CN106431836A - A process for coupling extraction, rectification and flash distillation to separate ethanol-water system - Google Patents
A process for coupling extraction, rectification and flash distillation to separate ethanol-water system Download PDFInfo
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- CN106431836A CN106431836A CN201610829622.4A CN201610829622A CN106431836A CN 106431836 A CN106431836 A CN 106431836A CN 201610829622 A CN201610829622 A CN 201610829622A CN 106431836 A CN106431836 A CN 106431836A
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- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 title claims abstract description 37
- 238000000034 method Methods 0.000 title claims abstract description 26
- 230000008878 coupling Effects 0.000 title claims abstract description 10
- 238000010168 coupling process Methods 0.000 title claims abstract description 10
- 238000005859 coupling reaction Methods 0.000 title claims abstract description 10
- 238000007701 flash-distillation Methods 0.000 title claims description 5
- 238000000605 extraction Methods 0.000 title description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 49
- 238000000895 extractive distillation Methods 0.000 claims abstract description 46
- 239000002608 ionic liquid Substances 0.000 claims abstract description 44
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 30
- -1 1-ethyl-3-methylimidazolium tetrafluoroborate Chemical compound 0.000 claims abstract description 12
- MKHFCTXNDRMIDR-UHFFFAOYSA-N cyanoiminomethylideneazanide;1-ethyl-3-methylimidazol-3-ium Chemical compound [N-]=C=NC#N.CCN1C=C[N+](C)=C1 MKHFCTXNDRMIDR-UHFFFAOYSA-N 0.000 claims abstract description 11
- 239000007788 liquid Substances 0.000 claims description 30
- 239000000203 mixture Substances 0.000 claims description 24
- 238000010992 reflux Methods 0.000 claims description 21
- 238000000926 separation method Methods 0.000 claims description 18
- 238000001704 evaporation Methods 0.000 claims description 5
- 230000008020 evaporation Effects 0.000 claims description 5
- 238000009833 condensation Methods 0.000 claims description 2
- 230000005494 condensation Effects 0.000 claims description 2
- 239000000463 material Substances 0.000 claims description 2
- 239000012498 ultrapure water Substances 0.000 claims description 2
- 239000003795 chemical substances by application Substances 0.000 abstract description 5
- 239000002904 solvent Substances 0.000 abstract description 5
- 238000005516 engineering process Methods 0.000 abstract description 4
- 235000019441 ethanol Nutrition 0.000 abstract 4
- 230000003247 decreasing effect Effects 0.000 abstract 1
- 238000004519 manufacturing process Methods 0.000 description 12
- 150000002500 ions Chemical group 0.000 description 7
- 230000000630 rising effect Effects 0.000 description 6
- 238000005265 energy consumption Methods 0.000 description 4
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical compound OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 239000002131 composite material Substances 0.000 description 2
- 229910017053 inorganic salt Inorganic materials 0.000 description 2
- 239000003960 organic solvent Substances 0.000 description 2
- 238000001577 simple distillation Methods 0.000 description 2
- IBZJNLWLRUHZIX-UHFFFAOYSA-N 1-ethyl-3-methyl-2h-imidazole Chemical class CCN1CN(C)C=C1 IBZJNLWLRUHZIX-UHFFFAOYSA-N 0.000 description 1
- VNXDRVGEKWGXAU-UHFFFAOYSA-N cyanocyanamide;1-ethyl-3-methyl-2h-imidazole Chemical compound N#CNC#N.CCN1CN(C)C=C1 VNXDRVGEKWGXAU-UHFFFAOYSA-N 0.000 description 1
- 230000006837 decompression Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 230000007812 deficiency Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000008018 melting Effects 0.000 description 1
- 238000002844 melting Methods 0.000 description 1
- 239000012046 mixed solvent Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000011084 recovery Methods 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000012827 research and development Methods 0.000 description 1
- 238000000638 solvent extraction Methods 0.000 description 1
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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
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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
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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
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- 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- 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
- Y02P20/54—Improvements relating to the production of bulk chemicals using solvents, e.g. supercritical solvents or ionic liquids
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- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
- Vaporization, Distillation, Condensation, Sublimation, And Cold Traps (AREA)
Abstract
Description
【技术领域】【Technical field】
本发明属于化工分离纯化领域，具体涉及一种萃取精馏与闪蒸分离乙醇-水物系的工艺。The invention belongs to the field of separation and purification of chemical industry, and in particular relates to a process for separating ethanol-water system by extractive distillation and flash distillation.
【背景技术】【Background technique】
在化工和制药行业中，乙醇为重要的溶剂及原料，需求不断增加。在工业生产中回收利用高纯度乙醇，这对于企业十分有经济意义。由于乙醇与水会形成共沸物，共沸温度为78.15℃，应用普通精馏方法难以对其进行有效的分离。近些年，由于离子液体具有极低蒸汽压、低熔点、热稳定性、无毒、无腐蚀性、可设计性等优良的性质，对于离子液体作为萃取剂的萃取精馏，扩大了研究与实践。随着离子液体的种类越来越多，选择对整个生产过程中有利的离子液体会解决节能、环境污染、设备投资等问题。In the chemical and pharmaceutical industries, ethanol is an important solvent and raw material, and the demand continues to increase. Recycling high-purity ethanol in industrial production is of great economic significance to enterprises. Since ethanol and water will form an azeotrope with an azeotropic temperature of 78.15°C, it is difficult to effectively separate them by ordinary distillation methods. In recent years, due to the excellent properties of ionic liquids such as extremely low vapor pressure, low melting point, thermal stability, non-toxicity, non-corrosiveness, and designability, the research and development of extractive distillation using ionic liquids as extraction agents has been expanded. practice. As there are more and more types of ionic liquids, choosing ionic liquids that are beneficial to the entire production process will solve problems such as energy saving, environmental pollution, and equipment investment.
专利(CN103073388A)公开了一种以离子液体和无机盐的复合萃取剂分离乙醇-水的方法，但该方法的萃取剂用量大，回流比较大，能耗较高，且因使用无机盐，对生产装置有腐蚀性。Patent (CN103073388A) discloses a method for separating ethanol-water with a composite extractant of ionic liquid and inorganic salt, but the extraction agent consumption of this method is large, the reflux ratio is large, and the energy consumption is high, and because of the use of inorganic salt, the Production equipment is corrosive.
专利(CN103435445A)公开了一种以离子液体或离子液体与有机溶剂的复合溶剂为萃取剂分离乙醇-水物系的方法，降低了能耗和生产成本，并且得到了高纯度乙醇，收率大于99.0％。专利(CN103601618A)涉及一种萃取精馏分离乙醇-水共沸物的方法，该方法采用乙二醇和氯化1-乙基-3-甲基咪唑为混合溶剂进行间歇萃取精馏操作，其应用实施例结果：乙醇产品纯度达99.5％。Patent (CN103435445A) discloses a method for separating ethanol-water system with ionic liquid or the composite solvent of ionic liquid and organic solvent as extractant, which reduces energy consumption and production cost, and obtains high-purity ethanol with a yield greater than 99.0%. The patent (CN103601618A) relates to a method for extracting and rectifying the separation of ethanol-water azeotrope, which uses ethylene glycol and chlorinated 1-ethyl-3-methylimidazole as a mixed solvent for intermittent extracting and rectifying operations. Example results: the purity of the ethanol product reaches 99.5%.
对于以离子液体作为萃取剂的萃取精馏过程，离子液体的选择是关键。上述现有的分离技术中存在的缺陷和不足是：忽略了离子液体的粘度、热稳定性等性质对生产过程的影响；分离过程的成本比较高；并在一定程度上影响了产品质量；工艺流程复杂。与传统的有机溶剂萃取分离过程相比，离子液体与水或有机物的分离只需采用简单的蒸馏而无需复杂的精馏过程，且离子液体可循环使用，几乎无损失。For the extractive distillation process using ionic liquid as extractant, the choice of ionic liquid is the key. The defects and deficiencies in the above-mentioned existing separation technology are: the influence of properties such as the viscosity and thermal stability of the ionic liquid on the production process is ignored; the cost of the separation process is relatively high; and the product quality is affected to a certain extent; the process The process is complicated. Compared with the traditional organic solvent extraction separation process, the separation of ionic liquid and water or organic matter only needs simple distillation without complicated rectification process, and the ionic liquid can be recycled with almost no loss.
开发乙醇-水混合物的绿色高效分离技术具有重要意义，有关分离乙醇-水混合物的文章和专利中尚未见公开发表的以离子液体1-乙基-3-甲基咪唑四氟硼酸盐和1-乙基-3-甲基咪唑二氰胺盐作为萃取剂进行萃取精馏与闪蒸耦合分离乙醇-水物系的工艺。本发明采用的离子液体因常温下液态状态、粘度较小而对整个生产过程有利。The development of green and high-efficiency separation technology for ethanol-water mixtures is of great significance. In the articles and patents related to the separation of ethanol-water mixtures, there is no published ionic liquid 1-ethyl-3-methylimidazolium tetrafluoroborate and 1 -Ethyl-3-methylimidazolium dicyanamide salt is used as an extractant to carry out a process of coupling extraction rectification and flash evaporation to separate ethanol-water systems. The ionic liquid adopted in the present invention is beneficial to the whole production process because of its liquid state and low viscosity at normal temperature.
【发明内容】【Content of invention】
本发明的目的是提供一种萃取精馏与闪蒸耦合分离乙醇-水物系的装置和方法，通过对乙醇-水物系采用离子液体萃取精馏分离出乙醇后，将萃取精馏塔塔釜含萃取剂和水混合物进行减压闪蒸，降低了生产操作过程中的能耗，该方法采用的设备投资少，操作条件易于控制，得到的乙醇纯度较高。The object of the present invention is to provide a device and method for extractive distillation and flash distillation coupling separation of ethanol-water system, after ethanol is separated by ionic liquid extraction and rectification for ethanol-water system, the extractive distillation column The kettle contains the extractant and water mixture for decompression and flash evaporation, which reduces the energy consumption in the production operation process. The method adopts less investment in equipment, and the operation conditions are easy to control, and the obtained ethanol has a higher purity.
本发明是通过以下技术方案加以实现的。The present invention is achieved through the following technical solutions.
一种萃取精馏与闪蒸分离乙醇-水物系的方法，该方法采用萃取精馏装置实施连续精馏操作，所述的萃取精馏装置包括萃取精馏塔，萃取精馏塔塔底连接再沸器，塔顶连接冷凝器，冷凝器之后连接接收罐，离子液体回收闪蒸罐，其特征在于包括以下过程：乙醇-水混合物由塔中下部进入萃取精馏塔内，萃取剂为离子液体溶剂，由塔上部进入塔内；在萃取精馏塔塔内，塔顶物流经冷凝器冷凝后，一部分液体返回塔内回流，一部分液体作为高纯度的乙醇产品采出；塔底物流经再沸器再沸后，一部分返回塔内，一部分进入闪蒸罐；A method for extractive distillation and flash distillation to separate ethanol-water systems, the method adopts an extractive distillation device to implement continuous rectification operation, the extractive distillation device includes an extractive distillation tower, and the bottom of the extractive distillation tower is connected to The reboiler, the top of the tower is connected to the condenser, the condenser is connected to the receiving tank, and the ionic liquid recovery flash tank is characterized in that it includes the following process: the ethanol-water mixture enters the extractive distillation tower from the middle and lower part of the tower, and the extractant is ion The liquid solvent enters the tower from the upper part of the tower; in the extractive distillation tower, after the tower top stream is condensed by the condenser, part of the liquid returns to the tower for reflux, and part of the liquid is extracted as high-purity ethanol product; After the boiler reboils, part of it returns to the tower, and part of it enters the flash tank;
在闪蒸罐内实现萃取剂和水的混合物的分离，在闪蒸罐塔顶得到高纯度的水，经冷凝后直接采出；在闪蒸罐底部得到质量分数为0.2-0.4％的离子液体，由闪蒸罐底部采出，循环回萃取精馏塔；其中所述萃取剂采用离子液体，具体包括1-乙基-3-甲基咪唑四氟硼酸盐和1-乙基-3-甲基咪唑二氰胺盐。The separation of the mixture of extractant and water is realized in the flash tank, and high-purity water is obtained at the top of the flash tank, which is directly extracted after condensation; and an ionic liquid with a mass fraction of 0.2-0.4% is obtained at the bottom of the flash tank , extracted from the bottom of the flash tank, and circulated back to the extractive distillation column; wherein the extractant is an ionic liquid, specifically including 1-ethyl-3-methylimidazolium tetrafluoroborate and 1-ethyl-3- Methylimidazole dicyanamide salt.
所述萃取精馏塔内径为Φ400-500mm，塔板数为35-45块，操作压力为1atm，乙醇-水混合物在第29-35块塔板进料，萃取剂在第3-6块塔板进料，塔顶温度为77.8-80℃，塔底温度为95-120℃，所述闪蒸罐采用减压操作，操作压力为0.1-0.2atm绝压，温度为108-112℃。The inner diameter of the extractive distillation tower is Φ400-500mm, the number of trays is 35-45, the operating pressure is 1atm, the ethanol-water mixture is fed in the 29th-35th tray, and the extractant is fed in the 3rd-6th column Plate feed, the temperature at the top of the tower is 77.8-80°C, the temperature at the bottom of the tower is 95-120°C, the flash tank is operated under reduced pressure, the operating pressure is 0.1-0.2atm absolute pressure, and the temperature is 108-112°C.
所述的离子液体溶剂优选为1-乙基-3-甲基咪唑四氟硼酸盐和1-乙基-3-甲基咪唑二氰胺盐。The ionic liquid solvent is preferably 1-ethyl-3-methylimidazolium tetrafluoroborate and 1-ethyl-3-methylimidazolium dicyanamide.
所述的乙醇-水混合物物料中两种成分任意比例。The ratio of the two components in the ethanol-water mixture material is arbitrary.
所述的乙醇-水物系中两种成分质量比优选为乙醇：水＝0.25-1。The mass ratio of the two components in the ethanol-water system is preferably ethanol:water=0.25-1.
本发明的有益效果为：所述离子液体能提高乙醇-水物系中的乙醇的相对挥发度，降低了溶剂比。当离子液体的质量分数达到17％-50％时，可使乙醇-水的共沸点消失。由应用实施例知，当离子液体与乙醇-水物系的质量比为1:3时，即可很好地进行萃取精馏，得到大于99.5％的乙醇。对于乙醇-水物系，离子液体1-乙基-3-甲基咪唑四氟硼酸盐和1-乙基-3-甲基咪唑二氰胺盐与水有较好的互溶性，可通过化学亲和力、氢键力等与水作用，提高乙醇对于水的相对挥发度，从而离子液体加入量较少，利用简单的蒸馏回收使用离子液体，降低了分离过程的能耗与投资。The beneficial effects of the invention are: the ionic liquid can increase the relative volatility of ethanol in the ethanol-water system and reduce the solvent ratio. When the mass fraction of the ionic liquid reaches 17%-50%, the azeotropic point of ethanol-water can disappear. It is known from the application examples that when the mass ratio of the ionic liquid to the ethanol-water system is 1:3, the extractive distillation can be carried out well, and ethanol of more than 99.5% can be obtained. For the ethanol-water system, the ionic liquid 1-ethyl-3-methylimidazolium tetrafluoroborate and 1-ethyl-3-methylimidazolium dicyanamide salt have better miscibility with water, and can be passed Chemical affinity, hydrogen bond force, etc. interact with water to increase the relative volatility of ethanol to water, so that the amount of ionic liquid added is small, and the ionic liquid is recovered and used by simple distillation, which reduces the energy consumption and investment of the separation process.
【附图说明】【Description of drawings】
图1：本发明所述的一种萃取精馏与闪蒸耦合分离乙醇-水物系的流程示意图。Figure 1: A schematic flow chart of the coupling separation of ethanol-water system by extractive distillation and flash evaporation according to the present invention.
其中，T1–萃取精馏塔；T2–闪蒸罐；F1–萃取精馏塔原料进料口；F2–萃取剂进料口；B1–萃取精馏塔塔底出料口；B2–循环萃取剂出口；D1–乙醇产品出口；D2–水出口；1–再沸器；2,3–冷凝器。Among them, T1—extractive distillation tower; T2—flash tank; F1—feed inlet of extractive distillation tower; F2—feed inlet of extractant; B1—bottom outlet of extractive distillation tower; B2—circulation extraction Agent outlet; D1-ethanol product outlet; D2-water outlet; 1-reboiler; 2,3-condenser.
【具体实施方式】【detailed description】
实施例1：萃取精馏塔的内径为Φ500mm、理论板数为40、操作压力为101.325kPa、操作回流比为1.8、塔顶温度控制在77℃、塔釜温度为95℃，25℃的离子液体1-乙基-3-甲基咪唑四氟硼酸盐由第6块板进入，25℃的质量分数为20％乙醇-80％水混合物由第34块板以1000kg/h的流量进入，控制离子液体与乙醇-水的质量比为1:3，塔顶上升蒸汽由冷凝器进行冷凝。回流液由萃取精馏塔的塔顶回流，采出液为质量分数99.5％的乙醇。萃取精馏塔的塔釜为1-乙基-3-甲基咪唑四氟硼酸盐和水的混合物，回流液经再沸器于126℃再沸后回流，其余进入闪蒸罐，操作压力为0.12atm、闪蒸罐温度控制在112℃。闪蒸罐的底部为质量分数为0.4％水的离子液体。Example 1: The inner diameter of the extractive distillation tower is Φ500mm, the number of theoretical plates is 40, the operating pressure is 101.325kPa, the operating reflux ratio is 1.8, the temperature at the top of the tower is controlled at 77°C, the temperature at the bottom of the tower is 95°C, and the ions at 25°C The liquid 1-ethyl-3-methylimidazolium tetrafluoroborate enters from the sixth plate, and the mass fraction of 25°C is 20% ethanol-80% water mixture enters from the 34th plate at a flow rate of 1000kg/h. The mass ratio of the ionic liquid to ethanol-water is controlled to be 1:3, and the steam rising from the top of the tower is condensed by the condenser. The reflux liquid is refluxed from the top of the extractive distillation tower, and the production liquid is ethanol with a mass fraction of 99.5%. The tower kettle of the extractive distillation tower is a mixture of 1-ethyl-3-methylimidazolium tetrafluoroborate and water. The reflux liquid is reboiled at 126°C by the reboiler and then refluxed, and the rest enters the flash tank. The operating pressure It is 0.12atm, and the flash tank temperature is controlled at 112°C. The bottom of the flash tank is an ionic liquid with a mass fraction of 0.4% water.
实施例2：萃取精馏塔的内径为Φ400mm、理论板数为35、操作压力为101.325kPa、操作回流比为2.1、塔顶温度控制在77.8℃、塔釜温度为109℃，25℃的离子液体1-乙基-3-甲基咪唑四氟硼酸盐由第6块板进入，25℃的质量分数为30％乙醇-70％水混合物由第29块板以1000kg/h的流量进入，控制离子液体与乙醇-水的质量比为1:2.5，塔顶上升蒸汽由冷凝器进行冷凝。回流液由萃取精馏塔的塔顶回流，采出液为质量分数99.6％的乙醇。萃取精馏塔的塔釜为1-乙基-3-甲基咪唑四氟硼酸盐和水的混合物，回流液经再沸器于120℃再沸后回流，其余进入闪蒸罐，操作压力为0.15atm、闪蒸罐温度控制在109℃。闪蒸罐的底部为质量分数为0.3％水的离子液体。Example 2: The inner diameter of the extractive distillation tower is Φ400mm, the number of theoretical plates is 35, the operating pressure is 101.325kPa, the operating reflux ratio is 2.1, the temperature at the top of the tower is controlled at 77.8°C, the temperature at the bottom of the tower is 109°C, and the ions at 25°C The liquid 1-ethyl-3-methylimidazolium tetrafluoroborate enters from the 6th plate, and the mass fraction of 25°C is 30% ethanol-70% water mixture enters from the 29th plate with a flow rate of 1000kg/h. The mass ratio of ionic liquid to ethanol-water is controlled to be 1:2.5, and the steam rising from the tower top is condensed by the condenser. The reflux liquid is refluxed from the top of the extractive distillation tower, and the production liquid is ethanol with a mass fraction of 99.6%. The tower kettle of the extractive distillation tower is a mixture of 1-ethyl-3-methylimidazolium tetrafluoroborate and water. The reflux liquid is reboiled at 120°C through the reboiler and then refluxed, and the rest enters the flash tank. The operating pressure is is 0.15atm, and the flash tank temperature is controlled at 109°C. The bottom of the flash tank is an ionic liquid with a mass fraction of 0.3% water.
实施例3：萃取精馏塔的内径为Φ400mm、理论板数为35、操作压力为101.325kPa、操作回流比为2.6、塔顶温度控制在77.8℃、塔釜温度为107℃，25℃的离子液体1-乙基-3-甲基咪唑四氟硼酸盐由第6块板进入，25℃的质量分数为40％乙醇-60％水混合物由第30块板以1000kg/h的流量进入，控制离子液体与乙醇-水的质量比为1:2，塔顶上升蒸汽由冷凝器进行冷凝。回流液由萃取精馏塔的塔顶回流，采出液为质量分数99.6％的乙醇。萃取精馏塔的塔釜为1-乙基-3-甲基咪唑四氟硼酸盐和水的混合物，回流液经再沸器于120℃再沸后回流，其余闪蒸罐，操作压力为0.18atm、闪蒸罐温度控制在110℃。闪蒸罐的底部为质量分数为0.3％水的离子液体。Example 3: The inner diameter of the extractive distillation tower is Φ400mm, the number of theoretical plates is 35, the operating pressure is 101.325kPa, the operating reflux ratio is 2.6, the temperature at the top of the tower is controlled at 77.8°C, the temperature at the bottom of the tower is 107°C, and the ions at 25°C The liquid 1-ethyl-3-methylimidazolium tetrafluoroborate enters from the 6th plate, and the mass fraction of 25°C is 40% ethanol-60% water mixture enters from the 30th plate with a flow rate of 1000kg/h. The mass ratio of the ionic liquid to ethanol-water is controlled to be 1:2, and the steam rising from the top of the tower is condensed by the condenser. The reflux liquid is refluxed from the top of the extractive distillation tower, and the production liquid is ethanol with a mass fraction of 99.6%. The tower kettle of the extractive distillation tower is a mixture of 1-ethyl-3-methylimidazolium tetrafluoroborate and water, the reflux liquid is reboiled at 120°C through the reboiler and then refluxed, and the operating pressure of the remaining flash tanks is 0.18atm, flash tank temperature is controlled at 110°C. The bottom of the flash tank is an ionic liquid with a mass fraction of 0.3% water.
实施例4：萃取精馏塔的内径为Φ500mm、理论板数为40、操作压力为101.325kPa、操作回流比为1.2、塔顶温度控制在78.0℃、塔釜温度为119℃，25℃的离子液体1-乙基-3-甲基咪唑二氰胺盐由第5块板进入，25℃的质量分数为20％乙醇-80％水混合物由第32块板以1000kg/h的流量进入，控制离子液体与乙醇-水的质量比为1:4，塔顶上升蒸汽由冷凝器进行冷凝。回流液由萃取精馏塔的塔顶回流，采出液为质量分数99.8％的乙醇。萃取精馏塔的塔釜为1-乙基-3-甲基咪唑二氰胺盐和水的混合物，回流液经再沸器于127℃再沸后回流，其余进入闪蒸罐，操作压力为0.14atm、闪蒸罐温度控制在108℃。闪蒸罐的底部为质量分数为0.1％水的离子液体。Example 4: The inner diameter of the extractive distillation tower is Φ500mm, the number of theoretical plates is 40, the operating pressure is 101.325kPa, the operating reflux ratio is 1.2, the temperature at the top of the tower is controlled at 78.0°C, the temperature at the bottom of the tower is 119°C, and the ions at 25°C The liquid 1-ethyl-3-methylimidazolium dicyanamide salt enters from the fifth plate, and the mass fraction of 25°C is 20% ethanol-80% water mixture enters from the 32nd plate with a flow rate of 1000kg/h. The mass ratio of ionic liquid to ethanol-water is 1:4, and the steam rising from the top of the tower is condensed by the condenser. The reflux liquid is refluxed from the top of the extractive distillation tower, and the production liquid is ethanol with a mass fraction of 99.8%. The tower kettle of the extractive distillation tower is a mixture of 1-ethyl-3-methylimidazolium dicyanamide salt and water. The reflux liquid is reboiled at 127°C through the reboiler and then refluxed, and the rest enters the flash tank. The operating pressure is 0.14atm, flash tank temperature is controlled at 108°C. The bottom of the flash tank is an ionic liquid with a mass fraction of 0.1% water.
实施例5：萃取精馏塔的内径为Φ500mm、理论板数为45、操作压力为101.325kPa、操作回流比为1.8、塔顶温度控制在80℃，塔釜温度为112℃，25℃的离子液体1-乙基-3-甲基咪唑二氰胺盐由第3块板进入，25℃的质量分数为30％乙醇-70％水混合物由第31块板以1000kg/h的流量进入，控制离子液体与乙醇-水的质量比为1:3，塔顶上升蒸汽由冷凝器进行冷凝。回流液由萃取精馏塔的塔顶回流，采出液为质量分数99.9％的乙醇。萃取精馏塔的塔釜为1-乙基-3-甲基咪唑二氰胺盐和水的混合物，回流液经再沸器于126℃再沸后回流，其余进入闪蒸罐，操作压力为0.16atm、闪蒸罐温度控制在120℃。闪蒸罐的底部为质量分数为0.1％水的离子液体。Example 5: The inner diameter of the extractive distillation tower is Φ500mm, the number of theoretical plates is 45, the operating pressure is 101.325kPa, the operating reflux ratio is 1.8, the temperature at the top of the tower is controlled at 80°C, the temperature at the bottom of the tower is 112°C, and the ions at 25°C The liquid 1-ethyl-3-methylimidazolium dicyanamide salt enters from the third plate, and the mass fraction of 25°C is 30% ethanol-70% water mixture enters from the 31st plate with a flow rate of 1000kg/h. The mass ratio of ionic liquid to ethanol-water is 1:3, and the steam rising from the top of the tower is condensed by the condenser. The reflux liquid is refluxed from the top of the extractive distillation tower, and the production liquid is ethanol with a mass fraction of 99.9%. The tower kettle of the extractive distillation tower is a mixture of 1-ethyl-3-methylimidazolium dicyanamide salt and water. The reflux liquid is reboiled at 126°C through the reboiler and then refluxed, and the rest enters the flash tank. The operating pressure is 0.16atm, flash tank temperature is controlled at 120°C. The bottom of the flash tank is an ionic liquid with a mass fraction of 0.1% water.
实施例6：萃取精馏塔的内径为Φ500mm、理论板数为40、操作压力为101.325kPa、操作回流比为2.0、塔顶温度控制在77.9℃、塔釜温度为120℃，25℃的离子液体1-乙基-3-甲基咪唑二氰胺盐由第4块板进入，25℃的质量分数为40％乙醇-60％水混合物由第35块板以1000kg/h的流量进入，控制离子液体与乙醇-水的质量比为1:3，塔顶上升蒸汽由冷凝器进行冷凝。回流液由萃取精馏塔的塔顶回流，采出液为质量分数99.9％的乙醇。萃取精馏塔的塔釜为1-乙基-3-甲基咪唑二氰胺盐和水的混合物，回流液经再沸器于126℃再沸后回流，其余进入闪蒸罐，操作压力为0.2atm、闪蒸罐温度控制在112℃。蒸罐的底部为质量分数为0.2％水的离子液体。Example 6: The inner diameter of the extractive distillation tower is Φ500mm, the number of theoretical plates is 40, the operating pressure is 101.325kPa, the operating reflux ratio is 2.0, the temperature at the top of the tower is controlled at 77.9°C, the temperature of the tower bottom is 120°C, and the ions at 25°C The liquid 1-ethyl-3-methylimidazolium dicyanamide salt enters from the 4th plate, and the mass fraction of 25°C is 40% ethanol-60% water mixture enters from the 35th plate with a flow rate of 1000kg/h, the control The mass ratio of ionic liquid to ethanol-water is 1:3, and the steam rising from the top of the tower is condensed by the condenser. The reflux liquid is refluxed from the top of the extractive distillation tower, and the production liquid is ethanol with a mass fraction of 99.9%. The tower kettle of the extractive distillation tower is a mixture of 1-ethyl-3-methylimidazolium dicyanamide salt and water. The reflux liquid is reboiled at 126°C through the reboiler and then refluxed, and the rest enters the flash tank. The operating pressure is 0.2atm, flash tank temperature is controlled at 112°C. The bottom of the steamer is an ionic liquid with a mass fraction of 0.2% water.
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| CN112795397A (en) * | 2019-11-14 | 2021-05-14 | 中国石油天然气股份有限公司 | Composite solvent for separating cyclane and aromatic hydrocarbon from naphtha |
| CN113248378A (en) * | 2021-05-31 | 2021-08-13 | 鹤壁腾飞清洁能源有限公司 | A kind of system of extracting and rectifying methyl acetate and ethanol and using method thereof |
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| CN110028388A (en) * | 2019-05-23 | 2019-07-19 | 山东科技大学 | A method of with hydrophilic ionic-liquid separation of extractive distillation tetrafluoropropanol and water azeotropic mixture |
| CN110028388B (en) * | 2019-05-23 | 2023-01-17 | 山东科技大学 | A method for extracting and rectifying separation of tetrafluoropropanol and water azeotrope with hydrophilic ionic liquid |
| CN112795397A (en) * | 2019-11-14 | 2021-05-14 | 中国石油天然气股份有限公司 | Composite solvent for separating cyclane and aromatic hydrocarbon from naphtha |
| CN112795397B (en) * | 2019-11-14 | 2023-02-07 | 中国石油天然气股份有限公司 | Composite solvent for separating cyclane and aromatic hydrocarbon from naphtha |
| CN113248378A (en) * | 2021-05-31 | 2021-08-13 | 鹤壁腾飞清洁能源有限公司 | A kind of system of extracting and rectifying methyl acetate and ethanol and using method thereof |
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