CN113072425A - Method for separating ethanol, cyclohexanol and water by extractive distillation-pressure swing distillation of dividing wall tower - Google Patents

Method for separating ethanol, cyclohexanol and water by extractive distillation-pressure swing distillation of dividing wall tower Download PDF

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CN113072425A
CN113072425A CN202110422352.6A CN202110422352A CN113072425A CN 113072425 A CN113072425 A CN 113072425A CN 202110422352 A CN202110422352 A CN 202110422352A CN 113072425 A CN113072425 A CN 113072425A
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tower
water
pressure
cyclohexanol
extractive
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马恒
王英龙
霍冰洁
王佳
胡明月
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Qingdao University of Science and Technology
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • C07C29/84—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by extractive distillation
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/14—Fractional distillation or use of a fractionation or rectification column
    • B01D3/143—Fractional distillation or use of a fractionation or rectification column by two or more of a fractionation, separation or rectification step
    • B—PERFORMING OPERATIONS; TRANSPORTING
    • B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
    • B01D—SEPARATION
    • B01D3/00—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping
    • B01D3/34—Distillation or related exchange processes in which liquids are contacted with gaseous media, e.g. stripping with one or more auxiliary substances
    • B01D3/40—Extractive distillation
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
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    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C29/00—Preparation of compounds having hydroxy or O-metal groups bound to a carbon atom not belonging to a six-membered aromatic ring
    • C07C29/74—Separation; Purification; Use of additives, e.g. for stabilisation
    • C07C29/76—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment
    • C07C29/80—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation
    • C07C29/82—Separation; Purification; Use of additives, e.g. for stabilisation by physical treatment by distillation by azeotropic distillation
    • F—MECHANICAL ENGINEERING; LIGHTING; HEATING; WEAPONS; BLASTING
    • F28—HEAT EXCHANGE IN GENERAL
    • F28D—HEAT-EXCHANGE APPARATUS, NOT PROVIDED FOR IN ANOTHER SUBCLASS, IN WHICH THE HEAT-EXCHANGE MEDIA DO NOT COME INTO DIRECT CONTACT
    • F28D21/00—Heat-exchange apparatus not covered by any of the groups F28D1/00 - F28D20/00
    • C—CHEMISTRY; METALLURGY
    • C07—ORGANIC CHEMISTRY
    • C07C—ACYCLIC OR CARBOCYCLIC COMPOUNDS
    • C07C2601/00—Systems containing only non-condensed rings
    • C07C2601/12—Systems containing only non-condensed rings with a six-membered ring
    • C07C2601/14—The ring being saturated
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    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P20/00—Technologies relating to chemical industry
    • Y02P20/50—Improvements relating to the production of bulk chemicals
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
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    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
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Abstract

本发明公开了一种隔壁塔萃取精馏‑变压精馏分离乙醇‑环己醇‑水的方法，所述隔壁塔萃取精馏‑变压精馏分离乙醇‑环己醇‑水的方法是采用侧线采出、隔壁塔、变压精馏，以乙二醇作为萃取剂，在分离出高纯度的乙醇、环己醇产品的同时，将萃取精馏塔塔釜得到的萃取剂和高压精馏塔塔底馏出的水用于萃取精馏塔及高压精馏塔进料的预热。本发明在萃取精馏塔塔顶分离出质量浓度大于99.97wt％的乙醇，在高压精馏塔、低压精馏塔塔底分别分离出质量浓度大于99.98wt％的水和环己醇，同时实现了萃取剂乙二醇的回收利用，利用高压精馏塔水的热量与进入高压精馏塔的物料进行换热，萃取精馏塔塔底馏出的萃取剂乙二醇进入换热器对进入萃取精馏塔的物料醪液进行加热，大大降低了能耗。The invention discloses a method for separating ethanol-cyclohexanol-water by extractive distillation-pressure swing distillation of a partition wall column. Using side-drawing, dividing wall column, pressure swing rectification, and using ethylene glycol as the extractant, while separating high-purity ethanol and cyclohexanol products, the extractant and high-pressure rectification column obtained from the extractive distillation column kettle are separated. The water distilled from the bottom of the distillation column is used for the preheating of the feed of the extractive distillation column and the high pressure distillation column. The invention separates ethanol with a mass concentration of more than 99.97wt% at the top of the extractive rectification tower, and separates water and cyclohexanol with a mass concentration of more than 99.98wt% at the bottom of the high-pressure rectification tower and the low-pressure rectification tower. In order to recover and utilize the extraction agent ethylene glycol, the heat of the high-pressure rectifying tower water is used to exchange heat with the materials entering the high-pressure rectifying tower. The material mash of the extractive distillation column is heated, which greatly reduces the energy consumption.

Description

Method for separating ethanol, cyclohexanol and water by extractive distillation-pressure swing distillation of dividing wall tower
[ technical field ] A method for producing a semiconductor device
The invention relates to the technical field of rectification and purification, in particular to a method for separating ethanol, cyclohexanol and water by extractive distillation-pressure swing distillation of a dividing wall tower.
[ background of the invention ]
The fuel ethanol refers to absolute ethanol with volume concentration of more than 99.5 percent, is the most environment-friendly oxygenating agent and octane number promoter of gasoline, can effectively reduce greenhouse gas and PM2.5 emission, has positive effect on improving the quality of atmospheric environment, China is the third country of biofuel ethanol production and application in the world, is second to America and Brazil, and is mainly obtained by liquefying, saccharifying, fermenting, distilling, dehydrating and other process steps of sugar crops and starchy crops, the mass content of ethanol in mash obtained by biomass fermentation is only about 10 percent, most of ethanol is water, the key point of preparing the fuel ethanol from the fermented mash is to remove the water in the mash, the invention is an advanced technical scheme for removing water from the fermented mash, the mash of fuel ethanol production enterprises contains water, ethanol and cyclohexanol, a reasonable rectification separation process is designed, and the ethanol in the mash is recovered, Cyclohexanol.
The boiling point of water under normal pressure is 100.02 ℃, the boiling point of ethanol under normal pressure is 78.31 ℃, the boiling point of cyclohexanol under normal pressure is 161.84 ℃, the mixture of ethanol, cyclohexanol and water can form two azeotropes, namely a water and ethanol binary azeotrope and a water and cyclohexanol binary azeotrope, under normal temperature and normal pressure, the azeotropic point of the water and ethanol mixture is 78.16 ℃, the molar fraction of ethanol in azeotropic composition is 89.99%, the molar fraction of water is 10.01%, the azeotropic point of the water and cyclohexanol mixture is 97.80 ℃, the molar fraction of water in azeotropic composition is 80.00%, and the molar fraction of cyclohexanol is 20.00%.
The patent (CN106966866B) discloses a method for separating butanone-isopropanol-ethanol azeotrope by three-tower pressure swing distillation, which solves the problem of difficult separation caused by the existence of multiple groups of azeotropic and rectifying boundaries in a near-boiling point ternary system, realizes heat integration among three towers through a partial heat integration mode, reduces energy consumption to the maximum extent, but adopts 3 rectifying towers in the pressure swing distillation process, and the process is relatively complex.
The design process of an ethanol-water rectifying tower is reported in the literature (Qinhibo, Yan Shaofeng, Shanghan, Guo. ethanol-water rectifying tower design [ J ]. times agricultural machinery, 2020, 47(03):97-98.), the structure of equipment is improved, the rectifying effect is obviously improved, the separation of ethanol and water is realized, but only ethanol can be recovered, and the separation of cyclohexanol and water is not realized.
The literature (maoruajun, in crane, celebrate, gentamica. the simulation and optimization of a dividing wall column extractive distillation separation tert-butanol-ethanol-water azeotrope [ J ] chemical technology, 2019, 27(05):61-65.) reports a method for extracting and separating a tert-butanol-ethanol-water azeotrope by using a dividing wall column with ethylene glycol as an extracting agent, and compared with the conventional extractive distillation process, the process reduces the energy consumption by 38.66%, but the process is relatively complex in operation and does not relate to a cyclohexanol-water system.
At present, no report about separating cyclohexanol-ethanol-water by adopting a bulkhead column extractive distillation-pressure swing distillation process exists in patents and documents, so that a novel and energy-saving method for separating a cyclohexanol-ethanol-water azeotropic system has great environmental protection significance and industrial value, and a method for separating ethanol-cyclohexanol-water by adopting bulkhead column extractive distillation-pressure swing distillation is urgently needed to solve the problems.
[ summary of the invention ]
[ problem to be solved ]
The invention aims to provide a method for separating ethanol-cyclohexanol-water by extractive distillation-pressure swing distillation of a bulkhead tower, which aims to solve the problem that the ethanol-cyclohexanol-water mixture proposed in the background technology is difficult to separate due to the existence of azeotropy.
[ solution ]
In order to achieve the purpose, the invention provides the following technical scheme: a method for separating ethanol-cyclohexanol-water by partition column extractive distillation-pressure swing distillation is characterized in that a side draw, a partition column and pressure swing distillation are adopted, ethylene glycol is used as an extractant, heat exchange network optimization is performed while high-purity ethanol and cyclohexanol products are separated, the extractant obtained at the bottom of the extractive distillation column and water distilled from the bottom of a high-pressure distillation column are used for preheating of feeding materials of the extractive distillation column and the high-pressure distillation column, and the method specifically comprises the following steps:
(1) the raw material liquid enters the extraction rectifying tower after being preheated by the heat exchanger, so that the heat load of a reboiler is reduced. Raw material liquid enters an extraction and rectification tower from a heat exchanger to a mixer at the 20 th tower plate under normal temperature, the number of the tower plates of the extraction and rectification tower is 50, the operation pressure of the tower top is 0.2atm, and the reflux ratio is 3.6;
(2) 6000kg/h of ethylene glycol is added at the 4 th tower plate of the extraction rectifying tower, the discharge temperature at the top of the tower is 42.32 ℃, the feed liquid enters the 35 th tower plate of the auxiliary rectifying tower, the discharge at the bottom of the extraction rectifying tower is the ethylene glycol, the discharge temperature is 149.9 ℃, the feed liquid is used for preheating mash feed, and the feed liquid extracted from the lateral line is azeotrope of water and cyclohexanol and ethylene glycol;
(3) the feed liquid from the extraction rectifying tower enters an auxiliary rectifying tower at a 35 th tower plate, the number of the tower plates of the auxiliary rectifying tower is 35, the operation pressure of the tower top is 0.2atm, the discharge of the tower top is an azeotrope of water and cyclohexanol, and the discharge temperature is 59.94 ℃;
(4) the feed liquid is pumped to a heat exchanger for heating and then enters the 20 th tower plate of the high-pressure rectifying tower;
(5) the feed liquid from the auxiliary rectifying tower enters a high-pressure rectifying tower at a 20 th tower plate, the number of the tower plates of the high-pressure rectifying tower is 27, the operating pressure of the tower top is 3atm, the reflux ratio is 1.1, the discharge of the tower top is an azeotrope of water and cyclohexanol under 3atm, and the discharge temperature is 130.835 ℃;
(6) the feed liquid from the high-pressure rectifying tower enters a low-pressure rectifying tower at a 20 th tower plate, the total number of the tower plates of the low-pressure rectifying tower is 23, the operating pressure of the tower top is 0.1atm, the reflux ratio is 1, the discharge of the tower top is an azeotrope of water and cyclohexanol under 0.1atm, the discharge temperature is 45.24 ℃, and the feed liquid can circularly enter the high-pressure rectifying tower through a pump until the mass concentration of the water and the cyclohexanol reaches more than 99.9 wt%.
A method for separating ethanol, cyclohexanol and water by extractive distillation-pressure swing distillation of a bulkhead tower is characterized by comprising the following steps: the top discharge of the extraction rectifying tower is ethanol with the mass concentration of more than 99.97 wt%, the bottom discharge of the high-pressure rectifying tower is water with the mass concentration of more than 99.98 wt%, and the bottom discharge of the low-pressure rectifying tower is cyclohexanol with the mass concentration of more than 99.98 wt%.
[ advantageous effects ]
Compared with the prior art, the invention has the beneficial effects that:
(1) by selecting glycol as an extracting agent, adopting a side-draw, dividing wall tower rectifying technology and a pressure swing rectifying method, separating ethanol with the mass concentration of more than 99.97 wt% from the top of an extraction rectifying tower, separating water and cyclohexanol with the mass concentration of more than 99.98 wt% from the bottoms of a high-pressure rectifying tower and a low-pressure rectifying tower respectively, wherein the content of ethanol in water is less than 10ppm, the content of cycloethanol is less than 10ppm, and the purity is extremely high, meanwhile, the recycling of the extracting agent glycol is realized, simultaneously, the heat of the extracting agent is utilized to preheat a raw material liquid, the heat of the water in the high-pressure rectifying tower is utilized to exchange heat with a material entering the high-pressure rectifying tower, the extracting agent glycol distilled from the bottom of the extraction rectifying tower enters a heat exchanger to heat a material mash entering the extraction rectifying tower, and the energy consumption is greatly reduced.
(2) By adopting a side line extraction and partition wall tower technology, side line extracted steam of the extraction rectifying tower is introduced to the bottom of the auxiliary rectifying tower and is used as rising steam of the auxiliary rectifying tower, so that a reboiler of the auxiliary rectifying tower is saved, meanwhile, raw material liquid is preheated by utilizing the heat of an extracting agent, heat exchange is carried out between the heat of water in the high-pressure rectifying tower and the material entering the high-pressure rectifying tower, the extracting agent glycol distilled from the bottom of the extraction rectifying tower enters a heat exchanger to heat material mash entering the extraction rectifying tower, the heat of each material is fully utilized, heat coupling is realized, an AEA heat exchange network is utilized for optimization, and the heat is fully utilized.
(3) The water-ethanol and water-cyclohexanol azeotropic system is separated by only adopting four rectifying towers, so that the equipment investment and later maintenance cost are low, the separation process is simple, the used extracting agent glycol has high efficiency and excellent cost performance, and the extracting agent is recycled by recycling the extracting agent, so that the amount of the extracting agent which needs to be replenished again at each time is small, the operation cost is reduced to the minimum, the replenishment amount is extremely small, and the raw material cost is reduced.
(4) The extractant obtained from the bottom of the extraction rectifying tower and the water distilled from the bottom of the high-pressure rectifying tower are used for preheating the feeding materials of the extraction rectifying tower and the high-pressure rectifying tower, so that the heat load of a reboiler of the extraction rectifying tower and the high-pressure rectifying tower is reduced, the heat pollution to the environment is reduced, and the purposes of energy conservation and environmental protection are achieved.
[ description of the drawings ]
FIG. 1 is a process flow diagram of the present invention for separating water-ethanol-cyclohexanol ternary system.
T1-extractive distillation column, T2-auxiliary distillation column, T3-high pressure distillation column, T4-low pressure distillation column, C1-extractive distillation column condenser, C2-auxiliary distillation column condenser, C3-high pressure distillation column condenser, C4-low pressure distillation column condenser, R1-extractive distillation column reboiler, R2-high pressure distillation column reboiler, R3-low pressure distillation column reboiler, B1-ethylene glycol mixer, B2-heat exchanger for two streams of ethylene glycol and mash, B3-auxiliary distillation column overhead stream to heat exchanger B4 pump, B4-heat exchanger for two streams of water and cyclohexanol azeotrope, B5-heat stream to high pressure distillation column pump
[ detailed description ] embodiments
Example 1:
the feed temperature of mash of an extractive distillation tower (T1) is 66 ℃, the flow rate is 10000kg/h, a feed plate is a 20 th plate, the feed temperature of an extractant glycol is 40 ℃, the flow rate is 6000kg/h, the feed plate is a 4 th plate, the operating pressure is 0.2atm, the mass concentration of water in the feed mash is 85 wt%, the mass concentration of ethanol is 10 wt%, the mass concentration of cyclohexanol is 5 wt%, the number of theoretical plates of the extractive distillation tower (T1) is 50, the reflux ratio is 3.6, the temperature of the top of the tower is 42.3214 ℃, the temperature of the bottom of the tower is 149.921 ℃, and the lateral line extraction position of the extractive distillation tower (T1) is a 46 th plate; the operating pressure of the secondary rectifying tower (T2) is 0.2atm, the theoretical plate number is 35, the feeding plate is the 35 th plate, the feeding temperature is 67 ℃, the top temperature is 59.9426 ℃, and the bottom temperature is 67.0642 ℃; the theoretical plate number of the high-pressure rectifying tower (T3) is 27 plates, the feeding pressure is 3atm, the feeding position of the mixed liquid discharged from the top of the secondary rectifying tower (T2) entering the high-pressure rectifying tower (T3) is the 20 th plate, the feeding temperature is 125 ℃, the feeding position of the circulating liquid is the 20 th plate, the feeding temperature is 45 ℃, the reflux ratio is 1.1, the temperature at the top of the tower is 130.835 ℃, and the temperature at the bottom of the tower is 134.044 ℃; the theoretical plate number of the low-pressure rectifying tower (T4) is 23 plates, the feeding plate is the 20 th plate, the feeding temperature is 44.78 ℃, the feeding pressure is 0.1atm, the tower top temperature is 45.2443 ℃, the tower bottom temperature is 99.2151 ℃, and the reflux ratio is 1. The mass concentration of the separated water is 99.99 wt%, the mass concentration of the ethanol can reach 99.98 wt%, and the mass concentration of the cyclohexanol can reach 99.99 wt%.

Claims (6)

1.一种隔壁塔萃取精馏-变压精馏分离乙醇-环己醇-水的方法，其特征在于：所述隔壁塔萃取精馏-变压精馏分离乙醇-环己醇-水的方法是采用侧线采出、隔壁塔、变压精馏，以乙二醇作为萃取剂，在分离出高纯度的乙醇、环己醇产品的同时，进行了换热网络优化，将萃取精馏塔T1塔釜得到的萃取剂和高压精馏塔T3塔底馏出的水用于萃取精馏塔T1及高压精馏塔T3进料的预热；1. a method for separating ethanol-cyclohexanol-water by next-door tower extractive distillation-pressure swing distillation, it is characterized in that: described next-door column extractive distillation-pressure swing distillation separates ethanol-cyclohexanol-water The method is to use side line extraction, partition column, pressure swing rectification, and use ethylene glycol as the extractant to separate high-purity ethanol and cyclohexanol products, and optimize the heat exchange network. The extraction agent that T1 tower still obtains and the water that the high-pressure rectifying tower T3 column bottom distills are used for the preheating of extractive rectifying tower T1 and high-pressure rectifying tower T3 feed; 具体包含以下步骤：Specifically includes the following steps: (1)原料液由换热器B2至混合器B1在常温下在第20块塔板处进入萃取精馏塔T1，萃取精馏塔T1塔板数为50，塔顶操作压力为0.2atm，回流比为3.6；(1) the raw material liquid enters the extractive distillation column T1 at the 20th plate at normal temperature from the heat exchanger B2 to the mixer B1, and the number of plates in the extractive distillation column T1 is 50, and the operating pressure at the top of the column is 0.2 atm, The reflux ratio is 3.6; (2)在萃取精馏塔T1的第4块塔板处加入6000kg/h的乙二醇，塔顶出料温度为42.32℃，料液进入副精馏塔T2第35块塔板，萃取精馏塔T1塔底出料为乙二醇，出料温度为149.9℃；(2) add the ethylene glycol of 6000kg/h at the 4th plate of extractive rectification tower T1, and the top discharge temperature is 42.32 ° C, and the feed liquid enters the 35th plate of secondary rectification tower T2, and the extractive The bottom discharge of distillation column T1 is ethylene glycol, and the discharge temperature is 149.9 °C; (3)来自萃取精馏塔T1的料液在第35块塔板处进入副精馏塔T2，副精馏塔T2的塔板数为35，塔顶操作压力为0.2atm；(3) the feed liquid from extractive rectification tower T1 enters secondary rectification tower T2 at the 35th plate, and the number of plates of secondary rectification tower T2 is 35, and the operating pressure at the top of the tower is 0.2 atm; (4)料液经泵B3至换热器B4加热后进入高压精馏塔T3第20块塔板；(4) feed liquid enters the 20th plate of high pressure rectifying tower T3 after being heated by pump B3 to heat exchanger B4; (5)来自副精馏塔T2的料液在第20块塔板处进入高压精馏塔T3，高压精馏塔T3的塔板数为27，塔顶操作压力为3atm，回流比为1.1，料液进入低压精馏塔T4第20块塔板；(5) the feed liquid from secondary rectifying tower T2 enters high-pressure rectifying tower T3 at the 20th plate, and the plate number of high-pressure rectifying tower T3 is 27, and the tower top operating pressure is 3 atm, and the reflux ratio is 1.1, The feed liquid enters the 20th plate of the low-pressure rectification tower T4; (6)来自高压精馏塔T3的料液在第20块塔板处进入低压精馏塔T4，低压精馏塔T4的塔板总数为23，塔顶操作压力为0.1atm，回流比为1，经泵B5可循环进入高压精馏塔T3，直至水和环己醇质量浓度达到99.9wt％以上。(6) the feed liquid from high-pressure rectifying tower T3 enters low-pressure rectifying tower T4 at the 20th plate, and the total number of plates of low-pressure rectifying tower T4 is 23, and the operating pressure at the top of the tower is 0.1 atm, and the reflux ratio is 1 , the pump B5 can be circulated into the high-pressure distillation column T3 until the mass concentration of water and cyclohexanol reaches more than 99.9wt%. 2.根据权利要求1所述的一种隔壁塔萃取精馏-变压精馏分离乙醇-环己醇-水的方法，其特征在于：所述步骤一中原料液经换热器B2预热后进入萃取精馏塔T1。2. the method for separating ethanol-cyclohexanol-water by a kind of bulkhead column extractive distillation-pressure swing distillation according to claim 1, it is characterized in that: in described step 1, raw material liquid is preheated through heat exchanger B2 Then enter the extractive distillation column T1. 3.根据权利要求1所述的一种隔壁塔萃取精馏-变压精馏分离乙醇-环己醇-水的方法，其特征在于：所述步骤一和步骤二中侧线采出料液为水和环己醇共沸物、乙二醇,步骤二中萃取精馏塔塔顶出料为质量浓度大于99.97wt％的乙醇。3. the method for separating ethanol-cyclohexanol-water by a kind of bulkhead column extractive rectification-pressure swing distillation according to claim 1, is characterized in that: described step 1 and step 2 middle side draw feed liquid is Water and cyclohexanol azeotrope, ethylene glycol, in step 2, the top discharge of the extractive distillation column is ethanol with a mass concentration greater than 99.97 wt%. 4.根据权利要求1所述的一种隔壁塔萃取精馏-变压精馏分离乙醇-环己醇-水的方法，其特征在于：所述步骤三中塔顶出料为水和环己醇共沸物，出料温度为59.94℃。4. the method for separating ethanol-cyclohexanol-water by a kind of bulkhead tower extractive rectification-pressure swing distillation according to claim 1, is characterized in that: in described step 3, tower top discharge is water and cyclohexane Alcohol azeotrope, the discharge temperature is 59.94 ℃. 5.根据权利要求1所述的一种隔壁塔萃取精馏-变压精馏分离乙醇-环己醇-水的方法，其特征在于：所述步骤五中塔底出料为质量浓度大于99.98wt％的水，出料温度为134.044℃，塔顶出料为在3atm下水和环己醇共沸物，出料温度为130.835℃。5. the method for separating ethanol-cyclohexanol-water by a kind of bulkhead tower extractive rectification-pressure swing rectification according to claim 1, is characterized in that: in described step 5, bottom discharge is that mass concentration is greater than 99.98 wt% of water, the discharge temperature is 134.044°C, and the top discharge is the azeotrope of water and cyclohexanol at 3 atm, and the discharge temperature is 130.835°C. 6.根据权利要求1所述的一种隔壁塔萃取精馏-变压精馏分离乙醇-环己醇-水的方法，其特征在于：所述步骤七中塔底出料是质量浓度大于99.98wt％的环己醇，出料温度为99.22℃，塔顶出料为在0.1atm下的水和环己醇共沸物，出料温度为45.24℃。6. the method for separating ethanol-cyclohexanol-water by a kind of bulkhead tower extractive rectification-pressure swing rectification according to claim 1, is characterized in that: in described step 7, the discharge at the bottom of the tower is that mass concentration is greater than 99.98 wt% of cyclohexanol, the discharge temperature is 99.22°C, and the top discharge is the azeotrope of water and cyclohexanol at 0.1 atm, and the discharge temperature is 45.24°C.
CN202110422352.6A 2021-04-20 2021-04-20 Method for separating ethanol, cyclohexanol and water by extractive distillation-pressure swing distillation of dividing wall tower Pending CN113072425A (en)

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113694556A (en) * 2021-09-30 2021-11-26 杭州浥能科技有限公司 Energy-saving device and method for separating cyclohexanol in hydration method

Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002045811A1 (en) * 2000-12-08 2002-06-13 Linde Aktiengesellschaft Method and device for separating a substance mixture into the component parts thereof by means of extractive distillation in a separating wall column

Patent Citations (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
WO2002045811A1 (en) * 2000-12-08 2002-06-13 Linde Aktiengesellschaft Method and device for separating a substance mixture into the component parts thereof by means of extractive distillation in a separating wall column

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
钱春键: ""DWC分离三组分混合物的研究"", 《化工进展》 *
马若君 等: "" 隔壁塔萃取精馏分离叔丁醇-乙醇-水共沸物的模拟与优化"", 《化工科技》 *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113694556A (en) * 2021-09-30 2021-11-26 杭州浥能科技有限公司 Energy-saving device and method for separating cyclohexanol in hydration method

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