed via conduit 67, which includes condensate = uncondensed exhaust gas under pressure, and moved to barrel 68 to release uncondensed gas from the condensate. The exhaust gas is sent for further processing, and the condensate is transferred to one or more vessels via line 71 to purify the aromatic carboxylic acid by hydrogenation reaction of the purified reaction solution, which contains dissolved aromatic hydrazine and liquid phase A by-product of the oxidation reaction or a liquid which is suitable for conversion to a higher than the production of 1352080 Å in an aqueous solution! The aromatic liquid-based impurities of the hydrogenated derivative are contained in the aqueous liquid therein. In a preferred embodiment of the inventive device, the device also includes a monthly b source recovery device for generating an energy source 5 in the form of a work from a gaseous material stream under pressure, such as an expander 9 〇, the gas under pressure The material stream is removed from the condensing unit, such as uncondensed pressurized exhaust gas from tank 68 via line 69. The energy recovery unit is preferably adapted to direct the unit by reducing the pressure of the gas stream. The volume of the gas expands, and borrows If the rotation of the turbine is rotated, the expansion is converted into mechanical work. As illustrated in Figure i, the expander can be directly connected to the condensing device. Alternatively, the condensing device can be indirectly contacted with the energy recovery device. This transfers the gas under pressure to one or more intermediate devices (not shown), such as in a high pressure scrubber or for selective removal or U recovery, prior to the energy recovery shock. An absorption tower of trace process chemicals or by-products remaining in the gas or in a thermal or catalytic oxidation system or other pollution control device capable of removing the rancidity or flammability component of the gas, and not Substantial pressure will be lost. Typically, the liquid and gaseous streams and materials used and used in the present method are transferred via a transfer line, a conduit, and a pipe made of materials suitable for operational use and safety. It should be understood that the physical juxtaposition special element = and, if appropriate, may have a flexible region, a rigid region or both. In the case of a material flow or compound, it may include an intermediate device or, where necessary, a device. For example, suitable fruit, valve, manifold, gas and liquid flow meters and dispensers, sampling and sensing devices, and other devices for monitoring, controlling, regulating 70 1352080 and transferring pressure, flow, and other operational parameters may be present. Aspects and embodiments of the present invention are further illustrated in Figure 2 and its description below. The _ indication system is specifically described with reference to the following specific aromatic nucleus (terephthalic acid) production method: by using as a preferred raw material, p-diphenylbenzene in water and 5 as a solvent carboxylic acid for the oxidation reaction. a liquid phase oxidation reaction carried out in the liquid phase reaction mixture, a high pressure gas phase for separating the acetic acid and water used for the autooxidation reaction, and condensing the high pressure gas removed from the separation step to recover the exhaust gas of the aqueous condensate The treatment, and the purification step for hydrogenating the crude terephthalic acid product containing the liquid phase oxidation which has been dissolved in the purification reaction solvent, should be understood to describe the specific examples, features and details described. The preferences and the like are intended to be illustrative of the invention, but are not intended to limit the invention or its features in any aspects or embodiments. The method illustrated in Fig. 2 also shows a preferred embodiment of the invention in which a liquid phase oxidation reaction, an exhaust gas treatment and a purification reaction are integrated, whereby 15 of the crude aromatic carboxylic acid product from the liquid phase oxidation reaction is carried out. Purification to form the pure/gluten solution, subjecting the pressurized exhaust gas from the emulsification reaction to exhaust gas treatment, and purifying the condensate from the exhaust gas treatment as a solvent for use in a purification solution and other uses; however, it should be understood The present invention is not limited to the specific integrated flow diagrams represented in the Figure 2, and it should be understood that the present invention encompasses various multi-device columns, shared device columns, and other configurations. By way of illustrative example, the product containing aromatic carboxylic acid and reaction by-products from the multi-liquid phase oxidation reaction can be sent to s. . An early purification step in which a liquid system condensed by a high pressure gas resulting from the treatment of one or more of the high pressure gas phases of these or other liquid phase gasification reactions is used as the aqueous liquid. As a further example, the crude product from a single liquid phase oxidation reaction can be purified in a separate purification unit operating in parallel with 71 1352080, wherein the high pressure gas phase from the liquid oxidation reaction is subjected to exhaust gas treatment to recover the condensation. Liquid, and transfer it to the column of such purification equipment - or both, or as an alternative - or different green, which will be obtained from different oxidations in the purification or process steps as described in 5 The reaction or the method of purifying the impure aromatic carboxylic acid. • _ refer to Figure 2, via the inlet, where – for clarification, the liquid para-xylene feed material is continuously loaded into the oxidation reactor 110 at 112 (which is a pressure-rated, continuous stirred tank reaction) In the liquid), the liquid p-diphenylbenzene feed material comprises at least about 99% by weight of p-nonylbenzene, and the aqueous acetic acid solution preferably contains about 70 to about 95% by weight of acetic acid, a soluble compound, and a soluble compound. Such individual acetates as the source of oxidizing catalyst metals,  The m compound 'is, for example, an evolved hydrogen as an agonist for the catalyst. The refrigerant and the dimethyl sulphate are based on the weight ratio of the feed of about 2: 丄 to about 5: i, and the weight of the silly feed material at the rate of μ.佳可可得_励至嶋0 ppmw. It is better to use (4) the atomic ratio of the catalytic metal to gas 1: i to about 1. 5 : 1 提供 Provides a search by the rotation of the axis 120, which is borrowed from an external power source (not shown in the figure). The drive is shown to be mounted on the shaft and in the liquid state of the reactor.  The continuation of the towel is the result of (4) mixing the gaseous objects and the gas dispersion and avoiding the solidification of the solid in the lower region. The catalyst and agonist' are each preferably introduced into the liquid object of the reactor in the form of a solution in an acetic acid solvent. In order to effectively obtain at least the postal feed per mole of aromatic substances

A 72 The molecular oxygen rate is supplied from the sweep path of the lower impeller and to the medium. The pair of -bifluorene benzene is primarily oxidized to terephthalic acid in the liquid-recovery mixture of the reactor but is also reacted to form by-products, the pot comprising partial and intermediate oxidation products, such as 4. M_ is methylbenzoic acid and p-toluic acid, and other acids such as benzoic acid. The solid reaction product containing the oxidation by-product of p-dicarboxylic acid and p-xylene is precipitated from the liquid reaction mixture, and a small amount of 4 is still dissolved in the body towel. The solids content of the liquid is typically up to about 4 G weight percent and is difficult to self from about 2 G to about 35 weight percent. The water (10) oxidized product produces 1 oxidation reaction with exothermicity, and the heat generated by the reaction can cause boiling of the liquid phase reaction mixture and vaporization of acetic acid, water vapor, gas oxidation products, carbon oxides of the oxidation reaction. The formation of the nitrogen gas from the air towel charged to the 2 reaction and the overhead gas phase of the unreacted gas. The internal volume of the reactor is maintained at a pressure sufficient to maintain the liquid phase properties of the reaction mixture, preferably from about 5 to about 21 kg/cm. The overhead steam is removed from the reactor via vent i16. Depending on the rate of gas phase removal, the temperature and flow rate of the stream from the reactor removed and returned to the reactor as described below are also contemplated, and the reaction is maintained at an operating temperature in the range of from about 160 to about 225 °C. Contents. The solid p-xylene oxidation product is contained from the reactor 110 via the slurry outlet 114, which is included in the liquid phase reaction mixture which also contains dissolved p-dioxane, oxidation by-products and catalytic metal. The liquid effluent of the dicarboxylic acid is sent to the crystallization zone as stream 115 to recover the oxidized solid product containing terephthalic acid and the oxidation by-product of the p-diphenylene benzene starting material. In the embodiment of the invention illustrated in Figure 2, the crystallization reaction is carried out in a plurality of agitated crystallization vessels 152 and 156 which are associated with the circulation and transfer the product slurry from the crystallization vessel 152 to the crystallization vessel 156. The cooling in the crystallization vessel is carried out by pressure release, wherein the slurry in the crystallization vessel 152 is cooled to a temperature in the range of about 150 to 190 t, and then cooled in the crystallization vessel 156 to about no to i5 〇 °c. . The crystallization vessels 154 and 158, respectively, are discharged - or a plurality of such crystallization vessels to remove steam from the pressure drop in the heat exchange means (not shown) and steam generated from the surge steam. Preferably, condensation is carried out from one or more upstream crystallization vessels, such as crystallization vessel 152, to a vapor of a heat exchange unit (not shown) and may contain condensate of aqueous, acetic acid solvent and soluble products and by-products of the oxidation reaction. It is sent to one or more downstream crystallization vessels 156 to recover crystallizable components, such as terephthalic acid, and oxidation by-products that enter and condense from the boiling enthalpy of one or more upstream crystallization vessels. The crystallization vessel 156 is circulated with a solid-liquid separator 19 adapted to receive solids from the crystallization vessel containing terephthalic acid and oxidation by-products in the mother liquor containing acetic acid and water from the oxidation reaction. a product slurry and is suitable for separating a crude solid product comprising terephthalic acid and by-products from the liquid. The separation device 190 is a centrifuge, a rotary vacuum filter or a pressure filter. In a preferred embodiment of the invention, the separation device is a solvent exchange adapted to replace the mother liquor in the cake with a water-containing lotion under pressure. The oxidized mother liquor formed from the separation step is separated from the separation unit 190 by a stream 19 to be transferred to the mother cylinder 192. Transferring a majority of the mother liquor from the cartridge 192 to the oxidation reactor to return acetic acid, water, catalyst, and liquids that have been dissolved in the mother liquor or as a by-product of the oxidation reaction of the fine solid particles in the mother liquor. Phase oxidation reaction. The crude carcass product containing impurities for the pico dicarboxylic acid and the oxidation by-product of the p-dimethyl stearate is transferred from the separation unit 190 to the purification solution in stream 197 with or without intermediate drying and storage steps. The container 202 is replenished. The crude solid product is slurried in a replenishing reaction solvent in a replenishing vessel 2〇2, all or at least a portion thereof, and preferably from about 6 Torr to about 1% by weight, comprising condensate from the exhaust gas treatment zone 300. The condensate is condensed in the condensing zone 350 and is condensed from the separation device 330 and continuously sent to the pressurized gases of the condensers 352 and 362. If used, the solvent may be replenished from vessel 2, 4, such as fresh demineralized water or a suitable recycle stream, such as, as described below, condensed from steam due to pressure drop during crystallization of the purified terephthalic acid product. The liquid 'sends to the supply tank 202. The slurry temperature in the replenishing tank is preferably from about 8 Torr to about KKTC. By heating in the supply tank 202, for example, to about 260 to about 290. (: or passing it through a heat exchanger (not shown) when transferring to the purification reactor 210, and dissolving the crude product to form a purified reaction solution. In the reactor 210, preferably from about 85 to about The purified reaction solution is contacted with hydrogen at a pressure of 95 kg/cm 2. Continuously from the hydrogenation reactor 210, a portion of the purified liquid reaction mixture is moved to a crystallization vessel 220 in a stream 211 where it is reduced by the liquid. The pressure is crystallization from the reaction mixture to the stearic acid and a small amount of impurities. The purified slurry of the stearic acid and the liquid formed in the crystallization vessel 220 is sent to the solid-liquid separation device 230 in the material flow line 221. The vapor formed from the pressure drop in the crystallization reactor can be transferred to a heat exchanger (not shown) for condensation to condense, and the formed condensate is sent to the process, for example, via a suitable transfer line. (not shown) is followed by a purification feed replenishment tank 202. The purified terephthalic acid exits the solid-liquid separation unit 23 in a stream 231. The separation unit may be a centrifuge, a rotary vacuum filter, a pressure filter or One A combination of more than one. The condensate recovered in the condensing unit 350 can be sent to the separation unit as a washing liquid for use in a separation step for replacing or depleting the demineralized water demand for the final washing of the purified product. a mother liquor in which the solid purified terephthalic acid product is separated in a solid-liquid separator 230 by containing water, a small amount of dissolved and suspended terephthalic acid, and comprising hydrogenation dissolved or suspended in the mother liquor. Impurities of oxidation byproducts. According to preferred embodiment embodiments illustrated in Figure 2, preferably at least a portion, and preferably all or substantially all of the purified mother liquor is sent to oxidation reaction exhaust gas treatment system 300 as stream 233. Wherein the purified mother liquor is directed to a high pressure distillation column 30 to separate water and solvent acetic acid from the high pressure steam removed from the oxidation reactor 110. The purified mother liquor sent to column 330 is directed to the column above portion 336 In order to provide a liquid reflux for separation, the step of moving the purified mother liquid to the high-pressure distillation column from the solid-liquid separation device 230 may also re-circulate the terephthalic acid and impurities in the mother liquid to the oxidation reactor 1 10, wherein the impurities are oxidized or converted into p-dicarboxylic acid, and the water content of the purified mother liquor is substantially in the vapor in the distillation column, leaving the heated gas removed from the column, and does not significantly affect oxidation The water balance in the reaction. The step of transferring the purified mother liquor to the distillation column from the solid-liquid separation device 230 can also reduce the volume of the liquid discharge liquid required for the treatment of the liquid waste and return the valuable terephthalic acid to the oxidation reaction. And then removed therefrom for backwatering 1352080 in the oxidizing crystallizers 152 and 156. The liquid phase oxidation reaction of the para-xylene in the reactor 110 is removed from the reactor via the vent 116. The reaction waste gas is sent to the separation unit 330 as a stream 111. The embodiment represented in Fig. 2 is disposed from the separation unit 5 as having a plurality of discs preferably providing about 30 to about 50 theoretical plates. High pressure • distillation column with liquid for reflow via liquid inlet 336. • preferably between about 150 and about 225, respectively. (At the temperature and at a pressure of from about 4 to about 21 kg / _ cm 2 , which is substantially not lower than the temperature and pressure within the oxidation reactor 11 ' 'will be derived from the oxidation reaction of the vapor stream Lead to column 33. 10 As described above, Figure 2 illustrates a preferred embodiment of the invention wherein a portion of the reflux liquid leading to the column comprises a purified mother liquor in which the solid is purified terephthalic acid The separation is carried out in the solid-liquid separation device 230. The column 330 includes, for example, 80 disks (not shown). In the embodiment described in the drawing, about 5 Torr to about 80 disk systems are disposed at the return inlet. At 336, a large amount of separated auto-oxidation anti-15 should be introduced into the solvent acetic acid and water in the pressurized exhaust gas in the column. As described in the next step I, about 10 to about 30 other disk systems are located at the reflux inlet 336, However, it is located under the inlet 344 of the second reflux liquid for washing off the oxidation by-products in the gas phase in the column. As shown in Fig. 2, the distillation column 330 also includes at least one other as a preferred 20 but may be visually required. Reflowing liquid inlet 344 of the selected device to supply a portion of the total reflux Preferably, from about 30 to about 70% of the constant volume flow to the column. The location of the inlet 344 is such that the additional reflux liquid supplied to the column can be directed to one or more theoretical equilibrium stages (and Preferably, from about 2 to about 10 such stages, the disk is spaced from the return inlet 336. In the illustration, the 77 inlets 336 and 344 are preferably separated by about 1 to about 3 disks. Additional reflux may be supplied to the column from the same or different sources as the inlet supplied to inlet 336, the same or different sources including, for example, self-recovering solids containing aromatic carboxylic acids in pure form from the purified liquid reaction mixture. The resulting mother liquor or, as in the embodiment of Figure 2, is recovered in the condensation zone 350 by a portion of the condensate recovered from the distillation column 33 and condensed with the high pressure gas. In the formation illustrated in Figure 2 The reflow supplied to the column 33 at the inlet 344 includes a disk which can provide a balance step, on which a washing of the oxidized by-product of the dioxin can be carried out, Material stream 331 is introduced into the oxidation reactor 110 from the column to purify the mother. a hydrogenated derivative introduced into the liquid. The water in the high pressure gas phase and the solvent acetic acid vapor which are led to the steam column are separated, thereby forming an acetic acid-rich, water-poor liquid phase and a separator output gas under pressure. The acetic acid is separated into a liquid phase from at least 95% by weight of the high pressure steam. The liquid phase preferably comprises from about 60 to about 85% by weight acetic acid and preferably no more than about 25% by weight water. It also contains a small amount of low volatility. The other components of acetic acid such as terephthalic acid and p-xylene oxidation by-products, such as p-quinone and benzoic acid introduced by refluxing the purified mother liquor, and which may also include other components, such as a solvent by-product derived from the oxidation reaction. The high pressure gas obtained from the separation step mainly comprises water vapor and contains unreacted oxygen, a small amount of solvent acetic acid vapor, unreacted p-dimethyl benzene, oxidation by-products, carbon oxides. 'and nitrogen introduced from the air as the source of oxygen for the oxidation reaction. The liquid phase from the separation step in distillation column 330 exits from the lower portion of the column and is preferably returned directly or indirectly to oxidation reactor 110 in stream 331. The step of returning the liquid phase to the oxidation reaction may provide replenishment of the solvent acetic acid to the oxidation reaction, and may convert the by-products condensed from the oxidation gas phase and the by-products recycled from the purified mother liquor to the column into the Desire to reduce the raw materials. The high pressure gas system formed by separating water and acetic acid vapor from the vapor column 330 is removed from the column and sent to a condensing unit 350 including condensers 352 and 362' and a discharge cylinder 372 as shown in Fig. 2. The condensation is preferably carried out at a temperature of from about 40 to about 60 ° C. whereby the liquid condensate water can be recovered in at least one stage. In the embodiment illustrated in the illustration, the condensation is performed by heat exchange between the condensation device 352 using water at a temperature of from about 12 Torr to about not and the effluent from the condenser 352 The stream 361 is sent to a condenser 362 for condensation using cooling water at about 30 to about 40 °C. The gas and liquid effluent from condenser 362 is sent to stream 372 as stream 363 where the aqueous condensate is collected and removed by stream 373, and the condenser effluent from the stream is at its source. 375 discharge. The condensate recovered from the pressurized effluent gas discharged from the distillation column 330 by condensation in the condensing unit is at least about 95% by weight of water and also contains a small amount of organic impurities. The condensate is moved by stream 373 to one or more containers or liquid containers for use in the purification step or for use therein. In the embodiment illustrated in FIG. 2, at least a portion, and preferably a majority of the condensate is transferred to a purification solution supply tank 2〇2 to form the crude product slurry and is sent to the purification reactor 210. The reaction solution is purified. Other purification containers and liquid receiving devices and applications for transferring the condensate include a crystallization vessel 220 used as a cleaning replenishing solvent to replace the purified reaction liquid vaporized by the crystallization device, and a solid-liquid separation used as a washing liquid or a sealing rinsing agent. Device 230. The condensate is also suitable for use outside the purification step of a wash solution such as a reflux to a distillation column 330 and a solvent exchange filter for separating the solid product recovered from the oxidation reaction of the mother liquor. The water as a heat exchange fluid for condensing the pressurized gas from the distillation column 330 is heated by heat exchange in the condensing unit 350 to form a method that can be sent to an energy recovery device, such as the method described in FIG. The steam in the turbine is full 450. As described with reference to Figure 1, the heat exchange fluid can be used at a continuously lower temperature, and the pressurized gas can be condensed by using two or more condensers connected in series. The pressurized gas system is derived from the high pressure gas of the oxidation reaction. The separation of the solvent acetic acid and water in the phase. In such embodiments, the steam produced by self-condensing at reduced temperatures is at a reduced pressure, so that steam can be operated with different heat or energy inputs, effectively at different pressures. Use steam under. The uncondensed off-gas removed from stream 375 from the condensing action comprises a non-condensable component, such as unconsumed oxygen from the oxidation reaction, nitrogen from the air source as the oxygen source for the oxidation reaction, From this air and the carbon oxides of the reactants obtained from the oxidation reaction, and a trace amount of unreacted p-xylene and its oxidation by-products, decyl acetate and methanol, and the bromine agonist used for the oxidation reaction. Methyl bromide formed. In the embodiment illustrated in the illustration, the non-condensed gas is substantially free of water vapor since it is substantially completely condensed into the condensate recovered in the condensing unit. The uncondensed exhaust gas from the condensing device 350 is at a pressure of from about 1 Torr to about 15 kg/cm 2 and can be transferred directly to an energy recovery unit or directly to a pollution control device to remove corrosive energy prior to energy recovery. And flammability types. As described in Figure 2, the non-condensed gas is first treated to remove uncondensed feed material and traces of solvent acetic acid and/or their reaction products remaining in the gas. The uncondensed gas is therefore moved in stream 375 to high pressure absorber 380 to strip p-terphenylbenzene, acetic acid, methanol and methyl acetate at substantial loss of pressure. The absorption column 380 is adapted to receive substantially water-lean gas remaining after condensation and adapted to separate p-xylene, solvent acetic acid, and the like from the oxidation reaction of the gas in contact with the one or more liquid scrubbers. product. The preferred absorber configuration illustrated by the illustration includes a column 380 having a plurality of internal configuration disks or beds or structural packing (not shown) that provide surface for mass transfer between the gas phase and the liquid phase. The inlets (not shown) for adding the scrubber to streams at streams 381 and 383, respectively, are disposed at one or more of the towers, and one or more lower portions. The absorber also includes an upper exhaust port 382' from which the non-condensable component of the inlet gas supplied to the absorber is transferred to the scrubbing gas system under pressure via line 385 and lower outlet 384 for removal. Wherein the component from the gas phase comprises one or more p-xylene, acetic acid, methanol and/or decyl acetate in a liquid-washed liquid acetic acid stream. The bottoms liquid is removed from the lower portion of the column and can be sent to reactor 110 for reuse of the recovered components. The self-condensing device 35 or, in the embodiment as illustrated in Figure 2, the pressurized gas removed from the vent 382 of the high pressure absorber may be sent to the pollution control device 390 for extraction or absorption from the condenser The organic component and carbon monoxide in the pressurized gas are converted into carbon dioxide and water. Preferably, the pollution control device is adapted to receive the second pressurized gas and is selectively heated to promote combustion and to contact the gas with a high temperature stable oxidation catalyst disposed on a porous or other substantially porous support, Thereby, the gas flowing through the device is 1352080 which is qualitatively unaffected by the catalytic oxidation unit. The overhead gas from absorber 380 is sent to a pollution control system 390 comprising a preheater 392 and a catalytic oxidation unit 394. The gas is heated in the preheater to about 250 to 450 ° C and sent to the oxidation unit 394 at a pressure of about 10 to 15 kg / cm 2 , wherein the organic component 5 and by-products are oxidized to A compound suitable for advantageous environmental management" An oxidizing high pressure gas system is supplied from an autocatalytic oxidation unit 394 to an expander 400 connected to a generator 420. The energy source from the oxidized high pressure gas is successfully converted in the expander 4' and the work is converted into a power source by the generator 420. The expanding gas exits the expander, preferably after alkali scrubbing and/or other treatment, and is released to the atmosphere to properly manage the release step. BRIEF DESCRIPTION OF THE DRAWINGS FIG. 1 is a schematic view illustrating an embodiment of a device according to the present invention and used in the method of the present invention; and FIG. 2 is a view illustrating a method according to a preferred embodiment of the present invention and according to the present invention A device, such as the device of Figure 1, and the integration of an apparatus for purifying an aromatic carboxylic acid according to an embodiment of the present invention. [Description of main component symbols] 110...oxidation reactor 11 Bu 115, 154, 158, 19 197, 211, 231, 233, 331, 361, 363, 373, 375, 381, 383... material flow 112, 336 , 338, 344 ·.. inlet 114'332, 345, 382, 384 ... outlet 116.. exhaust port 120.. shaft 152, 156'220... crystallization container 190, 230... solid-liquid separation Device 192.·· mother liquor cartridge 202.. purification solution replenishment container 204.. container 82 1352080 210...purification reactor 380...high pressure absorber 211...material flow line 385...pipe 300...exhaust gas treatment zone 390...contamination control device 330...high pressure distillation column 392...preheater 333,337...disk 394...catalytic oxidation unit 334...exhaust port 400.. Expander 350... Condensing Unit 420... Generators 352, 362... Condenser 372... Release Cartridges... Steam Turbines A, 83

Claims (1)

1352080 mesh photocopy I X. Patent application scope: 1. A method for preparing aromatic tannic acid, which is included in high temperature and high pressure. In the presence of a catalytic composition comprising at least one heavy metal having an atomic weight ranging from about 23 to about 178, the substituted aromatic hydrocarbon is contained in a liquid phase oxidation reaction mixture comprising a monodecanoic acid solvent and water. The feed material is contacted with gaseous oxygen, wherein the substituted aromatic hydrocarbon can be oxidized to a carboxylic acid group, and the high temperature and high pressure can effectively maintain the liquid phase oxidation reaction mixture and form dissolved or suspended in the liquid phase oxidation reaction. Mixture 15 An aromatic carboxylic acid of 20 and an impurity containing an oxidation by-product of the substituted aromatic hydrocarbon, and a high-pressure gas phase containing a solvent monocarboxylic acid, water and a small amount of the substituted aromatic hydrocarbon and by-product; being removed from the reaction zone Transferring the high pressure gas phase to the separation zone' The separation zone has a liquid reflux of the aqueous liquid and can separate the solvent monocarboxylic acid and water in the high pressure gas phase to form a solvent rich monobasic acid water-depleted liquid and a water vapor high pressure gas; Under the treatment of removing organic impurities, the high-pressure gas containing the money (9) from the suspension is transferred to the condensation zone, and the high-pressure gas is condensed to form a condensate containing water and substantially no organic impurities, and the contained liquid is transferred. The high-pressure gas to the condensing zone is non-condensable to the condensing zone exhaust gas under pressure; the aqueous condensate containing substantially no impurity is recovered from the condensing zone and it is suitable for removing organic impurities without additional treatment As at least one aqueous liquid in the method for purifying aromatic citric acid; and feeding the condensate containing water substantially free of organic impurities recovered from the condensation zone to a method for purifying the aromatic carboxylic acid One less step includes: (a) forming an aromatic acid and an impurity dissolved or mixed with an aqueous liquid 84 1352080 _ Patent No. 095112714 Patent Application No. PCT Application No. PCT Application No. And at a high pressure, the purified reaction solution containing the aromatic carboxylic acid and the impurity in the aqueous liquid is contacted with hydrogen in the presence of a hydrogenation catalyst to form a purified liquid reaction mixture; 5 (C) self-contained with the aromatic carboxylic acid and impurities a purified liquid reaction mixture in an aqueous liquid recovering an aromatic carboxylic acid-containing solid purified product having a reduced impurity content; and (d) washing at least one aqueous liquid from a purified liquid reaction containing the aromatic carboxylic acid, impurities, and aqueous liquid The solid pure 10 aromatic carboxylic acid product recovered by the mixture; whereby the aqueous liquid in at least one of the steps of the purification process comprises the condensate containing water substantially free of organic impurities. 2. The method of claim 1, wherein the purification method comprises the steps (a), (b), (c) and (d). The method of claim 2, wherein the purification reaction solution comprises a condensate recovered from the condensation zone and containing substantially no organic impurities. 4. The method of claim 2, wherein the purified reaction liquid reaction mixture comprises the condensate recovered from the condensation zone and containing substantially no organic impurities. The method of claim 2, wherein the solid purified aromatic carboxylic acid product recovered from the purified liquid reaction mixture is a condensate recovered from the condensation zone and containing substantially no organic impurities. washing. 6. The method of claim 5 wherein the aromatic carboxylic acid comprises terephthalic acid and the substituted aromatic hydrocarbon comprises p-xylene. S 85 Patent Application No. 095,112,714, the entire disclosure of which is incorporated herein by reference in its entirety, the entire disclosure of the entire disclosure of the disclosure of the disclosure of the disclosure of the disclosure of the disclosure of the disclosure of the disclosure of It is recovered from the liquid phase oxidation reaction mixture and sent to the method for purifying the aromatic carboxylic acid. 8. The method of claim 2, wherein the impure product containing the aromatic carboxylic acid and the impurity containing the by-product of the substituted aromatic hydrocarbon is recovered from the liquid phase oxidation reaction mixture and sent to the purified aromatic A method of carboxylic acid. 9. The method of claim 1, wherein the aromatic carboxylic acid comprises terephthalic acid and the substituted aromatic hydrocarbon is para-xylene. 10. The method of any one of claims 1 to 9 further comprising: feeding a purified mother liquor to a separation zone, wherein the purification mother liquor comprises aromatics having a reduced impurity content recovered from step (c) A solid purified product of the carboxylic acid, whereby the reflux liquid sent to the separation step comprises the purified mother liquor. 11. The method of claim 10, further comprising recovering the energy from the high pressure condenser exhaust gas from the condensing unit. 12. The method of claim 11, wherein the energy source is recovered by heat exchange with the heat exchange fluid. 13. The method of claim 11, wherein the energy source is recovered by work. 14. The method of claim 11, wherein the high pressure gas system removed from the separation zone is condensed by indirect heat exchange with a heat exchange fluid containing water to generate steam under one or more pressures in the condensation zone. . 15. The method of claim 10, wherein the high pressure gas system of the patent application scope modification 100.8.12 is removed from the separation zone and is subjected to water in the condensation zone under one or more pressures. Indirect heat exchange is performed by a heat exchange fluid that generates steam. The method according to any one of the preceding claims, wherein the high-pressure gas system removed from the separation zone is indirectly exchanged in the condensation zone with a heat exchange fluid containing water to generate steam under one or more pressures. And condensation. 17. A method of preparing an aromatic sharp comprising the steps of: at least one liquid phase deuteration step comprising: at a high temperature and a high pressure, in the reaction zone containing at least one atomic weight ranging from (10) to about 178 In the presence of a heavy gold-like composition, in a liquid phase oxidation reaction mixture containing a single solvent and water, the feed material containing at least one substituted aromatic smoke is contacted with gaseous oxygen, and the aromatic hydrocarbon is taken. The substituent can be oxidized to a nucleus group. The high temperature and high pressure can effectively maintain the liquid phase oxidation reaction mixture, and form the amphoteric acid and reaction by-products in the ship phase oxidation reaction mixture, and the high (four) phase. High pressure gas phase water, solvent single buffer, unreacted substituted aromatic hydrocarbon, oxygen and reaction by-products; and at least one purification step, which is carried out under high temperature and high pressure in the presence of a hydrogenation catalyst containing gold Contacting hydrogen with a purification reaction solution comprising a liquid comprising an aqueous solution of a mixture of aromatics and impurities recovered from the liquid phase oxidation reaction mixture of at least one liquid phase oxidation step to form a money-containing body containing the material Dai people reduce hydrogen a purified liquid reaction mixture of impurities; and at least one exhaust gas treatment step comprising separating from at least one liquid 1-352080 10 Patent Application No. 095,112,714, the application of the solvent in the high pressure gas phase removed from the reaction zone of the phase oxidation step to mono-acid and water to form a solvent-containing monocarboxylic acid liquid and an aqueous unreacted feed material a reaction by-product, a high-pressure gas of oxygen and a small amount of a solvent monocarboxylic acid, and, after the treatment of removing the organic impurities is not required, the step of condensing the water from the pressurized gas and having substantially no organic impurities is at least a step, The utility model comprises a condensate which is condensed from at least one exhaust gas and which is condensed by the high-pressure gas and has substantially no organic impurities, and is sent to at least one purification step without treatment for removing organic impurities. The aqueous liquid in this purification step contains the condensate. 18. The method of claim 17, wherein the at least one purification step comprises at least one of the following additional steps in which the aqueous liquid is used: 0) comprising the liquid reaction mixture from at least one liquid phase oxidation step Recovering a solid product containing an aromatic carboxylic acid and an impurity suspended or dissolved in an aqueous liquid to form the purified reaction solution; (b) forming the aromatic compound recovered from the purified liquid reaction mixture in an aqueous liquid a step of repelling acid and reducing the slurry of the solid product of the impurity content; (c) washing the solid product containing the aromatic carboxylic acid having a reduced impurity content recovered from the purified liquid reaction mixture with an aqueous liquid. 19. The method of claim 17, wherein the at least one purification step comprises modifying the liquid reaction range of the patent application range of the patent application No. 095112, 714, the disclosure of which is incorporated herein by reference. a solid product of the recovered aromatic carboxylic acid and impurities containing oxidation by-products, dissolved in an aqueous liquid to form the purified solution, and the aqueous liquid comprising condensation from the high pressure gas in at least one exhaust gas treatment step Condensate. 5. The method of claim 17, wherein the at least one purification step comprises forming a slurry comprising an aromatic carboxylic acid recovered from the purified liquid reaction mixture and a solid product having a reduced impurity content in an aqueous liquid. And the aqueous liquid comprises condensate condensed from the high pressure gas in at least one of the exhaust gas treatment steps. 10. The method of claim 2, wherein the at least one purification step comprises the step of washing the solid product of the aromatic carboxylic acid having a reduced impurity content recovered by the purified liquid reaction mixture with an aqueous liquid, and the aqueous The liquid contains condensate condensed from the high pressure gas in at least one of the exhaust gas treatment steps. The method of claim 17, wherein the at least one exhaust gas treatment step comprises separating the solvent monocarboxylic acid removed from the reaction zone in the high pressure gas phase in at least one liquid phase oxidation step in a separation unit. Acid and water, wherein the separation apparatus is provided with a reflux liquid containing a purified mother liquor, wherein the aromatic carboxylic acid having a reduced content of impurities is recovered in at least one pure 20 step. 23. The method of claim 17, wherein the purified reaction solution comprises - a crude product in at least one purification step, the crude product is recovered from the liquid phase oxidation reaction mixture in at least one oxidation step and sent The aromatic citric acid and impurities to the purification step. S 89 1352080 5 The invention is the method of claim 17, wherein the aromatic carboxylic acid comprises terephthalic acid and the substituted aromatic hydrocarbon is para-dioxin . 25. A process for the preparation of an aromatic acid comprising the steps of: (a) in the presence of a catalyst composition of a heavy metal having a atomic weight ranging from about 23 to about 178 in the reaction zone at elevated temperature and pressure. And contacting a feed material of the substituted aromatic hydrocarbon containing the aromatic acid retardant with gaseous oxygen in a liquid phase oxidation reaction mixture containing a mono-acid buffer and water, wherein the substituted aromatic hydrocarbon substituent is oxidizable a carboxylic acid group, the high temperature and high pressure can effectively maintain the liquid oxidation reaction mixture, and form an aromatic carboxylic acid and an impurity containing a reaction by-product dissolved or suspended in the liquid phase oxidation reaction mixture, and a high pressure gas phase, The high pressure gas phase contains a solvent monocarboxylic acid, water, unreacted substituted aromatic hydrocarbon, oxygen, and reaction by-products; (b) recovery of aromatic carboxylic acid and reaction by-products from the liquid phase oxidation reaction mixture a solid product of impurities; (c) suspending or dissolving the solid product recovered from the liquid phase oxidation reaction mixture containing the aromatic acid and the reaction by-product impurities in an aqueous liquid to form a purified reaction solution 'At least a portion of the aqueous liquid comprises a condensate condensed according to step (h); (d) contacting the purified solution with hydrogen in the presence of a hydrogenation catalyst at a temperature of south and under pressure to form a purified liquid reaction a mixture; (e) recovering, from the purified liquid reaction mixture, a solid purified product containing a tetracarboxylic acid having a reduced amount of impurities and a liquid containing a combination of a small amount of an oxidized substituted aromatic hydrocarbon, a hydrogenated derivative thereof, or the like Pure 90 1352080 _ _ _ · Patent Application No. 095112714 Patent Application No. 100.8.12 Mother liquor; (f) From step (a) solvent-containing monocarboxylic acid, water vapor, unreacted feed material, The high pressure gas phase of oxygen and a by-product of the liquid phase oxidation reaction is transferred to a separation zone which has a reflux liquid and can substantially separate the monocarboxylic acid solvent and water in the high pressure gas phase 5; (g) under high temperature and high pressure Separating the solvent monocarboxylic acid and water in the high pressure gas phase in the separation zone into a monocarboxylic acid-containing solvent and a water-depleted liquid, and an aqueous, aromatic feed material, a by-product of the oxidation step, and a small amount of a monocarboxylic acid High solvent Pressurizing gas; 10 (h) transferring the high pressure gas from the separation zone to the condensation zone without treatment for removing organic impurities, and transferring heat between the pressurized gas and the heat exchange fluid from the high pressure The gas is condensed into a condensate of water substantially free of organic impurities and forms a high pressure condensing zone exhaust gas; and (i) at least a portion of the condensate from which the pressurized gas in step (h) is condensed 15 is sent to the step ( c). 26. The method of claim 25, wherein the energy source is recovered from the high pressure chilling zone. 27. The method of claim 25, further comprising recovering at least one of the substituted aromatic hydrocarbon, the solvent monocarboxylic acid, and the by-product from the liquid phase reaction from the high pressure condensing zone off-gas. 28. The method of claim 27, further comprising returning at least one of the substituted aromatic hydrocarbon, the solvent monocarboxylic acid recovered from the high pressure exhaust gas, and a by-product obtained from the liquid phase reaction container. 29. The method of claim 27, further comprising the step (h) S 91 1352080 5 10 15 20 Patent Application No. 095112714, the scope of the patent application, the condensed area of the 100, 8.12 I---------------- is recovered containing the substituted aromatic hydrocarbon, the solvent monoacid and After it is obtained from at least one of the by-products of the liquid phase reaction, the high-pressure condensing zone exhaust gas removed from the condensation zone recovers energy. The method of any one of claims 25 to 29, further comprising a step of feeding at least a portion of the purified mother liquor recovered in the step (e) to the separation zone, The reflux liquid supplied thereby to the separation zone contains the purified mother liquor. 31. An apparatus for preparing an aromatic carboxylic acid, comprising: a reaction vessel having a discharge port for removing steam on top of the reactor; separating CK8 monocarboxylic acid gas and water in a high pressure gaseous mixture containing monocarboxylic acid and water a vapor, and a separation device circulated with the reaction vessel to receive the high pressure gas phase removed from the reaction vessel; and circulated with the separation device, adapted to condense at least one portion without treatment for removing organic impurities thereof a high-pressure gas and exchange heat with the heat sink material, and a high-pressure gas extraction energy condensing device received from the separating device; and a condensate for condensing the high-pressure gas to at least one container of the device to purify A member of a family of carboxylic acids. The apparatus of claim 31, further comprising means for circulating with the condensing unit to receive high pressure exhaust gas from the condensing unit and recovering mechanical energy from the high pressure gas. The apparatus of claim 31, wherein the separating apparatus comprises one or more distillation columns. The device of claim 31, wherein the condensing device comprises one or more heat exchangers. 92 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 。 The apparatus of claim 31, wherein the separation device is circulated with the reaction vessel to send the liquid separated in the separation device to the reaction vessel. 37. The device of claim 31, wherein the separation device is Providing at least 20 theoretical equilibrium stages for the separation of Ci.8 mono-rebel gas and water vapor in a high pressure gaseous mixture comprising the monocarboxylic acid and water. 38. The apparatus of claim 31, wherein the separation The apparatus can separate CN8 monocarboxylic acid gas and water vapor in a high pressure gaseous mixture containing 10 of the monocarboxylic acid and water into a liquid phase containing at least 95% of the monocarboxylic acid of the gaseous mixture and a pressurized gas phase containing water. A device for preparing an aromatic tannic acid, comprising: (a) a reaction vessel adapted to a first pressure and adapted to effectively maintain a liquid phase reaction mixture and produce a high pressure gas phase, a liquid phase reaction mixture comprising a monocarboxylic acid solvent and water, subjecting the aromatic feed material to a liquid phase oxidation reaction with gaseous oxygen, and comprising at least one exhaust port for removing the pressurized gas phase from the reaction vessel; (b) - a separation device adapted to be substantially no less than 20 second pressure of the first pressure and comprising at least one high pressure gas circulated with the reactor vessel for receiving at least one vent from the reactor vessel a gas inlet of the phase, at least one liquid inlet for delivering reflux liquid to the apparatus, at least one gas outlet for removing pressurized gas from the apparatus, and at least one liquid for removing liquid material flow from the apparatus S 93 1352080 . 5 Patent Application No. 95,511 Solvent monocarboxylic acid and water, thereby forming a solvent-containing monocarboxylic acid and a substantially anhydrous liquid stream and a high pressure gas containing water and a substantially solvent-free monocarboxylic acid (C) a condensing unit comprising at least one gas inlet for receiving a high pressure gas removed from at least one gas outlet of the separation device to be removed to remove organic impurities; An exchange member for transferring heat from the high pressure gas to the heat exchange fluid in the condensing device, thereby condensing the liquid condensate from the high pressure gas and forming a heat exchange fluid having an increased temperature or pressure; at least one for Removing an outlet of high pressure exhaust gas from the condensing unit; and at least one outlet for removing condensate from the condensing unit; and (d) - condensing liquid for removing 15 from at least one outlet of the condensing unit A device for delivery to at least one container of an aromatic carboxylic acid purification unit. 40. The apparatus of claim 39, wherein the fractionation zone of the separation device provides at least 20 theoretical plates for the separation of water and a mixture of monocarboxylic acids for use in water and monocarboxylic acid. . 41. The apparatus of claim 39, wherein the separation device separates C!-8 monocarboxylic acid gas and water vapor in a high pressure gaseous mixture containing 20 of the monocarboxylic acid and water into a gaseous mixture. At least 9 5 % of the liquid phase of the monocarboxylic acid and the pressurized gas phase containing water. 42. The device of claim 39, wherein the separation device comprises one or more columns, wherein the fractionation zone comprises a plurality of disks or a plurality of structural fillers. 94 1352080 Patent Application No. 096112714 .12 bed. 43. The device of claim 39, wherein the separation device comprises one or more columns, wherein the fractionation zone comprises at least one disk and at least one structured packing bed. The device of any one of claims 39 to 43 wherein at least one of the outlets for removing liquid from the condensing device is used for direct or Means for indirect transfer of liquid to at least one of the following devices: (e) a slurry tank suitable for dissolving a solid containing aromatic carboxylic acid in an aqueous liquid, (f) suitable for high temperature and high pressure Hydrogenating a purification reaction vessel containing a solution of an aromatic carboxylic acid dissolved in an aqueous liquid, (g) a liquid reaction mixture obtained by a hydrogenation reaction at a high temperature and a high pressure to recover a condensed solution containing an aqueous solution a solution of a family carboxylic acid, a solid containing an aromatic carboxylic acid and a small amount of impurities, and a crystallization vessel substantially free of the aromatic mother carboxylic acid purification mother liquor, and (h) suitable for separating the aromatic carboxylic acid and a small amount from the 15 purification mother liquor Solid-liquid separation device for solids of impurities. S 95