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WO2009081458A1 - Procédé de filtration d'une boue de cristallisation - Google Patents

Procédé de filtration d'une boue de cristallisation Download PDF

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Publication number
WO2009081458A1
WO2009081458A1 PCT/JP2007/074518 JP2007074518W WO2009081458A1 WO 2009081458 A1 WO2009081458 A1 WO 2009081458A1 JP 2007074518 W JP2007074518 W JP 2007074518W WO 2009081458 A1 WO2009081458 A1 WO 2009081458A1
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WO
WIPO (PCT)
Prior art keywords
washing
filtering
washed
crystals
temperature
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Ceased
Application number
PCT/JP2007/074518
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English (en)
Japanese (ja)
Inventor
Tokuaki Hara
Hiroyuki Toyoshima
Hatsutaro Yamazaki
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
Hitachi Ltd
Original Assignee
Hitachi Plant Technologies Ltd
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by Hitachi Plant Technologies Ltd filed Critical Hitachi Plant Technologies Ltd
Priority to CN2007801019499A priority Critical patent/CN101903072B/zh
Priority to PCT/JP2007/074518 priority patent/WO2009081458A1/fr
Publication of WO2009081458A1 publication Critical patent/WO2009081458A1/fr
Anticipated expiration legal-status Critical
Ceased legal-status Critical Current

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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C63/00—Compounds having carboxyl groups bound to a carbon atoms of six-membered aromatic rings
    • C07C63/14—Monocyclic dicarboxylic acids
    • C07C63/15—Monocyclic dicarboxylic acids all carboxyl groups bound to carbon atoms of the six-membered aromatic ring
    • C07C63/24—1,3 - Benzenedicarboxylic acid
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D33/00—Filters with filtering elements which move during the filtering operation
    • B01D33/06—Filters with filtering elements which move during the filtering operation with rotary cylindrical filtering surfaces, e.g. hollow drums
    • B01D33/073—Filters with filtering elements which move during the filtering operation with rotary cylindrical filtering surfaces, e.g. hollow drums arranged for inward flow filtration
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D33/00—Filters with filtering elements which move during the filtering operation
    • B01D33/06—Filters with filtering elements which move during the filtering operation with rotary cylindrical filtering surfaces, e.g. hollow drums
    • B01D33/073—Filters with filtering elements which move during the filtering operation with rotary cylindrical filtering surfaces, e.g. hollow drums arranged for inward flow filtration
    • B01D33/09—Filters with filtering elements which move during the filtering operation with rotary cylindrical filtering surfaces, e.g. hollow drums arranged for inward flow filtration with surface cells independently connected to pressure distributors
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D33/00—Filters with filtering elements which move during the filtering operation
    • B01D33/44—Regenerating the filter material in the filter
    • B01D33/48—Regenerating the filter material in the filter by flushing, e.g. counter-current air-bumps
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D33/00—Filters with filtering elements which move during the filtering operation
    • B01D33/58—Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element
    • B01D33/60—Handling the filter cake in the filter for purposes other than for regenerating the filter cake remaining on the filtering element for washing
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D9/00—Crystallisation
    • B01D9/0059—General arrangements of crystallisation plant, e.g. flow sheets
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C63/00—Compounds having carboxyl groups bound to a carbon atoms of six-membered aromatic rings
    • C07C63/14—Monocyclic dicarboxylic acids
    • C07C63/15—Monocyclic dicarboxylic acids all carboxyl groups bound to carbon atoms of the six-membered aromatic ring
    • C07C63/26—1,4 - Benzenedicarboxylic acid

Definitions

  • the present invention relates to a filtration method for efficiently performing continuous reduced pressure rotary filtration in which crystallization slurry is repeatedly subjected to steps of suction filtration, crystal washing, suction devolatilization, and crystal peeling in order, and particularly for recovering crystals by continuous reduced pressure rotary filtration. Further, the present invention relates to a filtration method capable of suppressing clogging of a filter medium (filter cloth) and allowing continuous filtration and washing treatment of crystals for a long time.
  • the oxidation reaction product is reduced in pressure and reduced in temperature by releasing (flashing) the solvent from the pressure and temperature of the solvent. Then, after obtaining a product slurry in which crystals are precipitated, the crystallized slurry is filtered and washed by a continuous vacuum rotary filtration method to recover aromatic dicarboxylic acid crystals.
  • the above-mentioned crude aromatic dicarboxylic acid crystal obtained as another method is dissolved in water, and through a hydrorefining process, the product is similarly reduced in pressure and cooled to obtain a product slurry in which crystals are precipitated. After that, the crystallization slurry is filtered and washed by a continuous reduced pressure rotary filtration method to recover crystals.
  • the product obtained by the reaction is reduced in pressure and cooled to obtain a slurry of the product from various solvents in which crystals are precipitated, and then the crystallization slurry is filtered and washed by a continuous reduced pressure rotary filtration method.
  • a method for recovering the crystal product produced by the reaction is often carried out in the production of organic chemical industrial products.
  • the filter cloth (filter material) is laid in a cylindrical shape or a belt shape, and the steps of suction filtration, crystal washing, suction drainage, and crystal peeling are repeated in order while rotating or moving the crystallization slurry. It is performed by a continuous vacuum rotary filtration / cleaning method.
  • the filtration / washing process is stopped, the filter cloth is washed / dissolved with an alkaline solution such as an aqueous solution of caustic soda to eliminate clogging of the filter cloth, and the filtration / washing operation is restarted. Therefore, when recovering crystals from the crystallization slurry by a continuous reduced pressure rotary filtration method, an inefficient treatment operation for stopping the filtration / washing treatment as described above has been forced.
  • Patent Document 1 Japanese Patent Laid-Open No. 1-2996178
  • Patent Document 2 Japanese Patent Laid-Open No. 2004-231636
  • Patent Document 3 Japanese Patent Application Laid-Open No. 2006-265124
  • the crystallization slurry is cooled to a temperature (about 90 ° C.) below the boiling point (under atmospheric pressure) of the solvent by boiling under reduced pressure or a heat exchanger, and then suction filtration is performed.
  • a method has been proposed in which the evaporation of the solvent on the filter cloth is suppressed and the clogging of the mesh is suppressed.
  • Patent Document 4 Japanese Patent Application Laid-Open No. 2002-203264 discloses a method for completely removing crystal particles from a filter cloth and eliminating clogging by supplying a vapor of a solvent component to a blowing gas for crystal peeling. Has been proposed, and methods for efficient treatment with a long continuous filtration and washing time have been devised and proposed.
  • Patent Document 1 it is necessary to pressurize the inside of the outer casing (casing) of the rotary filter, and not only the filter body but also incidental facilities such as a supply pump and a filtrate tank become heavy pressure-resistant facilities and reduce the equipment cost. Invite rise. Further, it is necessary to improve the equipment for smoothly transferring the collected wet crystals from under pressure to a dryer at normal pressure (atmospheric pressure) (Japanese Patent Application Laid-Open No. 11-179115, Special Table 2003-519205). Increases equipment costs.
  • Patent Document 4 in order to supply the vapor of the solvent component to the blowing gas for performing crystal peeling, moisture is given to the crystal dried in the previous step, and the wetness of the recovered crystal increases, and the subsequent drying step The load of increases.
  • the present invention provides a filtration method capable of suppressing clogging of a filter medium (filter cloth) and recovering continuous crystal filtration and washing for a long time when recovering crystals by continuous reduced pressure rotary filtration. is there. Further, even in a vacuum rotary filter performed under normal pressure (atmospheric pressure), the filter cloth is prevented from being clogged with crystallized particles, and can be continuously operated for a long time.
  • the present invention relates to a method for recovering crystals by continuous reduced pressure rotary filtration in which a slurry comprising crystals and a solvent is repeatedly filtered, washed, and peeled in order, and in the washing step, at least a temperature accompanied by vapor generation is overheated.
  • the crystal is washed using the washed solvent.
  • the continuous type is obtained from the crystallization slurry obtained by reducing the pressure and lowering the temperature.
  • the crystal is washed using a washing solvent heated to at least a temperature accompanied with vapor generation in the washing step.
  • the aromatic hydrocarbon is a dialkyl aromatic hydrocarbon composed of para-xylene or meta-xylene
  • the produced aromatic carboxylic acid is composed of terephthalic acid or isophthalic acid.
  • the crystal is washed with acetic acid heated to 120 ° C. or higher, preferably 130 ° C. or higher, more preferably 140 ° C. or higher as the cleaning solvent.
  • the crystal is washed using a washing solvent heated to a temperature at which the rate of vapor generation is preferably about 7% or more, more preferably about 14% or more. .
  • the clogging of the filter cloth is suppressed by washing the filtered crystals with at least a superheated washing solvent accompanied by vapor generation.
  • the filtration and washing operation can be performed continuously for a long time, and the crystal recovery operation can be performed under normal pressure.
  • FIG. 1 is a flow chart
  • FIG. 2 schematically shows a filtration section of the continuous vacuum rotary filter 2 therein.
  • the filter 2 is installed such that a cylindrical rotating body 11 having a filter surface with a filter medium (filter cloth) on the outer surface is rotated in the filter 2 so as to rotate in the clockwise direction.
  • the partition wall is fixed so as not to rotate. While the rotating body 11 rotates in the clockwise direction, first, the crystallization slurry retained in the bottom 12 of the filter 2 in the filtration step is sucked from the filtration region 13 inside the rotating body 11 by the suction of the rotating body 11. A crystal grain layer is formed on the outer surface of the substrate. This is done by sucking the mother liquor of the crystallization slurry that has entered the filtration zone 13 into the filtrate tank 3 of FIG.
  • the rotating surface 11 rotates while the filtration surface on which the crystal particle layer is formed is separated from the immersion of the crystal slurry, and rises up the cleaning / drainage zone 14 to reach the upper part.
  • the cleaning liquid is supplied from the outside of the rotating body 11 to the upper surface of the crystal particle layer by a method such as spraying and spraying, and the cleaning liquid that has passed through the rotating body 11 passes through the cleaning / drainage area 14 in the cleaning drainage tank of FIG. 4 sucked.
  • the cleaning liquid pushes out the residual mother liquor (slurry mother liquid) adhering to the surface of the crystal particle layer and the mesh of the filter medium, and is removed to the cleaning / drainage zone 14 inside the rotating body 11. To do.
  • the cleaning liquid (acetic acid) supplied by a method such as spraying and spraying is heated and controlled by the heater E-1 so that it is heated to at least a temperature exceeding the boiling point (118 ° C.) and accompanied by steam generation.
  • the superheated cleaning liquid is sprayed on the surface of the filtration (crystal particle) layer with steam.
  • the superheating temperature in the heater E-1 is preferably overheated to a temperature exceeding the boiling point (118 ° C.) with acetic acid, but by overheating to 120 ° C. or more, an improvement effect in suppressing clogging appears. Further, it is more preferable to overheat to about 130 ° C.
  • heating of the cleaning liquid is considered to require at least the presence of the cleaning liquid at the time of introduction and spraying (the liquid disappears if it is overheated). I think it's not good.
  • the crystal particle layer further rotates together with the rotator 11, and the internal suction is continued while moving from the upper part of the cleaning / dehydrating zone 14 to the right side, and the residual cleaning liquid in the crystal particle layer is the atmospheric vapor on the surface of the crystal particle layer. Then, the liquid is sucked together with the gas, and the liquid removal is performed while suppressing the evaporation of the residual cleaning liquid. By suppressing the evaporation, it is possible to suppress the precipitation of the solute of the residual cleaning liquid on the mesh of the filter cloth.
  • the crystal particle layer drained as described above is further rotated and moved to the crystal exfoliation region 15, and in the exfoliation region 15, an inert gas is sprayed from the inside of the rotating body 11 by the supply pulser M-2. Is removed from the rotating body 11, falls down the crystal discharge pipe 16, and is collected as wet terephthalic acid crystals in the screw discharge machine M- 1. Since the exfoliated crystals are heated to near the boiling point of the cleaning solvent, gas blowing in the exfoliation zone 15 causes evaporation of the residual cleaning liquid in the crystal particle layer, resulting in a decrease in wetness.
  • the crystals from the screw discharger M-1 are supplied to the dryer 8 and become terephthalic acid crystals that are sufficiently dried.
  • the rotating body 11 from which the crystal has been peeled enters the slurry retaining portion of the bottom 12 while further rotating, starts suction filtration again, and is repeatedly filtered, washed and drained.
  • the filtrate (mother liquid) sucked into the rotary body 11 by suction filtration in the process of filtering and washing on the rotary body filtration surface is almost recovered in the filtrate tank 3, and the solvent recovery process and oxidation are performed. It is recycled for reuse in the reaction.
  • the vapor components not collected in the filtrate tank 3 are condensed in the upper cooler E-2, and the condensed liquid is collected and refluxed in the gas-liquid separation tank 5.
  • the non-condensable gas component that has not been condensed is sucked into the vacuum pump M-3 and circulated, but excess gas is discharged out of the system.
  • the cleaning waste liquid sucked into the rotating body 11 by the cleaning is recovered in the cleaning drain tank 4 like the slurry filtrate, and then the cooler E-3 ⁇ the gas-liquid separator 6 ⁇ the vacuum pump
  • the condensate is collected and the non-condensable gas is circulated through the path M-3. Since the vacuum pump M-3 is expected to contain condensable vapor, it is preferable to use a liquid ring pump for suction and exhaust.
  • the outer cover of the filter 2 is usually sealed and sealed with an inert gas or the like. is there. Therefore, it is sealed with a non-condensable gas that is sucked together with the filtration / cleaning liquid and circulated through the vacuum pump M-3, and the supply / replenishment of the gas is mainly performed with a blowing gas for crystal peeling.
  • the terephthalic acid crystallization slurry When continuously collecting terephthalic acid crystals from the terephthalic acid crystallization slurry using the crystallization slurry filtration / separation system as described above, first, the high-temperature, high-pressure reaction product is released (flash) or the like. The terephthalic acid crystallization slurry whose pressure has been lowered and lowered is transferred to the slurry supply tank 1. In the slurry supply tank 1, the crystallization slurry is supplied to the bottom of the filter 2 while being circulated by an external pump.
  • the crystallization slurry at the bottom of the filter 2 is suction filtered at the bottom of the cylindrical rotating body 11 by suction from the inside of the cylindrical rotating body 11, and the excess slurry overflows (overflows) and is returned to the slurry supply tank 1.
  • the retained liquid level (filtrate level) of the slurry is maintained.
  • the supplied cleaning liquid (acetic acid) is heated and controlled so as to be heated to at least a temperature exceeding the boiling point (118 ° C.) and generating steam in the heater E-1.
  • This heating is based on the knowledge obtained by the present inventors, that is, the crystal cleaning solvent (cleaning liquid) is heated to a temperature at which vapor generation occurs at least above the boiling point of the cleaning liquid, and the cleaning liquid is released. Based on the knowledge that clogging due to crystals in the filter cloth can be suppressed by supplying (flush) and washing the filtration (crystal particle) layer as a mixed phase flow of high-temperature (liquid boiling point) vapor and liquid vapor. ing.
  • the crystallization slurry is supplied to the filter 2 and suction filtered in the filter zone 13, and then the cleaning solution heated in the cleaning step in the cleaning zone 14 is supplied in a flash form.
  • the filtration (crystal particle) layer is washed at a high speed as a mixed-phase flow of vapor and liquid having an increased capacity accompanied by high-temperature (liquid boiling point) vapor.
  • the generation of solvent vapor in the filtrate and washing waste liquid is suppressed, and the solute in the network is Clogging due to precipitation is suppressed.
  • the introduction of the cleaning liquid in the pressure release (flush) state by overheating supply causes the casing of the filter 2 to be filled with high-temperature (liquid boiling point) vapor (wet gas), and the filter cloth sucks the slurry.
  • high-temperature atmospheric vapor wet gas
  • the filter cloth sucks the slurry.
  • the temperature at which the cleaning liquid is heated is heated to a pressure exceeding the boiling point, and the pressure is released (flushed) and sprayed to the cleaning area in the atmospheric pressure state.
  • the high-temperature (boiling point) vapor generated at the time can exist in the atmosphere (in the filter casing) on the surface of the crystal particle layer, so that the period until clogging (clogging time) is improved. become.
  • the clogging time is improved if several percent of the supplied cleaning liquid generates steam, and long-term continuous operation (the clogging time of the terephthalic acid-producing slurry at about 90 ° C. is about 10 days or more) is achieved. Therefore, it has been found that the cleaning solution to be supplied is heated to a temperature at which about 7% (calculated) or more of steam is generated. And it is suggested that it is sufficient to overheat to a temperature at which steam with a temperature of overheating of about 13% (calculated) or more is generated.
  • the continuous vacuum rotary filter 2 under normal pressure that has been used in the past is implemented by the fact that a heater and a flash valve are installed in the supply line of the cleaning solvent. It is possible to operate the filter continuously for a long time with an easy improvement in terms of equipment.
  • it is not limited to application to crystallization slurry from the production of aromatic dicarboxylic acid by oxidation reaction in acetic acid solvent, and there are many such as crystallization slurry of aromatic dicarboxylic acid crystal from water solvent The same method can be applied to crystallization slurries of organic industrial chemicals.
  • the crystal particle layer on the filter cloth that has been washed and sucked and drained is peeled off by blowing (blowing) gas from the inside of the filter cloth.
  • a peeling method such as gas blowing using a shock wave (pulsar) can be used. It is done.
  • steam is not mixed compared with the method of supplying the solvent vapor
  • the crystal particle layer is maintained at a high temperature (solvent boiling point) during the cleaning / dehydrating process, there is also a decrease in wetness due to evaporation of the wet cleaning liquid remaining in the process of crystal peeling and crystal discharging. .
  • a vacuum rotary filter in addition to the vacuum rotary cylindrical filter 2 shown in FIGS. 1 and 2 called a rotary vacuum filter (RVF), a vacuum horizontal filter called a belt filter is used.
  • a filter such as a band type filter may be used in which the filter cloth moves and suction filtration, crystal washing, suction liquid removal, and crystal peeling are repeated in this order for continuous filtration and washing.
  • the slurry containing the crude terephthalic acid crystals flash-crystallized from the crystallization tank to the slurry supply tank 1 (FIG. 1), and filtered and washed with RVF2 according to the filtration and washing process described in the above embodiment and the flow of FIG. 1 to collect wet crystals. And after drying with dryer 8, it implemented by the method of collect
  • the terephthalic acid-containing slurry in the slurry supply tank 1 supplied to the RVF 2 contains about 33 wt% terephthalic acid crystals in the reaction solvent (acetic acid) and has a temperature of about 90 ° C.
  • RVF2 for crystal recovery uses a Young-type reduced-pressure rotating cylindrical filter (manufactured by Bird Co., USA), and rotates the cylindrical rotating body 11 under normal pressure (gas seal 100 mmAq or less) at a speed of 4.5 RPM.
  • the vacuum pump E-3 vacuum degree: about 400 mmHg
  • suction filtration, crystal washing and suction drainage are performed.
  • a shock wave maximum of about 0.2 Kg / cm 2 G.
  • the acetic acid cleaning liquid is heated (superheated) to a predetermined temperature by the heater E-1, and is introduced into the upper part of the cleaning zone 14 as a liquid (comparative example) or a flash vapor mixed phase (Examples 1 to 4). Washing was performed.
  • the acetic acid for washing was heated through a heater E-1 using a pressurized metering pump (discharge pressure of about 5 Kg / cm 2 G), and adjusted and supplied at a ratio of about 0.6 weight to the supplied terephthalic acid crystals. Therefore, the supply of the cleaning liquid to the RVF 2 is a pressure release supply through the flash valve 17 from under pressure.
  • Example 1 the temperature of the supplied acetic acid was overheated (120 ° C.) exceeding the boiling point on the basis of a comparative example (temperature conventionally practiced) conducted at the same temperature as the supplied slurry (temperature without steam generation).
  • Example 2 it was found that the clogging time was improved.
  • the clogging time was greatly improved at 130 ° C. (Example 2 / generated steam: about 7% in calculation), which is considered to have significant steam generation, but 140 ° C. or higher (Examples 3 and 4 / generation) Vapor: 14% or more calculated) was almost unchanged.
  • the terephthalic acid wet crystals obtained from RVF2 were collected at the receiving port of the crystal screw discharger M-1, and the wet rate (weight loss on drying wt%) of the recovered crystals and the ash content (ppm) as the contained inorganic substance were measured.
  • 3 shows the relationship with the washing acetic acid temperature as a table. As a result, both tended to improve as the temperature of the washing acetic acid increased.
  • FIG. 4 is a graph showing the characteristics of Examples 1 to 4 shown in FIG. 3.
  • the horizontal axis represents acetic acid temperature as a cleaning solution
  • the vertical axis represents clogging time. Judging from this graph and FIG. 3, in the cleaning step, it is clogged that the crystal is cleaned using acetic acid heated to 120 ° C. or higher, preferably 130 ° C. or higher, more preferably 140 ° C. or higher as the cleaning solvent.
  • the time can be lengthened. It can also be seen that the longest clogging time and a low wetting rate are obtained at 140 ° C. or higher, but are efficiently obtained at around 140 ° C. from the viewpoint of energy saving.
  • FIG. 5 is a characteristic diagram plotting Examples 1 to 4.

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Chemical Kinetics & Catalysis (AREA)
  • Crystallography & Structural Chemistry (AREA)
  • Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
  • Filtration Of Liquid (AREA)

Abstract

Dans l'art antérieur, les cristaux sont séparés et récupérés à partir d'une boue de cristallisation par des étapes de filtration par aspiration, de lavage des cristaux et d'élimination des liquides, à l'aide d'une machine de filtration rotative à vide. Dans l'étape de lavage, une partie du solvant d'un filtrat ou d'un liquide de lavage est évaporée et refroidie par l'aspiration du liquide de lavage, provoquant ainsi la cristallisation du soluté sur la maille du tissu filtrant appliqué. Par conséquent, la maille du tissu filtrant est colmatée par des micrograins cristallins, ce qui rend difficile la formation d'une couche de filtration (grain cristallin) par filtration par aspiration. En outre, le passage du liquide de lavage devient non satisfaisant, empêchant ainsi la poursuite d'une filtration/d'un lavage en continu. La présente invention concerne donc un procédé de filtration rotative qui inhibe le colmatage du tissu filtrant et qui permet une poursuite prolongée de la filtration/du lavage. Le colmatage de microcristaux sur la maille du tissu filtrant a été inhibé par chauffage du liquide de lavage à l'aide d'un élément chauffant afin d'effectuer une surchauffe jusqu'à au moins la température (pression) permettant la formation de vapeur et par alimentation du liquide de lavage sous forme de flux à phase mixte entraîné par la vapeur produite dans une région de lavage au sein de la machine de filtration dans l'étape de lavage. Comme solvant de lavage, de l'acide acétique surchauffé à 120 °C ou plus, de préférence à 130 °C ou plus, mieux encore à 140 °C ou plus, est utilisé. Le solvant de lavage est surchauffé de préférence à la température pour environ 7 % ou plus de formation de vapeur, mieux encore à la température pour environ 14 % ou plus de formation de vapeur.
PCT/JP2007/074518 2007-12-20 2007-12-20 Procédé de filtration d'une boue de cristallisation Ceased WO2009081458A1 (fr)

Priority Applications (2)

Application Number Priority Date Filing Date Title
CN2007801019499A CN101903072B (zh) 2007-12-20 2007-12-20 结晶浆料的过滤方法
PCT/JP2007/074518 WO2009081458A1 (fr) 2007-12-20 2007-12-20 Procédé de filtration d'une boue de cristallisation

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