CN103435445A - Method for separating mixture of ethanol alcohol and water - Google Patents
Method for separating mixture of ethanol alcohol and water Download PDFInfo
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- CN103435445A CN103435445A CN2013103658117A CN201310365811A CN103435445A CN 103435445 A CN103435445 A CN 103435445A CN 2013103658117 A CN2013103658117 A CN 2013103658117A CN 201310365811 A CN201310365811 A CN 201310365811A CN 103435445 A CN103435445 A CN 103435445A
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- 238000000034 method Methods 0.000 title claims abstract description 50
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 title claims abstract description 50
- 239000000203 mixture Substances 0.000 title claims abstract description 23
- IDGUHHHQCWSQLU-UHFFFAOYSA-N ethanol;hydrate Chemical compound O.CCO IDGUHHHQCWSQLU-UHFFFAOYSA-N 0.000 title claims abstract description 14
- AZHSSKPUVBVXLK-UHFFFAOYSA-N ethane-1,1-diol Chemical compound CC(O)O AZHSSKPUVBVXLK-UHFFFAOYSA-N 0.000 title abstract 4
- 239000003795 chemical substances by application Substances 0.000 claims abstract description 61
- 239000002994 raw material Substances 0.000 claims abstract description 33
- 239000002608 ionic liquid Substances 0.000 claims abstract description 22
- 239000002904 solvent Substances 0.000 claims abstract description 22
- 239000003960 organic solvent Substances 0.000 claims abstract description 12
- 238000000605 extraction Methods 0.000 claims description 95
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 63
- 238000011084 recovery Methods 0.000 claims description 53
- 238000010992 reflux Methods 0.000 claims description 22
- LYCAIKOWRPUZTN-UHFFFAOYSA-N Ethylene glycol Chemical group OCCO LYCAIKOWRPUZTN-UHFFFAOYSA-N 0.000 claims description 12
- 239000000463 material Substances 0.000 claims description 12
- PEDCQBHIVMGVHV-UHFFFAOYSA-N Glycerine Chemical compound OCC(O)CO PEDCQBHIVMGVHV-UHFFFAOYSA-N 0.000 claims description 9
- -1 imidazol ion Chemical class 0.000 claims description 9
- 239000007788 liquid Substances 0.000 claims description 9
- IBZJNLWLRUHZIX-UHFFFAOYSA-N 1-ethyl-3-methyl-2h-imidazole Chemical compound CCN1CN(C)C=C1 IBZJNLWLRUHZIX-UHFFFAOYSA-N 0.000 claims description 6
- BTBUEUYNUDRHOZ-UHFFFAOYSA-N Borate Chemical group [O-]B([O-])[O-] BTBUEUYNUDRHOZ-UHFFFAOYSA-N 0.000 claims description 6
- ZXLOSLWIGFGPIU-UHFFFAOYSA-N 1-ethyl-3-methyl-1,2-dihydroimidazol-1-ium;acetate Chemical compound CC(O)=O.CCN1CN(C)C=C1 ZXLOSLWIGFGPIU-UHFFFAOYSA-N 0.000 claims description 4
- ZMXDDKWLCZADIW-UHFFFAOYSA-N N,N-Dimethylformamide Chemical compound CN(C)C=O ZMXDDKWLCZADIW-UHFFFAOYSA-N 0.000 claims description 4
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims description 3
- 150000001298 alcohols Chemical class 0.000 claims description 3
- 229910052799 carbon Inorganic materials 0.000 claims description 3
- FXHOOIRPVKKKFG-UHFFFAOYSA-N N,N-Dimethylacetamide Chemical compound CN(C)C(C)=O FXHOOIRPVKKKFG-UHFFFAOYSA-N 0.000 claims description 2
- SECXISVLQFMRJM-UHFFFAOYSA-N N-Methylpyrrolidone Chemical class CN1CCCC1=O SECXISVLQFMRJM-UHFFFAOYSA-N 0.000 claims description 2
- 238000009835 boiling Methods 0.000 claims description 2
- 150000002500 ions Chemical class 0.000 claims description 2
- 239000003021 water soluble solvent Substances 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 abstract description 12
- 238000005265 energy consumption Methods 0.000 abstract description 9
- 238000000895 extractive distillation Methods 0.000 abstract description 3
- 150000001875 compounds Chemical class 0.000 abstract 1
- 229960004756 ethanol Drugs 0.000 description 28
- 238000005516 engineering process Methods 0.000 description 8
- 238000000926 separation method Methods 0.000 description 6
- NJMWOUFKYKNWDW-UHFFFAOYSA-N 1-ethyl-3-methylimidazolium Chemical compound CCN1C=C[N+](C)=C1 NJMWOUFKYKNWDW-UHFFFAOYSA-N 0.000 description 5
- 239000002131 composite material Substances 0.000 description 4
- 239000000126 substance Substances 0.000 description 4
- 229910017053 inorganic salt Inorganic materials 0.000 description 3
- 238000010533 azeotropic distillation Methods 0.000 description 2
- 239000012141 concentrate Substances 0.000 description 2
- 239000000284 extract Substances 0.000 description 2
- 238000000409 membrane extraction Methods 0.000 description 2
- 238000002203 pretreatment Methods 0.000 description 2
- IQQRAVYLUAZUGX-UHFFFAOYSA-N 1-butyl-3-methylimidazolium Chemical compound CCCCN1C=C[N+](C)=C1 IQQRAVYLUAZUGX-UHFFFAOYSA-N 0.000 description 1
- WXMVWUBWIHZLMQ-UHFFFAOYSA-N 3-methyl-1-octylimidazolium Chemical compound CCCCCCCCN1C=C[N+](C)=C1 WXMVWUBWIHZLMQ-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000005260 corrosion Methods 0.000 description 1
- 230000007797 corrosion Effects 0.000 description 1
- 229960000935 dehydrated alcohol Drugs 0.000 description 1
- 238000004821 distillation Methods 0.000 description 1
- 238000004134 energy conservation Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 231100000252 nontoxic Toxicity 0.000 description 1
- 230000003000 nontoxic effect Effects 0.000 description 1
- 238000002360 preparation method Methods 0.000 description 1
- 238000000746 purification Methods 0.000 description 1
- 230000008929 regeneration Effects 0.000 description 1
- 238000011069 regeneration method Methods 0.000 description 1
- 238000005185 salting out Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
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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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- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention provides a method for separating a mixture of ethanol alcohol and water. The method comprises the following steps: the mixture of the ethanol alcohol and water at any ratio is used as a raw material, an ionic liquid or a compound solvent comprising the ionic liquid and an organic solvent is used as an extracting agent, the ethanol alcohol and the water are sequentially extracted after the raw material is processed in the extractive distillation stage and the extracting agent recovering stage, and the extracting agent can be recycled after being extracted in the recovering stage. The method provided by the invention has the advantages of low energy consumption, no pollution to the environment, high production purity, easiness in industrialization, low equipment cost, good economic return and the like.
Description
Technical field
The invention belongs to the separation technology field of ethanol-water mixture, particularly relate to a kind of method of separating alcohol-water mixture.
Background technology
Ethanol is a kind of important chemical industry synthesis material and organic solvent, due to of many uses, demand is large, its preparation technology and method of purification have become academia and industrial study hotspot.Especially the alcohol-water system forms azeotrope, and conventional distillation is difficult to obtain high purity ethanol, should adopt special extract rectification, as azeotropic distillation, and extracting rectifying and membrane extraction technology.Because the azeotropic distillation energy consumption is larger; In the membrane extraction technology, the cost of film is high, regeneration is difficult, limits its industrialization.So, industrial normal employing separation of extractive distillation alcohol-water system.
Chinese patent CN1323773A discloses a kind of with ethylene glycol, Reaction Separation agent (Ca (OH)
2deng), salting-out agent (CaCl
2, K
2cO
3deng) mixture be the method that the double solvents extracting rectifying is produced dehydrated alcohol, at first this method is concentrated into the alcohol-water stripping of low-purity 70%-80%, then, with the double solvents purifying ethanol, obtains the ethanol that purity is greater than 99.8%.The method main drawback: material purity is had relatively high expectations, and the low levels raw material needs the pre-treatment concentrate, and production cost is high; Double solvents forms complicated, has increased the control parameter of technique; Extraction agent, containing inorganic salt, is corrosive to production equipment.
Lie group is given birth to and is waited (modern chemical industry, 2012,32 (2), 69) to utilize 1,3-methylimidazole dimethyl phosphate salt is cooked extraction agent, obtains the ethanol of massfraction 99.5%, but optimum reflux ratio 3-4, energy consumption is larger, and requiring raw material is 95% ethanol, and material purity is had relatively high expectations, and production cost is high.
Wang Wenhua, Feng Yongmei etc. (brewing science and technology, the 2nd phase in 2006,34) disclose [EMIM]
+[BF4]
-the impact that ethanol-water system is balanced each other, they have measured [EMIM] under 101.3kPa+[BF4]-mole fraction x3=0.1 with improved Othmer Vapor-Liquid Equilibrium Still, 0.2 the vapor-liquid equilibrium data of alcohol-water-[EMIM]+[BF4]-system, and carried out association with the NRTL model, average deviation is 0.967% as a result.Experiment shows: [EMIM]+[BF4]-can eliminate the azeotropic point of ethanol-water system can be used as the solvent of separation of extractive distillation ethanol-water system.But the possibility of 1-ethyl-3-methylimidazole a tetrafluoro borate as the ethanol-water system extraction agent only has been described in literary composition, concrete operations parameter and step do not explained.
Similar to the present invention is that Chinese patent CN103073388A discloses a kind of method that mixture of take ionic liquid and inorganic salt is the composite extractant separating alcohol-water, but the Solvent quantity of the method large (solvent ratio 0.5-6.0), reflux ratio is large (reflux ratio 1.0-5.0), energy consumption is higher, and introduced inorganic salt, production equipment is corrosive.
Summary of the invention
The object of the invention is to overcome in above-mentioned technology the shortcomings such as energy consumption is large, equipment corrosion, production cost height, provide a kind of energy consumption low, corrosion-free, simple to operate, to the material purity no requirement (NR), extraction agent easily reclaims the method for free of contamination separating alcohol-water, and the double solvents that adopts ionic liquid or ionic liquid and organic solvent to form is extraction agent separating alcohol-water Wuxi, and the production equipment that is applied to described method is provided.
For solving the problems of the technologies described above, the technical solution used in the present invention is:
A kind of method of separating alcohol-water mixture, described method adopts continuity operation or intermittent operation: described continuity operation comprises rectifying tower and recovery tower, that to take the ethanol-water mixture of arbitrary proportion be raw material, the double solvents that ionic liquid or ionic liquid and organic solvent form of take is extraction agent, raw material is by 15-45 piece theoretical tray, extraction agent is entered into respectively in the described rectifying tower that 25-50 piece theoretical plate number is housed by 2-25 piece theoretical stage, ethanol is by the extraction of described rectifying tower tower top, extraction agent-water mixed liquid is entered to described recovery tower by the recovery tower opening for feed after by described tower bottom of rectifying tower extraction, water is by described recovery tower overhead extraction, extraction agent recycles after by the extraction of described recovery tower tower reactor,
Described intermittent operation comprises rectifying tower, be divided into extracting rectifying stage and extraction agent recovery stage, the described extracting rectifying stage is that to take the ethanol-water mixture of arbitrary proportion be raw material, the double solvents that ionic liquid or ionic liquid and organic solvent form of take is extraction agent, raw material is by 15-45 piece theoretical tray, extraction agent is entered into respectively by 2-25 piece theoretical stage in the described rectifying tower that 25-50 piece theoretical plate number is housed or directly raw material is added in the tower reactor of rectifying tower, extraction agent is entered in the described rectifying tower that 24-50 piece theoretical plate number is housed by 2-25 piece theoretical stage, ethanol by the extraction of described rectifying tower tower top after, extraction agent-water mixed liquid is stayed to tower bottom of rectifying tower and carry out the operation of extraction agent recovery stage in rectifying tower, water is by the extraction of described rectifying tower tower top, extraction agent recycles by described tower bottom of rectifying tower extraction and after collecting.
Described ionic liquid is the non-AlCl that positively charged ion is imidazol ion
3the mixture of one or more in the type ionic liquid.
Preferably, described ionic liquid is 1-ethyl-3-methylimidazole acetate ([EMIM] OAc), 1-ethyl-3-methylimidazole a tetrafluoro borate ([EMIM] BF
4), 1-butyl-3-methyl imidazolium tetrafluoroborate ([BMIM] BF
4), 1-octyl group-3-methyl imidazolium tetrafluoroborate ([OMIM] BF
4) in one or more mixture.
Described organic solvent is low carbon number alcohols or DMF or N,N-dimethylacetamide or N-Methyl pyrrolidone class high boiling point and water-soluble solvent preferably.
Preferably, described organic solvent is ethylene glycol or glycerol.
Described in described continuity operating process, the rectifying tower working pressure is 65-101.3kPa, and reflux ratio is 0.2-4.0, and the add-on of extraction agent and the mass ratio of raw material are (0.2-4.8): 1, and described recovery tower working pressure is 45-101.3kPa;
In described intermittent operation flow process, the described rectifying tower working pressure in extracting rectifying stage is 65-101.3kPa, reflux ratio is 0.2-4.0, the add-on of extraction agent and the mass ratio of raw material are (0.2-4.8): 1, and the described rectifying tower working pressure of extraction recovery stage is 45-101.3kPa.
Preferably, described in described continuity operating process, the rectifying tower working pressure is 101.3kPa, and reflux ratio is 0.1-1.0, and the add-on of extraction agent and the mass ratio of raw material are (0.2-1.0): 1, and described recovery tower working pressure is 45-90kPa;
In described intermittent operation flow process, the described rectifying tower working pressure in extracting rectifying stage is 101.3kPa, reflux ratio is 0.1-1.0, the add-on of extraction agent and the mass ratio of raw material are (0.2-1.0): 1, and the described rectifying tower working pressure of extraction recovery stage is 45-90kPa.
Another object of the present invention is to provide a kind of rectifier unit for described method, it is characterized in that: the rectifier unit of described continuity operation comprises rectifying tower and the recovery tower that 25-50 piece theoretical plate number is housed, the discharge port of the tower reactor of described rectifying tower is connected with the opening for feed of described recovery tower, the discharge port of described recovery tower bottom is connected with the extractant feed mouth of described rectifying tower, and the material inlet of described rectifying tower, extractant feed mouth are located at respectively 15-45 piece theoretical tray place and the 2-25 piece theoretical tray place of described rectifying tower; The opening for feed of described recovery tower is located at described recovery tower middle and lower part;
The rectifier unit of described intermittent operation comprises the rectifying tower that 25-50 piece theoretical plate number is housed, and the material inlet of described rectifying tower, extractant feed mouth are located at respectively 15-45 piece theoretical tray place and the 2-25 piece theoretical tray place of described rectifying tower.
The beneficial effect that the present invention has is:
It is extraction agent that the double solvents that ionic liquid or ionic liquid and organic solvent form is take in the present invention, and the relative volatility that can significantly increase alcohol-water realizes the high efficiency separation of system.With the disclosed method of Chinese patent CN1323773A, compare, novel method of the present invention can be processed the mixture of the alcohol-water of any composition, saved because raw material extracts concentrated production cost and the energy consumption caused, and extraction agent used is corrosion-free to production equipment, safe.With the method in " modern chemical industry " article, compare, novel method of the present invention adopts less reflux ratio (the better reflux ratio of rectifying tower≤1 in the present invention) can obtain the alcohol product that purity is greater than 99.9%, energy-conservation more than 70%, and the low-purity raw material, without the pre-treatment concentrate, significantly reduces production costs.With the disclosed method of Chinese patent CN103073388A, compare, novel method Solvent quantity of the present invention and reflux ratio all significantly reduce (in the present invention preferred solvents than 0.2-1, better reflux ratio 0.1-1), have reduced energy consumption and production cost, and extraction agent is corrosion-free, safe.The purity of alcohol of using novel method of the present invention to obtain is greater than 99.9%, and yield is greater than 99.0%, all higher than aforementioned three kinds of process programs.
In addition, it is extraction agent that method of the present invention adopts green solvent ionic liquid and low carbon number alcohols, nontoxic, corrosion-free, pollution-free, easily reclaims, and thermostability and chemical stability are good, lossless, can be recycled; Production equipment provided by the invention is simple, easy handling, and treatment capacity is large, and energy consumption is low, good in economic efficiency.
The accompanying drawing explanation
Fig. 1 is that in the present invention, the continuity for separating of ethanol-water mixture operates rectifier unit.
In figure, the T1-rectifying tower; The T2-recovery tower; F1-rectifying tower material inlet; F2-rectifying tower extractant feed mouth; The tower top discharge port of P1-rectifying tower; The tower top discharge port of P2-recovery tower; S1-tower bottom of rectifying tower discharge port; The tower reactor discharge port of S2-recovery tower; 1,2-tower reactor reboiler; 3,4-overhead condenser.
Fig. 2 is for separating of the intermittent operation rectifier unit of ethanol-water mixture in the present invention.
In figure, the T1-rectifying tower; F1-rectifying tower material inlet; The tower top discharge port of P1-rectifying tower; S1-tower bottom of rectifying tower discharge port; 1-tower reactor reboiler; The 3-overhead condenser.
During use, can be according to shown in Fig. 1, adopt the continuity operation, the alcohol-water raw material is entered in rectifying tower T1 from the material inlet F1 of the 15-45 piece theoretical tray of rectifying tower T1 that 25-50 piece theoretical plate number is housed; Extraction agent enters in rectifying tower T1 from the extractant feed mouth F2 of the 2-25 piece theoretical tray of rectifying tower, and after extracting rectifying, ethanol is from the tower top discharge port P1 extraction of rectifying tower T1; After the discharge port S1 extraction of extraction agent-water mixed liquid by tower bottom of rectifying tower, enter in recovery tower T2, after separation, water is from the tower top discharge port P2 extraction of recovery tower T2; Extraction agent continues to join in rectifying tower by the extractant feed mouth F2 of rectifying tower from the discharge port S2 extraction of recovery tower tower reactor, recycles.
Can also be according to shown in Fig. 2, adopt intermittent operation, comprise extracting rectifying stage and extraction agent recovery stage, the extracting rectifying stage can adopt two kinds of feeding manners, a kind of is that the alcohol-water raw material is entered in rectifying tower T1 from the material inlet F1 of the 15-45 piece theoretical tray of rectifying tower T1 that 25-50 piece theoretical plate number is housed, and extraction agent enters in rectifying tower T1 from the extractant feed mouth F2 of the 2-25 piece theoretical tray of rectifying tower; Another kind is directly the alcohol-water raw material to be joined in tower bottom of rectifying tower, and extraction agent enters in rectifying tower T1 from the extractant feed mouth F2 of the 2-25 piece theoretical tray of rectifying tower.After extracting rectifying, ethanol is from the tower top discharge port P1 extraction of rectifying tower T1, extraction agent-water mixed liquid is stayed in tower bottom of rectifying tower, enter the extraction agent recovery stage in rectifying tower, after the extracting rectifying stage completes, with rectifying tower, replace recovery tower to carry out the recovery of extraction agent, by resulting extraction agent-water mixed liquid of extracting rectifying stage through after reclaiming, water is from the tower top discharge port P1 extraction of rectifying tower T1, and extraction agent recycles after being collected by the discharge port S1 extraction of tower bottom of rectifying tower.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but do not limit protection scope of the present invention.
According to technical process shown in accompanying drawing 1,40 theoretical stages of rectifying tower, raw material is containing ethanol 27%(massfraction, as follows), water 73%, with the flow of 1000kg/hr from the 35th theoretical stage of rectifying tower (calculating at the bottom of from tower top to tower, as follows) charging, extraction agent 1-ethyl-3-methylimidazole acetate is from the 5th theoretical stage charging of rectifying tower, working pressure is 101.3kPa, solvent ratio 1, reflux ratio 4.0.Recovery tower working pressure 85kPa.Rectifying tower tower top produced quantity 268.1kg/hr, form: ethanol 99.90%, water 0.10%, ethanol yield 99.2%.Extraction extraction agent at the bottom of the recovery tower tower, water content 0.15%, return to rectifying tower and recycle.
According to technical process shown in accompanying drawing 1,25 theoretical stages of rectifying tower, raw material is containing ethanol 49%, water 51%, with the flow of 1000kg/hr from the 15th theoretical stage charging of rectifying tower, extraction agent 1-butyl-3-methyl imidazolium tetrafluoroborate is from the 3rd theoretical stage charging of rectifying tower, working pressure is 80kPa, solvent ratio 0.8, reflux ratio 2.0.Recovery tower working pressure 75kPa.Rectifying tower tower top produced quantity 487.0kg/hr, form: ethanol 99.92%, water 0.08%, ethanol yield 99.3%.Extraction extraction agent at the bottom of the recovery tower tower, water content 0.13%, return to rectifying tower and recycle.
According to technical process shown in accompanying drawing 1,40 theoretical stages of rectifying tower, raw material is containing ethanol 65%, water 35%, with the flow of 1200kg/hr from the 35th theoretical stage charging of rectifying tower, extraction agent is the composite extractant that 1-ethyl-3-methylimidazole a tetrafluoro borate and 1-octyl group-3-methyl imidazolium tetrafluoroborate form with volume ratio 1:1, and from the 2nd theoretical stage charging of rectifying tower, working pressure is 65kPa, solvent ratio 0.5, reflux ratio 0.5.Recovery tower working pressure 60kPa.Rectifying tower tower top produced quantity 778.0kg/hr, form: ethanol 99.95%, water 0.05%, ethanol yield 99.7%.Extraction extraction agent at the bottom of the recovery tower tower, water content 0.10%, return to rectifying tower and recycle.
Embodiment 4
According to technical process shown in accompanying drawing 1,40 theoretical stages of rectifying tower, raw material is containing ethanol 90%, water 10%, with the flow of 1500kg/hr from the 35th theoretical stage charging of rectifying tower, extraction agent is the composite extractant that 1-ethyl-3-methylimidazole a tetrafluoro borate and ethylene glycol volume ratio 1:1 form, and from the 5th theoretical stage charging of rectifying tower, working pressure is 101.3kPa, solvent ratio 0.2, reflux ratio 0.1.Recovery tower working pressure 45kPa.Rectifying tower tower top produced quantity 1344.9kg/hr, form: ethanol 99.98%, water 0.02%, ethanol yield 99.6%.Extraction extraction agent at the bottom of the recovery tower tower, water content 0.05%, return to rectifying tower and recycle.
Embodiment 5
According to technical process shown in accompanying drawing 1,50 theoretical stages of rectifying tower, raw material is containing ethanol 10%, water 90%, with the flow of 1000kg/hr from the 45th theoretical stage charging of rectifying tower, extraction agent is the composite extractant that 1-ethyl-3-methylimidazole acetate and glycerol volume ratio 2:1 form, and from the 25th theoretical stage charging of rectifying tower, working pressure is 101.3kPa, solvent ratio 4.8, reflux ratio 1.Recovery tower working pressure 90kPa.Rectifying tower tower top produced quantity 99.5kg/hr, form: ethanol 99.91%, water 0.09%, ethanol yield 99.4%.Extraction extraction agent at the bottom of the recovery tower tower, water content 0.11%, return to rectifying tower and recycle.
Embodiment 6
Press technical process shown in accompanying drawing 2, raw material is containing ethanol 80%, water 20%, and the disposable 500kg of feeding intake is in the tower bottom of rectifying tower that 35 theoretical stages are housed, and extraction agent 1-ethyl-3-methylimidazole a tetrafluoro borate is from the tower top charging.The extracting rectifying stage: working pressure is 101.3kPa, Solvent quantity 241kg, reflux ratio 0.2, overhead extraction ethanol 397.4kg, purity 99.96%, yield 99.3%.The extraction agent recovery stage: the rectifying tower working pressure is 70kPa, and without refluxing, phase 3.5kg in the middle of the first extraction of tower top, containing ethanol 74.3%; Recovered water subsequently, tower reactor finally obtains the 239kg extraction agent, and water content 0.08%, can be recycled.
Above preferred embodiment of the present invention is had been described in detail, but described content is only preferred embodiment of the present invention, can not be considered to for limiting practical range of the present invention.All equalization variations of doing according to the present patent application scope and improvement etc., within all should still belonging to patent covering scope of the present invention.
Claims (8)
1. the method for a separating alcohol-water mixture, it is characterized in that: described method adopts continuity operation or intermittent operation: described continuity operation comprises rectifying tower and recovery tower, that to take the ethanol-water mixture of arbitrary proportion be raw material, the double solvents that ionic liquid or ionic liquid and organic solvent form of take is extraction agent, raw material is by 15-45 piece theoretical tray, extraction agent is entered into respectively in the described rectifying tower that 25-50 piece theoretical plate number is housed by 2-25 piece theoretical stage, ethanol is by the extraction of described rectifying tower tower top, extraction agent-water mixed liquid is entered to described recovery tower by the recovery tower opening for feed after by described tower bottom of rectifying tower extraction, water is by described recovery tower overhead extraction, extraction agent recycles after by the extraction of described recovery tower tower reactor,
Described intermittent operation comprises rectifying tower, be divided into extracting rectifying stage and extraction agent recovery stage, the described extracting rectifying stage is that to take the ethanol-water mixture of arbitrary proportion be raw material, the double solvents that ionic liquid or ionic liquid and organic solvent form of take is extraction agent, raw material is by 15-45 piece theoretical tray, extraction agent is entered into respectively by 2-25 piece theoretical stage in the described rectifying tower that 25-50 piece theoretical plate number is housed or directly raw material is added in the tower reactor of rectifying tower, extraction agent is entered in the described rectifying tower that 25-50 piece theoretical plate number is housed by 2-25 piece theoretical stage, ethanol by the extraction of described rectifying tower tower top after, extraction agent-water mixed liquid is stayed to tower bottom of rectifying tower and carry out the operation of extraction agent recovery stage in rectifying tower, water is by the extraction of described rectifying tower tower top, extraction agent recycles by described tower bottom of rectifying tower extraction and after collecting.
2. method according to claim 1, it is characterized in that: described ionic liquid is the non-AlCl that positively charged ion is imidazol ion
3the mixture of one or more in the type ionic liquid.
3. method according to claim 2 is characterized in that: described ionic liquid is one or more the mixture in 1-ethyl-3-methylimidazole acetate, 1-ethyl-3-methylimidazole a tetrafluoro borate, 1-butyl-3-methyl imidazolium tetrafluoroborate, 1-octyl group-3-methyl imidazolium tetrafluoroborate.
4. method according to claim 1, it is characterized in that: described organic solvent is low carbon number alcohols or DMF or N,N-dimethylacetamide or N-Methyl pyrrolidone class high boiling point and water-soluble solvent preferably.
5. method according to claim 4, it is characterized in that: described organic solvent is ethylene glycol or glycerol.
6. according to the described method of claim 1-5 any one, it is characterized in that: described in described continuity operating process, the rectifying tower working pressure is 65-101.3kPa, reflux ratio is 0.2-4.0, the add-on of extraction agent and the mass ratio of raw material are (0.2-4.8): 1, and described recovery tower working pressure is 45-101.3kPa;
In described intermittent operation flow process, the described rectifying tower working pressure in extracting rectifying stage is 65-101.3kPa, reflux ratio is 0.2-4.0, the add-on of extraction agent and the mass ratio of raw material are (0.2-4.8): 1, and the described rectifying tower working pressure of extraction recovery stage is 45-101.3kPa.
7. according to the described method of claim 1-5 any one, it is characterized in that: described in described continuity operating process, the rectifying tower working pressure is 101.3kPa, reflux ratio is 0.1-1.0, the add-on of extraction agent and the mass ratio of raw material are (0.2-1.0): 1, and described recovery tower working pressure is 45-90kPa;
In described intermittent operation flow process, the described rectifying tower working pressure in extracting rectifying stage is 101.3kPa, reflux ratio is 0.1-1.0, the add-on of extraction agent and the mass ratio of raw material are (0.2-1.0): 1, and the described rectifying tower working pressure of extraction recovery stage is 45-90kPa.
8. the rectifier unit for the described method of claim 1, it is characterized in that: the rectifier unit of described continuity operation comprises rectifying tower and the recovery tower that 25-50 piece theoretical plate number is housed, the discharge port of the tower reactor of described rectifying tower is connected with the opening for feed of described recovery tower, the discharge port of described recovery tower bottom is connected with the extractant feed mouth of described rectifying tower, and the material inlet of described rectifying tower, extractant feed mouth are located at respectively 15-45 piece theoretical tray place and the 2-25 piece theoretical tray place of described rectifying tower; The opening for feed of described recovery tower is located at the middle and lower part of described recovery tower;
The rectifier unit of described intermittent operation comprises the rectifying tower that 25-50 piece theoretical plate number is housed, and the material inlet of described rectifying tower, extractant feed mouth are located at respectively 15-45 piece theoretical tray place and the 2-25 piece theoretical tray place of described rectifying tower.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN2013103658117A CN103435445A (en) | 2013-08-20 | 2013-08-20 | Method for separating mixture of ethanol alcohol and water |
Applications Claiming Priority (1)
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| CN103901142A (en) * | 2014-04-01 | 2014-07-02 | 深圳市检验检疫科学研究院 | Method for separating water in alcoholic beverage for assaying isotope of H and O |
| CN104370694A (en) * | 2014-11-07 | 2015-02-25 | 济南大学 | Separation method of isobutanol-ethyl isobutyrate azeotrope by batch extraction rectification |
| CN104370693A (en) * | 2014-11-07 | 2015-02-25 | 济南大学 | Separation method for batch extractive distillation of methanol-propyl formate azeotrope |
| CN104610021A (en) * | 2015-01-12 | 2015-05-13 | 济南大学 | Method for continuous extractive distillation and separation of ethanol-toluene azeotrope with mixed solvent |
| CN104628522A (en) * | 2015-01-12 | 2015-05-20 | 济南大学 | Intermittent extractive distillation process for ethanol-methylbenzene azeotropic mixture |
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| CN105001050A (en) * | 2015-05-06 | 2015-10-28 | 青岛科技大学 | Recovery processing method for methyl alcohol and ethyl alcohol in carboxymethyl cellulose flash distillation tail gas |
| CN105001051A (en) * | 2015-05-13 | 2015-10-28 | 青岛科技大学 | Method for treatment of carboxymethyl cellulose centrifugal tail gas containing ethyl alcohol on basis of heat integration |
| CN106431836A (en) * | 2016-09-19 | 2017-02-22 | 青岛科技大学 | A process for coupling extraction, rectification and flash distillation to separate ethanol-water system |
| CN107488103A (en) * | 2017-08-24 | 2017-12-19 | 章德恩 | A kind of water azeotropic mixture extraction rectifying method |
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| CN104370694A (en) * | 2014-11-07 | 2015-02-25 | 济南大学 | Separation method of isobutanol-ethyl isobutyrate azeotrope by batch extraction rectification |
| CN104370693A (en) * | 2014-11-07 | 2015-02-25 | 济南大学 | Separation method for batch extractive distillation of methanol-propyl formate azeotrope |
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| CN105001050A (en) * | 2015-05-06 | 2015-10-28 | 青岛科技大学 | Recovery processing method for methyl alcohol and ethyl alcohol in carboxymethyl cellulose flash distillation tail gas |
| CN105001051A (en) * | 2015-05-13 | 2015-10-28 | 青岛科技大学 | Method for treatment of carboxymethyl cellulose centrifugal tail gas containing ethyl alcohol on basis of heat integration |
| CN106431836A (en) * | 2016-09-19 | 2017-02-22 | 青岛科技大学 | A process for coupling extraction, rectification and flash distillation to separate ethanol-water system |
| CN106431836B (en) * | 2016-09-19 | 2019-03-29 | 青岛科技大学 | A kind of technique of extracting rectifying and flash distillation integrated separation alcohol-water object system |
| CN107488103A (en) * | 2017-08-24 | 2017-12-19 | 章德恩 | A kind of water azeotropic mixture extraction rectifying method |
| CN107488103B (en) * | 2017-08-24 | 2020-06-05 | 王婵 | Extraction and rectification method for water-isopropanol azeotropic mixture |
| 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 |
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