CN1283604C - Method for producting absolute ethyl alcohol - Google Patents
Method for producting absolute ethyl alcohol Download PDFInfo
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- CN1283604C CN1283604C CN 200510013319 CN200510013319A CN1283604C CN 1283604 C CN1283604 C CN 1283604C CN 200510013319 CN200510013319 CN 200510013319 CN 200510013319 A CN200510013319 A CN 200510013319A CN 1283604 C CN1283604 C CN 1283604C
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- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 title claims abstract description 248
- 238000000034 method Methods 0.000 title claims abstract description 31
- 238000011084 recovery Methods 0.000 claims abstract description 37
- 238000004519 manufacturing process Methods 0.000 claims abstract description 34
- 239000002994 raw material Substances 0.000 claims abstract description 31
- 239000002808 molecular sieve Substances 0.000 claims abstract description 27
- URGAHOPLAPQHLN-UHFFFAOYSA-N sodium aluminosilicate Chemical compound [Na+].[Al+3].[O-][Si]([O-])=O.[O-][Si]([O-])=O URGAHOPLAPQHLN-UHFFFAOYSA-N 0.000 claims abstract description 27
- 239000007788 liquid Substances 0.000 claims abstract description 26
- 230000008929 regeneration Effects 0.000 claims abstract description 7
- 238000011069 regeneration method Methods 0.000 claims abstract description 7
- 238000010438 heat treatment Methods 0.000 claims description 7
- 229960004756 ethanol Drugs 0.000 claims 11
- 229960000935 dehydrated alcohol Drugs 0.000 claims 3
- CSDREXVUYHZDNP-UHFFFAOYSA-N alumanylidynesilicon Chemical compound [Al].[Si] CSDREXVUYHZDNP-UHFFFAOYSA-N 0.000 claims 1
- 238000001179 sorption measurement Methods 0.000 abstract description 31
- 230000018044 dehydration Effects 0.000 abstract description 28
- 238000006297 dehydration reaction Methods 0.000 abstract description 28
- 239000007791 liquid phase Substances 0.000 abstract description 5
- 239000012071 phase Substances 0.000 abstract description 5
- 238000003860 storage Methods 0.000 abstract description 4
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 22
- 238000003795 desorption Methods 0.000 description 11
- 239000003463 adsorbent Substances 0.000 description 9
- 238000005516 engineering process Methods 0.000 description 7
- 238000000605 extraction Methods 0.000 description 4
- 239000000446 fuel Substances 0.000 description 4
- 238000000926 separation method Methods 0.000 description 4
- 239000002904 solvent Substances 0.000 description 4
- UHOVQNZJYSORNB-UHFFFAOYSA-N Benzene Chemical compound C1=CC=CC=C1 UHOVQNZJYSORNB-UHFFFAOYSA-N 0.000 description 3
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 238000010533 azeotropic distillation Methods 0.000 description 3
- 238000001704 evaporation Methods 0.000 description 3
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 2
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000008020 evaporation Effects 0.000 description 2
- 229910052680 mordenite Inorganic materials 0.000 description 2
- 238000010926 purge Methods 0.000 description 2
- XDTMQSROBMDMFD-UHFFFAOYSA-N Cyclohexane Chemical compound C1CCCCC1 XDTMQSROBMDMFD-UHFFFAOYSA-N 0.000 description 1
- 150000001299 aldehydes Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 238000012824 chemical production Methods 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 239000002537 cosmetic Substances 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 description 1
- 238000000855 fermentation Methods 0.000 description 1
- 230000004151 fermentation Effects 0.000 description 1
- 239000001760 fusel oil Substances 0.000 description 1
- 239000012535 impurity Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 238000004886 process control Methods 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000002699 waste material Substances 0.000 description 1
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- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
本发明是涉及无水乙醇的生产方法。采用无水乙醇液相进料生产新方法，解决了远离乙醇精馏脱水装置的无水乙醇分子筛吸附脱水生产装置，需单独设置淡酒回收系统的难题，使得非酒精生产企业可以低投资和低成本实现无水乙醇的生产。本发明采用的主要设备是乙醇回收塔、吸附器、冷凝器、再沸器和淡酒预热器等，将酒精浓度为90～99%体积比的高浓度酒精的原料液、酒精浓度为1%～90%体积比的低浓度的酒精原料液和分子筛再生过程产生的淡酒送入乙醇回收塔。流程先进合理，设备功能多，热量利用合理，实现了无水乙醇液相进料分子筛吸附脱水生产工艺与气相进料工艺相近的蒸汽消耗量。降低了无水乙醇产品的生产、运输和储存成本。
The present invention relates to the production method of absolute ethanol. The new production method of anhydrous ethanol liquid-phase feed has solved the problem that the anhydrous ethanol molecular sieve adsorption and dehydration production device far away from the ethanol rectification and dehydration device needs to set up a light alcohol recovery system separately, so that non-alcohol production enterprises can reduce investment and cost. The cost realizes the production of anhydrous ethanol. The main equipment that the present invention adopts is ethanol recovery tower, adsorber, condenser, reboiler and light wine preheater etc., the raw material liquid of the high-concentration alcohol that alcohol concentration is 90～99% volume ratio, alcohol concentration is 1 The low-concentration alcohol raw material liquid with a volume ratio of % to 90% and the light alcohol produced during the molecular sieve regeneration process are sent to the ethanol recovery tower. The process is advanced and reasonable, the equipment has many functions, and the heat utilization is reasonable. The steam consumption of the anhydrous ethanol liquid-phase feed molecular sieve adsorption dehydration production process is similar to that of the gas-phase feed process. The production, transportation and storage costs of absolute ethanol products are reduced.
Description
技术领域Technical field
本发明是涉及无水乙醇的生产方法。The present invention relates to the production method of absolute ethanol.
背景技术 Background technique
无水乙醇主要作为燃料(该用途的无水乙醇也称为燃料乙醇)、电子元件制造、高级化妆品的溶剂和化工生产原料等广泛应用。Absolute ethanol is mainly used as fuel (anhydrous ethanol for this purpose is also called fuel ethanol), electronic component manufacturing, solvent for high-grade cosmetics, and raw materials for chemical production.
无水乙醇生产过程一般以乙醇含量为5～30％体积比的发酵醪液为原料，通过精馏和特殊分离两个操作过程得到。采用精馏技术脱除大部分水、醛和杂醇油等杂质，得到水含量小于5％体积比的接近乙醇与水共沸组成的高浓度乙醇，再通过共沸萃取精镏或吸附等特殊分离手段将乙醇中的水脱除得到无水乙醇，产品标准参见无水乙醇标准GB678-90和燃料乙醇标准GB18350-2001。在无水乙醇生产过程中，产品精制脱水过程控制着产品收率及公用工程消耗。The production process of anhydrous ethanol generally uses fermentation mash with an ethanol content of 5-30% by volume as raw material, and is obtained through rectification and special separation. Use rectification technology to remove most of the impurities such as water, aldehydes and fusel oil, and obtain high-concentration ethanol with a water content of less than 5% volume ratio, which is close to the azeotropic composition of ethanol and water, and then use special methods such as azeotropic extraction, rectification or adsorption The separation method removes the water in the ethanol to obtain absolute ethanol. For product standards, refer to the absolute ethanol standard GB678-90 and the fuel ethanol standard GB18350-2001. In the production process of absolute ethanol, the product refining and dehydration process controls the product yield and utility consumption.
传统的无水乙醇工业生产方法，对于高浓度乙醇进一步脱水过程主要是基于精馏技术的分离过程，即共沸精馏。在共沸精馏方面，苯是工业化无水乙醇生产过程中使用最多的溶剂，其它溶剂还有环己烷、戊烷、乙醚、乙二醇等。无水乙醇脱水采用共沸精馏工艺能耗较高，蒸汽单耗高达1.6吨蒸汽/吨乙醇产品，而且设备投资大，操作不稳定。In the traditional industrial production method of absolute ethanol, the further dehydration process of high-concentration ethanol is mainly based on the separation process of rectification technology, that is, azeotropic distillation. In terms of azeotropic distillation, benzene is the most used solvent in the production process of industrial anhydrous ethanol, and other solvents include cyclohexane, pentane, ether, ethylene glycol, etc. The azeotropic distillation process for dehydration of anhydrous ethanol has high energy consumption, and the unit steam consumption is as high as 1.6 tons of steam/ton of ethanol product, and the equipment investment is large and the operation is unstable.
当代迅速发展的无水乙醇主流生产方法，对于高浓度乙醇进一步脱水过程主要采用分子筛吸附脱水方法。首先通过精馏过程得到水含量接近共沸组成的高浓度乙醇气体，乙醇气体通过分子筛气相吸附脱除乙醇中的残余水份获得无水乙醇产品。并通过变压和变温等手段实现吸附剂的再生。The mainstream production method of anhydrous ethanol, which is rapidly developing in the contemporary era, mainly adopts the molecular sieve adsorption dehydration method for the further dehydration process of high-concentration ethanol. Firstly, the high-concentration ethanol gas with water content close to azeotropic composition is obtained through the rectification process, and the ethanol gas is adsorbed by molecular sieve gas phase to remove residual water in ethanol to obtain anhydrous ethanol product. The regeneration of the adsorbent is realized by means of variable pressure and temperature.
无水乙醇分子筛吸附吸附脱水装置要求毗邻乙醇精馏脱水装置，吸附脱水原料来自乙醇精馏脱水装置的精塔顶的酒精浓度接近共沸组成的高浓度乙醇蒸汽，直接进入分子筛气相吸附装置，脱去乙醇中残余的水分，得到无水乙醇产品；吸附剂再生过程产生的富含水的乙醇溶液，俗称淡酒，返回乙醇精馏脱水装置，回收其中的乙醇。该气相进料工艺蒸汽消耗较少，吨无水乙醇产品的分子筛吸附脱水过程增加蒸汽消耗0.7吨左右，由于不引进第三种溶剂，其生产过程为绿色清洁生产工艺。但采用气相进料的分子筛吸附脱水装置不能远离精馏装置，无水乙醇分子筛吸附脱水装置的建设选址和操作缺乏灵活性；另外，无水乙醇在储存和运输过程中容易吸水，造成产品中的水含量增加，需采取一定措施，增加了无水乙醇产品的储存和运输成本。The anhydrous ethanol molecular sieve adsorption adsorption dehydration device is required to be adjacent to the ethanol rectification dehydration device. The raw material for adsorption and dehydration comes from the ethanol rectification dehydration device. The residual moisture in the ethanol is removed to obtain anhydrous ethanol product; the water-rich ethanol solution produced during the regeneration of the adsorbent, commonly known as light wine, is returned to the ethanol rectification and dehydration device to recover the ethanol in it. The gas-phase feeding process consumes less steam, and the molecular sieve adsorption and dehydration process of a ton of anhydrous ethanol product increases the steam consumption by about 0.7 tons. Since the third solvent is not introduced, the production process is a green and clean production process. However, the molecular sieve adsorption and dehydration device using gas phase feed cannot be far away from the rectification device, and the construction site selection and operation of the anhydrous ethanol molecular sieve adsorption and dehydration device lack flexibility; in addition, absolute ethanol is easy to absorb water during storage and transportation, resulting in As the water content increases, certain measures need to be taken, which increases the storage and transportation costs of absolute ethanol products.
发明内容Contents of Invention
本发明的无水乙醇的生产方法，采用无水乙醇液相进料生产新方法，解决了远离乙醇精馏脱水装置的无水乙醇分子筛吸附脱水生产装置，需单独设置淡酒回收系统的难题，使得非酒精生产企业可以实现无水乙醇的生产。本发明提供了一种利用酒精浓度为90～99％体积比的高浓度酒精的原料液，及酒精浓度为1％～90％体积比的低浓度酒精原料液，采用集原料蒸发和淡酒脱水为一体的多功能乙醇回收塔，以及精密精馏、变温变压吸附和能量多级多效利用等技术，实现了以高浓度酒精液相原料生产无水乙醇产品的生产过程。The production method of dehydrated ethanol of the present invention adopts a new production method of dehydrated ethanol liquid-phase feed, which solves the problem that the dehydrated ethanol molecular sieve adsorption and dehydration production device far away from the ethanol rectification and dehydration device needs to set up a light wine recovery system separately, It enables non-alcohol production enterprises to realize the production of absolute ethanol. The invention provides a high-concentration alcohol raw material liquid with an alcohol concentration of 90-99% volume ratio and a low-concentration alcohol raw material liquid with an alcohol concentration of 1%-90% volume ratio, and adopts raw material evaporation and light wine dehydration The integrated multi-functional ethanol recovery tower, as well as technologies such as precision rectification, temperature-swing pressure-swing adsorption, and multi-stage multi-effect utilization of energy, have realized the production process of producing anhydrous ethanol products from high-concentration alcohol liquid-phase raw materials.
本发明的具体技术是这样实现的：Concrete technology of the present invention is realized like this:
本发明采用的主要设备：乙醇回收塔、吸附器、产品冷凝器、再沸器和淡酒预热器等，在各设备之间设置有阀门和对应的管线，将酒精浓度为90～99％体积比的高浓度酒精的原料液、酒精浓度为1％～90％体积比的低浓度酒精原料液和分子筛再生过程产生的淡酒送入乙醇回收塔。Main equipment used in the present invention: ethanol recovery tower, adsorber, product condenser, reboiler and light wine preheater, etc., valves and corresponding pipelines are arranged between each equipment, and the alcohol concentration is 90-99%. The raw material solution of high concentration alcohol by volume ratio, the low concentration alcohol raw material solution with alcohol concentration of 1% to 90% by volume ratio and the light alcohol produced in the molecular sieve regeneration process are sent to the ethanol recovery tower.
所述酒精浓度为90～99％体积比的高浓度乙醇液体原料送至乙醇回收塔的塔顶，酒精浓度为1％～90％体积比的乙醇原料液及淡酒送至乙醇回收塔侧线进料口。The high-concentration ethanol liquid raw material with an alcohol concentration of 90-99% volume ratio is sent to the top of the ethanol recovery tower, and the ethanol raw material liquid and light wine with an alcohol concentration of 1%-90% volume ratio are sent to the side line of the ethanol recovery tower. feed port.
所述的酒精浓度为90～99％体积比的高浓度酒精的原料液、酒精浓度为1％～90％体积比的酒精原料液进料，经冷凝器分别预热后，进入乙醇回收塔。The high-concentration alcohol raw material liquid with an alcohol concentration of 90-99% by volume and the alcohol raw material liquid with an alcohol concentration of 1%-90% by volume are fed into the ethanol recovery tower after being respectively preheated by a condenser.
所述的淡酒经淡酒预热器预热后进入乙醇回收塔，淡酒预热器的加热介质为再沸器蒸气凝液，也可以考虑乙醇回收塔塔釜排出液。The light wine is preheated by the light wine preheater and then enters the ethanol recovery tower. The heating medium of the light wine preheater is the steam condensate of the reboiler, and the liquid discharged from the ethanol recovery tower can also be considered.
所述的乙醇回收塔的操作压力为常压～1.1MPa。乙醇回收塔塔顶的乙醇蒸气经加热器加热，温度为80～290℃，通过正处于吸附状态的分子筛吸附器进行吸附脱水操作。The operating pressure of the ethanol recovery tower is normal pressure ~ 1.1MPa. The ethanol vapor at the top of the ethanol recovery tower is heated by a heater at a temperature of 80-290°C, and the adsorption and dehydration operation is carried out by the molecular sieve adsorber in the adsorption state.
所述的分子筛吸附器对乙醇和水进行选择性吸附，在吸附器中水被吸附剂吸附，通过分子筛吸附器脱水后的乙醇气体，经品冷凝器冷却得到无水乙醇产品。分子筛吸附器设置两个以上，依次交替完成吸附、脱附操作，实现进料和采出连续稳定操作。The molecular sieve adsorber selectively adsorbs ethanol and water, water is adsorbed by the adsorbent in the adsorber, and the ethanol gas dehydrated by the molecular sieve adsorber is cooled by a product condenser to obtain anhydrous ethanol product. More than two molecular sieve adsorbers are installed, and the adsorption and desorption operations are completed alternately in sequence to realize continuous and stable operation of feeding and extraction.
本发明的乙醇回收塔具有将酒精浓度为90～99％体积比的高浓度乙醇液体原料蒸发，以及酒精浓度为1％～90％体积比的低浓度乙醇原料液和淡酒的脱水功能。The ethanol recovery tower of the present invention has the functions of evaporating high-concentration ethanol liquid raw material with alcohol concentration of 90-99% volume ratio, and dehydrating low-concentration ethanol raw material liquid and light wine with alcohol concentration of 1%-90% volume ratio.
需要说明的是：It should be noted:
乙醇回收塔设计上巧妙地将高效填料塔技术和板式塔技术相结合，使精馏单元的分离能力及设备的可靠性均得到提高，可实现侧线多股进料。来自淡酒罐的淡酒，采用淡酒预热器预热，加热介质为再沸器蒸气凝液，也可以考虑乙醇回收塔塔釜排出液。乙醇回收塔的操作压力为常压～1.1MPa。The design of the ethanol recovery tower cleverly combines the high-efficiency packed tower technology with the plate tower technology, which improves the separation ability of the rectification unit and the reliability of the equipment, and can realize multi-strand feed from the side line. The light wine from the light wine tank is preheated by the light wine preheater, and the heating medium is the steam condensate of the reboiler. It is also possible to consider ethanol recovery of the tower kettle discharge liquid. The operating pressure of the ethanol recovery tower is normal pressure ~ 1.1MPa.
乙醇回收塔塔顶的乙醇蒸气经加热器加热后，温度为80～290℃，通过正处于吸附状态的5分子筛吸附器进行吸附脱水操作。在吸附器中装有可对乙醇和水进行选择性吸附的吸附剂，此种吸附剂可以是硅铝型分子筛，可选择的分子筛为A型、X型、丝光沸石型、ZSM型等。在吸附器中水被吸附剂吸附，通过分子筛吸附器脱水后的乙醇气体，经产品冷凝器冷却得到无水乙醇产品，进入9无水乙醇产品罐收集。吸附压力为常压～1MPa，温度为80-300℃。After the ethanol vapor at the top of the ethanol recovery tower is heated by the heater, the temperature is 80-290°C, and the adsorption and dehydration operation is carried out through the 5 molecular sieve adsorber in the adsorption state. The adsorber is equipped with an adsorbent that can selectively adsorb ethanol and water. This adsorbent can be a silica-alumina molecular sieve, and the optional molecular sieves are A type, X type, mordenite type, ZSM type, etc. In the adsorber, water is adsorbed by the adsorbent, and the ethanol gas dehydrated by the molecular sieve adsorber is cooled by the product condenser to obtain anhydrous ethanol product, which enters the 9 anhydrous ethanol product tank for collection. The adsorption pressure is normal pressure to 1MPa, and the temperature is 80-300°C.
为了使整个吸附脱水工艺连续进行，设置两个以上的吸附器，依次交替完成吸附解吸操作，实现进料和采出连续操作。In order to make the whole adsorption and dehydration process run continuously, more than two adsorbers are set up, and the adsorption and desorption operations are completed alternately in turn to realize the continuous operation of feeding and extraction.
本发明有效地解决了无水乙醇分子筛吸附脱水生产中，采用接近乙醇与水共沸组成的高浓度液体乙醇为原料，设备投资大，蒸汽消耗和操作成本高等问题。流程合理，设备功能多，投资大幅度下降；热量利用合理，实现了无水乙醇液相进料的分子筛吸附脱水生产工艺与气相进料工艺相近的蒸汽消耗量；非酒精生产企业可以容易实现无水乙醇的生产；工艺灵活性强，装置可以建在无水乙醇产品用户附近，降低了无水乙醇产品的运输和储存成本。本发明将有利于增强无水乙醇产品，特别是燃料乙醇产品推广使用的市场竞争力。The invention effectively solves the problems of using high-concentration liquid ethanol close to the azeotropic composition of ethanol and water in the production of anhydrous ethanol molecular sieve adsorption and dehydration, large equipment investment, high steam consumption and high operating cost. The process is reasonable, the equipment has many functions, and the investment is greatly reduced; the heat utilization is reasonable, and the steam consumption of the molecular sieve adsorption dehydration production process of anhydrous ethanol liquid phase feed is similar to that of the gas phase feed process; non-alcohol production enterprises can easily realize no dehydration. The production of water ethanol; the process is flexible, and the device can be built near the users of absolute ethanol products, which reduces the transportation and storage costs of absolute ethanol products. The invention will be beneficial to enhance the market competitiveness of anhydrous ethanol products, especially the promotion and use of fuel ethanol products.
附图说明Description of drawings
图1：无水乙醇的生产方法流程示意图；Fig. 1: Schematic flow chart of the production method of absolute ethanol;
图中符号说明如下：The symbols in the figure are explained as follows:
1-乙醇回收塔；2-再沸器；3-加热器；4-淡酒预热器；5A/5B-吸附器或脱附器；6、7、8-产品冷凝器；9-无水乙醇产品罐；10-淡酒冷凝器；11-淡酒罐；12-淡酒后冷凝器。1-ethanol recovery tower; 2-reboiler; 3-heater; 4-light wine preheater; 5A/5B-adsorber or desorber; 6, 7, 8-product condenser; 9-anhydrous Ethanol product tank; 10-light wine condenser; 11-light wine tank; 12-light wine after condenser.
具体实施方式 Detailed ways
下面结合附图和实施例对本发明做进一步的详细描述：Below in conjunction with accompanying drawing and embodiment the present invention is described in further detail:
无水乙醇的生产方法操作步骤如图1所示，无水乙醇生产过程主要由乙醇回收塔、吸附器、产品冷凝器、再沸器和淡酒预热器等组成，在各设备之间设置有阀门和对应的管线。The operation steps of the production method of absolute ethanol are shown in Figure 1. The production process of absolute ethanol is mainly composed of an ethanol recovery tower, an adsorber, a product condenser, a reboiler, and a light wine preheater. There are valves and corresponding pipelines.
原料蒸发和淡酒脱水操作。将乙醇含量96％体积比、温度30℃的高浓度乙醇液体原料经产品冷凝器7预热后送至乙醇回收塔1的塔顶，另外酒精浓度为85％体积比、温度30℃的低浓度乙醇原料液经产品冷凝器8预热后送至乙醇回收塔进料口，同时将富含水的脱附再生过程产生的淡酒经淡酒经预热器4预热后，也送至乙醇回收塔进料口，淡酒经预热器4的加热介质为再沸器2加热蒸气凝液。乙醇回收塔通过再沸器2提供加热能量，加热蒸汽也可以通入塔釜直接加热，废液从塔釜排出。高浓度酒精原料液在乙醇回收塔中实现汽化，淡酒和低酒精浓度酒精在塔内通过传质和传热作用，实现酒精浓缩和汽化，操作压力为0.5MPa。乙醇回收塔塔塔顶的乙醇蒸气经加热器4加热到150℃，进入正处于吸附状态的分子筛吸附器5A进行吸附脱水操作。Evaporation of raw materials and dehydration of light wine. The high-concentration ethanol liquid raw material with an ethanol content of 96% volume ratio and a temperature of 30°C is preheated by the product condenser 7 and sent to the top of the ethanol recovery tower 1. In addition, the alcohol concentration is 85% volume ratio and a low concentration of 30°C. The ethanol raw material liquid is sent to the feed port of the ethanol recovery tower after being preheated by the product condenser 8. At the same time, the light wine produced in the desorption regeneration process rich in water is also sent to the ethanol after being preheated by the preheater 4. The feed port of the recovery tower, the heating medium of the light wine through the preheater 4 is the reboiler 2 to heat the steam to condensate. The ethanol recovery tower provides heating energy through the reboiler 2, and the heating steam can also be passed into the tower kettle for direct heating, and the waste liquid is discharged from the tower kettle. The high-concentration alcohol raw material liquid is vaporized in the ethanol recovery tower, and the light alcohol and low-alcohol concentration alcohol are concentrated and vaporized through mass transfer and heat transfer in the tower, and the operating pressure is 0.5MPa. The ethanol vapor at the top of the ethanol recovery tower is heated to 150°C by the heater 4, and then enters the molecular sieve adsorber 5A in the adsorption state for adsorption and dehydration operation.
在吸附器中装有可对乙醇和水进行选择性吸附的吸附剂。此种吸附剂可以是硅铝型分子筛，可选择的分子筛为A型、X型、丝光沸石型、ZSM型等。在吸附器中水被吸附剂吸附，乙醇通过分子筛吸附器5A后，经产品冷凝器6、冷凝器7和冷凝器8冷却得到无水乙醇产品。吸附压力为0.5Mpa，温度为150℃。Adsorbents capable of selectively adsorbing ethanol and water are installed in the adsorber. Such an adsorbent can be a silica-alumina molecular sieve, and the optional molecular sieves are A type, X type, mordenite type, ZSM type and the like. In the adsorber, water is adsorbed by the adsorbent, and after the ethanol passes through the molecular sieve adsorber 5A, it is cooled by the product condenser 6, condenser 7 and condenser 8 to obtain anhydrous ethanol product. The adsorption pressure is 0.5Mpa, and the temperature is 150°C.
脱附操作。当吸附器5A吸附操作完成后，吸附器5B进入吸附操作。吸附器5A脱附压力为-0.3Mpa。在脱附操作进行到一定程度，从正处于吸附状态的吸附器5B得到的水含量很低的部分乙醇蒸汽，引入正进行脱附操作的吸附器5A，对处于脱附操作的吸附器5A进行吹扫。经过脱附、吹扫，吸附器5A中所吸附的水被彻底脱除，可以重新进入吸附操作。脱附操作过程中产生的富含水的淡酒酒气，经淡酒冷凝器10和淡酒后冷凝器12冷凝冷却后进入淡酒罐11，经过淡酒加热器4预热后，返回乙醇回收塔脱水回收。为了使整个吸附脱水工艺连续进行，设置两个吸附器，依次交替完成吸附解吸操作，实现进料采出连续操作。Desorption operation. When the adsorption operation of the adsorber 5A is completed, the adsorber 5B enters the adsorption operation. The desorption pressure of the adsorber 5A is -0.3Mpa. When the desorption operation is carried out to a certain extent, the part of the ethanol vapor with a very low water content obtained from the adsorber 5B in the adsorption state is introduced into the adsorber 5A in the desorption operation, and the adsorber 5A in the desorption operation is carried out. purge. After desorption and purging, the water adsorbed in the adsorber 5A is completely removed, and the adsorption operation can be re-entered. The light wine gas rich in water produced during the desorption operation is condensed and cooled by the light wine condenser 10 and the light wine post-condenser 12, then enters the light wine tank 11, and after being preheated by the light wine heater 4, returns to ethanol The recovery tower dehydrates and recovers. In order to make the whole adsorption and dehydration process run continuously, two adsorbers are set up to alternately complete the adsorption and desorption operations in turn, realizing the continuous operation of feed and extraction.
按照以上叙述的工艺过程，通过图1所示的无水乙醇生产装置，可得到水含量小于0.1％的无水乙醇产品，吨乙醇产品的蒸汽消耗量为0.7吨。According to the process described above, through the absolute ethanol production device shown in Figure 1, anhydrous ethanol products with a water content of less than 0.1% can be obtained, and the steam consumption per ton of ethanol products is 0.7 tons.
在本实施例中，可以将原料的酒精浓度确定为90～99％体积比的高浓度酒精的原料液及酒精浓度为1％～90％体积比的酒精原料液；乙醇回收塔的操作压力为常压～1.1MPa；可得到水含量为0.01％～0.8％的无水乙醇产品，吨无水乙醇产品的蒸汽消耗量为0.5～1.0吨。In this embodiment, the alcohol concentration of the raw material can be determined as the raw material liquid of high-concentration alcohol of 90-99% volume ratio and the alcohol raw material liquid whose alcohol concentration is 1%-90% volume ratio; the operating pressure of the ethanol recovery tower is Atmospheric pressure ~ 1.1MPa; dehydrated ethanol products with a water content of 0.01% to 0.8% can be obtained, and the steam consumption per ton of dehydrated ethanol products is 0.5 to 1.0 tons.
本发明公开和提出的工艺和方法，本领域技术人员可通过借鉴本文内容，适当改变原料、工艺参数、结构设计等环节实现。本发明的方法与技术已通过较佳实施例子进行了描述，相关技术人员明显能在不脱离本发明内容、精神和范围内对本文所述的方法和技术进行改动或适当变更与组合，来实现本发明技术。特别需要指出的是，所有相类似的替换和改动对本领域技术人员来说是显而易见的，他们都被视为包括在本发明精神、范围和内容中。The process and method disclosed and proposed by the present invention can be realized by those skilled in the art by referring to the content of this article and appropriately changing the raw materials, process parameters, structural design and other links. The methods and techniques of the present invention have been described through preferred implementation examples, and those skilled in the art can obviously make changes or appropriate changes and combinations to the methods and techniques described herein without departing from the content, spirit and scope of the present invention to achieve The technology of the present invention. In particular, it should be pointed out that all similar substitutions and modifications will be obvious to those skilled in the art, and they are all considered to be included in the spirit, scope and content of the present invention.
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| BRPI0600553A (en) * | 2006-02-24 | 2007-11-20 | Siemens Ltda | process and system for the production of alcohol by multiple effect distillation |
| CN101648848B (en) * | 2009-09-09 | 2013-06-19 | 天津大学 | Combined production method for fuel alcohol and edible alcohol |
| CN102351644A (en) * | 2011-08-19 | 2012-02-15 | 天津大学 | Method and device for molecular sieve compound rectifying and refining ethanol product from biobutanol apparatus |
| CN102397707A (en) * | 2011-11-24 | 2012-04-04 | 中国船舶重工集团公司第七�三研究所 | Automatic heating device for alcohol recovery system |
| CN103706141B (en) * | 2014-01-22 | 2015-08-12 | 象山医疗精密仪器有限公司 | Steam compression type alcohol distillation column and distillating method |
| CN105418368B (en) * | 2015-12-31 | 2017-12-26 | 江苏九天高科技股份有限公司 | A kind of technique and device for producing high straight alcohol |
| CN105967977A (en) * | 2016-06-24 | 2016-09-28 | 河南天冠生物燃料工程技术有限公司 | Technology for preparing fuel ethanol through adsorption method |
| CN107417647A (en) * | 2017-05-10 | 2017-12-01 | 天津九源化工工程有限公司 | A kind of process for purification of water-containing tetrahydrofuran |
| CN107021872B (en) * | 2017-05-10 | 2021-07-23 | 天津九源化工工程有限公司 | Method for separating and purifying water-containing isopropanol |
| CN107253901A (en) * | 2017-07-26 | 2017-10-17 | 四川天采科技有限责任公司 | A kind of separation of high-purity isopropanol and purification method |
| CN117658776A (en) * | 2017-12-28 | 2024-03-08 | 内蒙古伊泰煤基新材料研究院有限公司 | Continuous adsorption dehydration device and method for water-containing light alcohol |
| CN112619192B (en) * | 2020-12-30 | 2024-10-29 | 肥城金塔机械科技有限公司 | Double-effect thermally coupled molecular sieve dehydration energy-saving system and method for producing absolute ethyl alcohol by using same |
| CN113105309A (en) * | 2021-03-23 | 2021-07-13 | 江苏罗迈特生物科技有限公司 | Alcohol molecular sieve dehydration method |
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