CN102267889A - Method for recovering spirit of vinegar by combining extraction with azeotropic distillation - Google Patents
Method for recovering spirit of vinegar by combining extraction with azeotropic distillation Download PDFInfo
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- CN102267889A CN102267889A CN2011101484323A CN201110148432A CN102267889A CN 102267889 A CN102267889 A CN 102267889A CN 2011101484323 A CN2011101484323 A CN 2011101484323A CN 201110148432 A CN201110148432 A CN 201110148432A CN 102267889 A CN102267889 A CN 102267889A
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Abstract
The invention relates to a method for recovering spirit of vinegar by combining extraction with azeotropic distillation. The method comprises the following steps of: performing liquid-liquid extraction on a part of acetic acid-water component to be separated, injecting an extraction agent into the bottom of an extraction column, and performing countercurrent contact and extraction on the spirit of vinegar to obtain a column top component (extraction phase) comprising acetic acid and the extraction agent and waste water (raffinate phase) meeting the environmental requirement for discharging; introducing the extraction phase and the other part of spirit of vinegar into an azeotropic rectification column together for performing azeotropic distillation, wherein a qualified acetic acid product is obtained from a column reactor of the azeotropic distillation column, and an azeotrope of an entrainer and water is obtained from the column top; and performing liquid-liquid separation on the entrainer and water in a phase splitter, returning an organic phase into the azeotropic distillation column for serving as an entrainer, returning to an extraction column for serving as an extraction agent, and introducing a water phase into an entrainer recovering column or discharging. The extraction agent and the entrainer used in the method are mixtures of acetic acid alkyl ester and corresponding alcohols. In the method, moisture entering azeotropic distillation is lowered by adopting an extraction technology, thus the using amount of the entrainer is reduced, heated steam flow on the column reactor of the azeotropic distillation column is saved, and the using amount of the entrainer and the energy consumption of a device are reduced.
Description
Technical field
The invention provides a kind of method of uniting the dilute acetic acid recovery of carrying out with the azeotropic distillation technology that extracts that adopts.It belongs to the separation engineering field of chemical engineering, is specially adapted to the processing of low-concentration acetic acid wastewater, is to take into account a kind of abstraction technique of benefit and environment protection and the acetic acid dehydration system that the azeotropic distillation technical tie-up is used.
Background technology
Acetic acid has been widely used industrial, and it can be used as the solvent of oxidizing reaction, also can be used as the important source material of organic synthesis industry.In the acetic acid use, usually need acetic acid is purified, made with extra care, usually relate to acetic acid and separation of water solution.The waste water that contains acetic acid of Chan Shenging in process of production, though acetic acid content is lower in the waste water, the acetic acid containing waste water total amount that produces in the industrial production is very big, and the acetic acid amount that is discharged every year is very high, and this is not only the waste of resource, returns environment and has caused significant damage.Industrial discharging to waste water has strict requirement.
General acetic acid dehydration is handled and is mainly contained dual mode, i.e. conventional distillation method and azeotropic distillation.Because water and acetic acid relative volatility approach 1, adopt conventional distillation to need more stage number and bigger reflux ratio, energy consumption is bigger.And acetic acid content is also higher in the tower top discharge water, and the acetic acid loss is big, environmental protection treatment expense height.The method of general at present employing heterogeneous azeotropic rectification is carried out acetic acid dehydration, and entrainer commonly used has n-propyl acetate, n-butyl acetate, isobutyl acetate etc.Heterogeneous azeotropic rectification is owing to have characteristics such as less energy-consumption, required stage number are less, separation efficiency height, and it is economy and environmental protection that the aqueous acetic acid that adopts azeotropy rectification column to carry out high density separates.But when the acetate concentration in the charging is low, adopt this azeotropic distillation mode to need higher energy consumption.This is because in the heterogeneous azeotropic rectification process of acetic acid-water system, water and entrainer are to leave rectifying tower from cat head with gas form, separates through liquid liquid after the condensation.If water concentration is low excessively, azeotropy rectification column will need more entrainer, and the vapour-liquid phase load in the rectifying tower increases, and the system energy consumption height is uneconomical.In view of above-mentioned shortcoming of the prior art, the present invention proposes a kind ofly to take into account cost benefit and energy benefit, and is applicable to " extraction-azeotropic distillation " technology of existing producing apparatus.
Summary of the invention
In order to reduce the energy consumption in the dilute acetic acid azeotropic distillation removal process, the invention provides the acetic acid dehydration method that a kind of extraction-azeotropic distillation technical tie-up is used, this method can realize by the acetic acid dehydration heterogeneous azeotropic rectification process of routine is improved.This is by on the basis of original azeotropy rectification column, sets up an extraction tower, and the part dilute acetic acid is carried dense content with water in the reduction azeotropy rectification column combined feed total feed, and then reduces the operational load of azeotropy rectification column, reaches purpose of energy saving.
Method of the present invention mainly contains following process:
1, extraction tower extraction process
In the liquid-liquid extraction tower, dilute acetic acid adds from the extraction tower top, and available extraction agent such as n-butyl acetate, isobutyl acetate, Iso Butyl Acetate and n-propyl acetate and composition thereof etc. add from the extraction tower bottom.Simultaneously, the used entrainer of extraction agent of selecting for use and azeotropy rectification column is a same substance.Through extracting and separating, the extraction tower cat head obtains the extraction phase that main component is acetic acid, water and extraction agent, and it is big and contain the extracting phase of a small amount of organic compound to obtain water content at the bottom of the tower.Extraction phase enters azeotropy rectification column and carries out azeotropic distillation, and the acetic acid massfraction in the extracting phase is lower than 0.1%, and extraction agent content is controlled at below 0.8%.Therefore in order better to reduce directly discharging to the pollution of environment, extracting phase at the bottom of the extraction Tata can join the processing of reclaiming extraction agent in the solvent recovery tower, but, because the massfraction of acetic acid is lower, at organic content under the lower and situation that environment is not polluted, can directly discharge, need not to feed solvent recovery tower and reclaim solvent.
2, azeotropy rectification column rectifying
The extraction phase that process 1 is obtained (its main component is extraction agent and water, acetic acid) injects the top of azeotropy rectification column, under the effect of entrainer (being same composition), carry out azeotropic distillation with the extraction agent that uses in the process 1, and at the bottom of cat head obtains tower that overhead fraction that main component is water and entrainer and main component be acetic acid solution.Overhead mixture enters the phase splitter layering after condensation, obtaining water and main component that main component is a water respectively is the organic phase of entrainer.The part of organic phase is returned the extraction tower bottom and is recycled as extraction agent, and its flow size is by the extraction ability decision of the content and the extraction tower tower body of acetic acid in the component to be separated.A part is as the backflow of azeotropy rectification column in addition.Water joins the recovery that solvent recovery tower carries out entrainer (extraction agent).
3, entrainer (extraction agent) removal process
Aqueous phase in the azeotropic distillation column overhead phase splitter contains a spot of entrainer and needs to reclaim.In addition, also containing a spot of extraction agent in the extracting phase of extraction tower needs to reclaim.This entrainer (extraction agent) recovery tower is similarly an azeotropic rectifying tower, determines extraction entrainer in cat head or the tower according to the impurity situation in technology and the charging.The tower still is the waste water that satisfies environmental requirement.
Be the top efficiency that realizes that the technical tie-up of extraction-azeotropic distillation is used, extraction agent can be selected single component for use, also can select two or more mixture of ingredients.
Adopt that the acetic acid mass content is (10～30) % in the dilute acetic acid of this kind treatment process.Process 1 preferably temperature be not higher than carry out under 50 ℃ of conditions extracting operation with preliminary reduction acetic acid containing waste water in the content of water.Extraction tower in this process can be rotating disc contactor or packing tower, is generally gravity phase-splitting form, can or not have the counter-current extraction tower that machinery stirs tower for mechanical stirring tower, pulse-column.
Extraction agent by tower at the bottom of charging, acetic acid-water component to be separated is by cat head or the charging of tower middle and upper part, one section zone arranged usually for the abundant layering of overhead stream on the top of acetic acid-aqueous solution charging.
Azeotropy rectification column in the process 2 be with tentatively dewatered extraction phase and under the effect of entrainer, carry out the high concentration vinegar acid solution that azeotropic distillation obtains meeting industrial requirements and can recycle through carrying dense dilute acetic acid.Join the different column plates place on azeotropy rectification column top respectively through the dilute acetic acid that tentatively dewaters and untreated dilute acetic acid.
Azeotropy rectification column of the present invention can adopt tray column or packing tower.To the feed entrance point of the extraction phase logistics that obtains in the process 1, general in the charging of the top of azeotropy rectification column.Do not add in addition and generally add in the middle and upper part of azeotropy rectification column through the dilute acetic acid aqueous solution that tentatively dewaters.
Based on the needs of experimental data and general principle and practical application in the present invention, entrainer can be selected single component for use, also can select to form with separated component two or more mixture of ingredients of azeotropic mixture.The present invention is based on the requirement of economy, easily separated principle, selecting the mixture of acetic acid alkyl ester and correspondent alcohol for use is entrainer, as selects for use n-butyl acetate and propyl carbinol jointly as extraction agent.
Recyclable the returning in the production system of the high concentration vinegar acid solution that obtains at the bottom of process 2 towers recycles as solvent or reactant again.The massfraction of acetic acid is 92～99% in the acetum at the bottom of the azeotropic distillation Tata, and the massfraction of entrainer is lower than below 0.1%, and the content of water generally is lower than below 10%.
Part or all extracting phase in extraction tower of water in the process 2 can also be added the recovery that solvent recovery tower carries out entrainer among the present invention.
A part that also comprises the water that will obtain in the process 2 among the present invention is injected the part that azeotropy rectification column refluxes as water, the operational stability of azeotropy rectification column when guaranteeing that acetic acid content changes in the charging.The flow of water that injects azeotropy rectification column is according to different operating and difference can realize zero backflow of water in the present invention.And the position of refluxing is generally the top of azeotropy rectification column.
The present invention unites abstraction technique and the azeotropic distillation technology used, treat the initial gross separation of the water in the separated stream by abstraction technique, thereby the content of the treating water in the azeotropy rectification column is reduced, and then reduce the energy consumption of azeotropic distillation, thereby fundamentally reduce the steam consumption of azeotropy rectification column.
Description of drawings
Fig. 1 is the extraction-azeotropic distillation-solvent recovery process schema of acetic acid dehydration.
Embodiment
To help to understand the present invention by the following description of the embodiments, but not limit content of the present invention.It is extraction agent and entrainer that the present invention adopts n-butyl acetate and propyl carbinol mixing solutions, is that solution below 30% is pending solution with the acetic acid massfraction.
Embodiment
The particular flow sheet of embodiment please refer to Fig. 1, and it all is benchmark with the massfraction that the material in the present embodiment is formed.
In mixture flow 1 to be separated, the injection rate of dilute acetic acid is 29225kg/h, and the massfraction of acetic acid is 0.15, and the massfraction of water is 0.85.Logistics 2 extracts in the charging of the top of extraction tower as the part of stream thigh 1, and flow is 10000kg/h; Logistics 3 is another part of stream thigh 1, and directly entering azeotropy rectification column carries out heterogeneous azeotropic rectification, and flow is 19225kg/h.
Extraction tower 1 adopts packing tower, and the theoretical plate number of extraction tower 1 is 30, and the selection operation condition is 25 ℃ of normal temperature, can also choose 40～50 ℃ of stream temperature, and working pressure is generally normal pressure.
Logistics 9 is the required extraction agent of extraction, and promptly main component is the mixture flow of n-butyl acetate and propyl carbinol, and wherein n-butyl acetate content is 91%, and propyl carbinol content is 4%, and water-content is 4%.Injection rate is 26000kg/h.
Mixture flow 2 to be separated after the process extraction, obtains extracting phase logistics 10 with logistics 9 at the bottom of the extraction tower in extraction tower, enter solvent recovery tower 5, and its flow is 25374kg/h, and wherein the massfraction of acetic acid is lower than 0.05%, and the concentration of n-butyl acetate is lower than 0.8%.
The extraction phase logistics 4 of extraction tower 1 enters on the 15th layer of column plate of azeotropy rectification column 2 that stage number is 61 plates (sequence number from cat head begin calculate), and another 3 of untreated mixture flow to be separated enters the 35th layer of column plate of azeotropy rectification column 2.
The operational condition selection operation temperature of azeotropy rectification column 2 is 90～115 ℃, and working pressure is 5～25kPag.The required heat of azeotropy rectification column 2 (be evaporator tower at the bottom of the required heat of liquid) provides by reboiler.
Behind azeotropic distillation, the still liquid logistics 8 that obtains at the bottom of azeotropy rectification column 2 towers is a acetum more than 95% for acetate concentration, and flow is 4508kg/h.
The overhead fraction 5 that azeotropy rectification column 2 cats head obtain mainly is made up of water and entrainer, by introducing separating tank 4 after condenser 3 condensations of using water coolant.In separating tank 4,, be divided into the organic phase logistics 15 and the main aqueous water logistics 13 that mainly contain n-butyl acetate and propyl carbinol with the phlegma layering.
Logistics 9 is the part of organic phase logistics 15, and its mass rate is 27000kg/h, and wherein n-butyl acetate content is 91%, and propyl carbinol content is 4%, and water-content is 4%, and this logistics loops back the bottom of extraction tower 1, i.e. the tenth column plate charging is as extraction agent.Remaining part organic phase, promptly its mass rate is the logistics 7 of 15719kg/h, the 25th plate that is circulated back to azeotropy rectification column 2 recycles as entrainer.
In order to make the azeotropy rectification column stable operation, a part of logistics 6 of water loops back first block of column plate in top of azeotropy rectification column 2, and its mass rate is 100kg/h.Remaining part water, i.e. logistics 14 enters solvent recovery tower 5 and carries out organic recovery and wastewater treatment.
The entrainer that loses in the whole recovery process adds in separating tank 4 tops additional by logistics 11.
Solvent recovery tower 5 is the azeotropy rectification column of 27 blocks of plates for stage number.Water logistics 14 and extracting phase logistics 10 are in the 14th column plate charging of solvent recovery tower.And main component to be the organic phase returned logistics 16 of n-butyl acetate and propyl carbinol carry out the side line extraction at the 8th block of plate, and add separating tank 4 tops.The logistics 18 that cat head obtains is impurity ritalin in the dilute acetic acid charging, and tower base stream 19 obtains meeting the waste water of environment protection emission requirement.
Claims (11)
1. the method for purification of a dilute acetic acid is characterized in that, adopts extraction tower, and azeotropy rectification column and solvent recovery tower are realized the purification of dilute acetic acid jointly.Before azeotropy rectification column and solvent recovery tower, set up an extraction tower, under the extraction of extraction tower, reduce the water-content of azeotropy rectification column combined feed total feed.Dilute acetic acid is divided into two strands, and one joins the extraction tower top, and another strand joins the middle part of azeotropy rectification column.In phase splitter, be divided into organic phase and water after the overhead gas phase mixture condensation of azeotropy rectification column.An organic phase part is injected the extraction tower bottom as extraction agent, extracts with the dilute acetic acid counter current contact.A part is returned the top of azeotropy rectification column as the backflow of azeotropy rectification column.The water small part is returned the azeotropic distillation top of tower as backflow, and major part enters into the solvent recovery tower middle part and reclaims solvent.The extraction phase at extraction tower top enters the top of azeotropy rectification column and carries out azeotropic distillation.Solvent recovery tower be can inject according to circumstances through the waste water after the extraction and solvent or directly discharging reclaimed.
2. method according to claim 1 is characterized in that, handled dilute acetic acid mass content is (10～30) %.The mass flux ratio that enters the dilute acetic acid of the dilute acetic acid of extraction tower and azeotropy rectification column is 1: (1～4).
3. method according to claim 1 is characterized in that, the mass flux ratio of handled dilute acetic acid and extraction agent is 1: (2～4).
4. method according to claim 1, the acetic acid quality branch in the tower base stream of extraction tower is lower than 0.5%, and the content of extraction agent is lower than 0.8%.
5. method according to claim 1, extraction agent is selected from the acetic acid alkyl ester, forms as the mixture of isobutyl acetate, n-butyl acetate, Iso Butyl Acetate, n-propyl acetate and correspondent alcohol thereof.
6. method according to claim 1 is characterized in that, the acetic acid mass content in the tower base stream of azeotropy rectification column can be 80～99%, and overhead stream is a water, the mixture of entrainer and acetic acid, and wherein the acetic acid massfraction is less than 0.2%.Overhead stream obtains the higher logistics of solvent after water is removed in the phase splitter layering, this logistics part turns back to azeotropy rectification column, and a part turns back to extraction tower and uses as extraction agent.
7. want 5 described methods according to right, entrainer and extraction agent are elected the mixture of identical acetic acid alkyl ester and corresponding alcohol thereof as, as the extraction agent and the entrainer of n-butyl acetate and propyl carbinol composition, extraction agent and entrainer that isobutyl acetate and isopropylcarbinol are formed.
8. method according to claim 1, the logistics that enters azeotropy rectification column comprises the dilute acetic acid of handling without extraction tower, and the organic phase reflux of extracting rectifying column overhead extraction phase and azeotropy rectification column and water reflux.
9. method according to claim 8, the water part in the phase splitter is returned azeotropy rectification column as backflow, and another part enters solvent recovery tower and reclaims the solvent cycle use.
10. method according to claim 8, the part of organic phase phlegma are returned extraction tower and are made extraction agent and recycle, and make entrainer and recycle and another part enters azeotropy rectification column.The mass flux ratio that enters extraction Tahe azeotropy rectification column is (0.5～2.5): 1.
11. method according to claim 1, the part of the water in the tower still extracting phase of extraction tower and the azeotropy rectification column cat head phase splitter together joins solvent recovery tower and reclaims solvent, recovered solvent can turn back to the phase splitter of azeotropy rectification column from side line extraction or cat head extraction.
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|---|---|---|---|---|
| CN102746135A (en) * | 2012-08-01 | 2012-10-24 | 中国石油化工股份有限公司 | Method for recovering acetic acid and water through azeotropic distillation in aromatic carboxylic acid production |
| CN103073412A (en) * | 2012-11-09 | 2013-05-01 | 浙江逸盛石化有限公司 | PAT solvent dehydration system and dehydration technology |
| CN104045549A (en) * | 2013-03-15 | 2014-09-17 | 江苏天成生化制品有限公司 | Method for recovery of acetic acid from ethenone wastewater by side dedusting rectification |
| CN105037131A (en) * | 2015-06-17 | 2015-11-11 | 福州大学 | Novel process for recovering PTA (purified terephthalic acid) wastewater |
| CN106831336A (en) * | 2017-01-16 | 2017-06-13 | 南京师范大学 | Ethanol and hydrazine hydrate mixed liquor are reclaimed and circulation utilization method in a kind of pyraclostrobin production |
| CN106866409A (en) * | 2017-03-23 | 2017-06-20 | 中石化上海工程有限公司 | The method of cyclohexyl acetate extraction and recovery spirit of vinegar |
| CN107459449A (en) * | 2016-06-02 | 2017-12-12 | 中国石化扬子石油化工有限公司 | A kind of acetic acid is separated from water method |
| CN107459448A (en) * | 2016-06-02 | 2017-12-12 | 中国石化扬子石油化工有限公司 | A kind of acetic acid is separated from water method |
| CN107501085A (en) * | 2017-09-25 | 2017-12-22 | 华东理工大学 | A kind of method that economic benefits and social benefits are thermally integrated separation of extractive distillation acetic acid and aqueous mixtures |
| CN108976115A (en) * | 2017-06-05 | 2018-12-11 | 中国石油化工股份有限公司 | A kind of method and system of separating benzene-cyclohexane and acetic acid |
| CN109020806A (en) * | 2018-10-31 | 2018-12-18 | 天津中福环保科技股份有限公司 | A kind of recycling purification acetic acid extraction-entrainer |
| CN109053424A (en) * | 2018-10-31 | 2018-12-21 | 天津中福环保科技股份有限公司 | System and method of the field of new materials from multiple types acetic acid devil liquor recovery purification acetic acid |
| CN109232235A (en) * | 2018-10-31 | 2019-01-18 | 天津中福环保科技股份有限公司 | A kind of acetic acid recovery method of saline extraction-azeotropic distillation |
| CN109467497A (en) * | 2018-08-03 | 2019-03-15 | 内蒙古蒙维科技有限公司 | A kind of recovery process and device of polyvinyl alcohol alcohol hydrolysis mother liquor |
| CN109467501A (en) * | 2018-08-03 | 2019-03-15 | 内蒙古蒙维科技有限公司 | Acetic acid refining and entrainer regeneration technology and device in polyvinyl alcohol disposing mother liquor unit |
| CN111606877A (en) * | 2020-06-10 | 2020-09-01 | 安庆亿成化工科技有限公司 | Acetic acid azeotropic dehydration device and method suitable for producing trimellitic anhydride |
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5167774A (en) * | 1992-02-06 | 1992-12-01 | Lloyd Berg | Dehydration of acetic acid by extractive distillation |
| CN1626494A (en) * | 2004-08-09 | 2005-06-15 | 天津大学 | Method for recovering acetic acid from wastewater generated in production of furfural |
| CN101172941A (en) * | 2006-11-02 | 2008-05-07 | 中国石油化工股份有限公司 | Method for recycling acetic acid in dilute acetic acid |
| CN101445444A (en) * | 2008-12-17 | 2009-06-03 | 中国石化仪征化纤股份有限公司 | Method for recovering dilute acetic acid by extraction and azeotropic distillation |
| CN101898952A (en) * | 2010-07-19 | 2010-12-01 | 天津市天大北洋化工设备有限公司 | Method and device for treating low-concentration acetic acid wastewater |
-
2011
- 2011-06-03 CN CN2011101484323A patent/CN102267889A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US5167774A (en) * | 1992-02-06 | 1992-12-01 | Lloyd Berg | Dehydration of acetic acid by extractive distillation |
| CN1626494A (en) * | 2004-08-09 | 2005-06-15 | 天津大学 | Method for recovering acetic acid from wastewater generated in production of furfural |
| CN101172941A (en) * | 2006-11-02 | 2008-05-07 | 中国石油化工股份有限公司 | Method for recycling acetic acid in dilute acetic acid |
| CN101445444A (en) * | 2008-12-17 | 2009-06-03 | 中国石化仪征化纤股份有限公司 | Method for recovering dilute acetic acid by extraction and azeotropic distillation |
| CN101898952A (en) * | 2010-07-19 | 2010-12-01 | 天津市天大北洋化工设备有限公司 | Method and device for treating low-concentration acetic acid wastewater |
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| CN102746135A (en) * | 2012-08-01 | 2012-10-24 | 中国石油化工股份有限公司 | Method for recovering acetic acid and water through azeotropic distillation in aromatic carboxylic acid production |
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| CN103073412A (en) * | 2012-11-09 | 2013-05-01 | 浙江逸盛石化有限公司 | PAT solvent dehydration system and dehydration technology |
| CN103073412B (en) * | 2012-11-09 | 2014-11-12 | 浙江逸盛石化有限公司 | PAT solvent dehydration system and dehydration technology |
| CN104045549A (en) * | 2013-03-15 | 2014-09-17 | 江苏天成生化制品有限公司 | Method for recovery of acetic acid from ethenone wastewater by side dedusting rectification |
| CN105037131A (en) * | 2015-06-17 | 2015-11-11 | 福州大学 | Novel process for recovering PTA (purified terephthalic acid) wastewater |
| CN107459448A (en) * | 2016-06-02 | 2017-12-12 | 中国石化扬子石油化工有限公司 | A kind of acetic acid is separated from water method |
| CN107459449A (en) * | 2016-06-02 | 2017-12-12 | 中国石化扬子石油化工有限公司 | A kind of acetic acid is separated from water method |
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| CN106866409A (en) * | 2017-03-23 | 2017-06-20 | 中石化上海工程有限公司 | The method of cyclohexyl acetate extraction and recovery spirit of vinegar |
| CN108976115A (en) * | 2017-06-05 | 2018-12-11 | 中国石油化工股份有限公司 | A kind of method and system of separating benzene-cyclohexane and acetic acid |
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