CN102153458A - Method for recovering dilute acetic acid by virtue of extraction-azeotropic distillation of sec-butyl acetate - Google Patents
Method for recovering dilute acetic acid by virtue of extraction-azeotropic distillation of sec-butyl acetate Download PDFInfo
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Abstract
The invention relates to a method for recovering dilute acetic acid by virtue of extraction-azeotropic distillation of sec-butyl acetate. In the method, the sec-butyl acetate is an extractant of an extraction tower and an entrainer of an azeotropic distillation tower. The method is characterized in that a part of dilute acetic acid is fed into the top of a filler extraction tower, a small portion of tower top reflux liquid of the azeotropic distillation tower is used as the extratant to be fed to the bottom of the extraction tower, and is subjected to room temperature counter current contact extraction together with the dilute acetic acid; an extraction phase containing the sec-butyl acetate, acetic acid and little water is obtained on the top of the extraction tower; raffinate water containing trace acetic acid is obtained at a tower kettle, and enters into a solvent recovering tower; and the extraction phase in the extraction tower is fed to the upper half part of the azeotropic distillation tower for further concentration, and the other part of sec-butyl acetate is fed to the tower top of the azeotropic distillation tower. The method has the characteristic of high separation efficiency; and the recovery of the acetic acid is more than 95%, and the content of the acetic acid in waste water is below 0.5%. By using the method, the defects of large reflux ratio, high energy consumption and the like which are caused by using a rectification method are directly overcome, and the production capability of dilute acetic acid recovery is enlarged.
Description
Technical field
The invention belongs to chemical production technical field, more specifically relate to the method that a kind of sec-butyl acetate extraction-azeotropic distillation reclaims dilute acetic acid.
Background technology
Acetic acid is a kind of important Organic Chemicals, be widely used in industries such as basic organic synthesis, medicine, food, dyestuff, spices, agricultural chemicals, as in PTA produces as the solvent of PX, in the PVA industry as raw material, as solvent etc., in these Industrial processes, can discharge a large amount of acetic acid containing waste waters in the pharmaceutical industry.The content of acetic acid will be lower than the 2%(mass percent in " national industry emission standard " regulation discharge of wastewater), though the concentration of acetic acid is very low in these acetic acid containing waste waters, the acetic acid containing waste water total amount that produces in industrial production is very big.Therefore the separation of acetic acid-water be many be the problem that the chemical process of raw material, product or solvent often runs into acetic acid; be the long-term problems of noting of people, because it is significant for production technique, economic performance, environment protection and the utilization of resources of each relevant industries.Though acetic acid-aqueous solution does not form azeotrope, its relative volatility is little, especially when production high density acetic acid, separates difficulty more.Industrial acetic acid-separation of water solution method mainly contains: rectification method, esterification process, absorption method, membrane separation process, electroosmose process and extraction process etc.More than these methods exist to some extent that the acetic acid rate of recovery is low, energy consumption is high, industrialization or scale operation difficulty, processed waste water be difficult to reach shortcomings such as discharging standards.
Chinese patent CN101172941 has reported a kind of method that reclaims acetic acid in the synthetic dilute acetic acid that produces of furfural, ritalin and Fischer-Tropsch that solves, and adopts pulse packed extraction tower, azeotropy rectification column combined recovery acetic acid.The extraction agent of extraction tower is for being selected from the composition of at least two kinds mixed amine, alphanol and kerosene in the carbon atom tertiary amine of C12 ~ 16, and azeotropy rectification column adopts a kind of with in benzene, hexanaphthene, vinyl acetic monomer, Iso Butyl Acetate and the n-butyl acetate.By this patent as can be seen, adopt the acetic acid of extraction-azeotropic associating rectifying in can effectively recovery dilute acetic acid, but the used extraction agent of this method is a mixture, is unfavorable for the recovery of back solvent.Patent CN101445444 has reported a kind of method that reclaims dilute acetic acid from PTA waste water, adopts n-propyl acetate as extraction agent and entrainer.But this kind solvent is limited by traditional processing technology, and price is high for a long time, causes using manufacturer production cost height, and profit margin is little.
Summary of the invention
To have the low problem of separation efficiency in order solving in the acetic acid process of prior art in reclaiming dilute acetic acid, to the invention provides the method that a kind of sec-butyl acetate extraction-azeotropic distillation reclaims dilute acetic acid, this method has the high characteristics of separation efficiency.
The present invention implements by following technical solution:
Sec-butyl acetate in a kind of method of sec-butyl acetate extraction-azeotropic distillation recovery dilute acetic acid is the extraction agent of extraction tower and the entrainer of azeotropy rectification column; Part dilute acetic acid is sent into the filler extraction top of tower, and the trim the top of column liquid of azeotropy rectification column divides a small gangs of to deliver to the bottom of extraction tower as extraction agent, carries out the extraction of normal temperature counter current contact with dilute acetic acid; The extraction tower cat head obtains containing the extraction phase of sec-butyl acetate, acetic acid and less water; The extracting phase that the tower still obtains is the water that contains acetate in minute, and extracting phase enters solvent recovery tower;
The extraction phase of extraction tower is sent into the first half of azeotropy rectification column and is further carried dense, another part sec-butyl acetate is sent into the azeotropic distillation column overhead, another strand dilute acetic acid solution adds azeotropic distillation Tata middle part simultaneously, through azeotropic distillation, the cat head of azeotropy rectification column distillates the two-phase mixture that comprises sec-butyl acetate and water, contain the secondary butyl ester of small amount of acetic acid through the water after the phase splitter layering, water enters solvent recovery tower after the cat head extraction, oil phase returns azeotropy rectification column, and azeotropic distillation Tata stilling goes out mass content greater than 95% acetic acid.
The packed height of described packed extraction tower is equivalent to 20～30 theoretical stages, and the extraction tower operational condition is: atmospheric operation, extraction temperature are 20～25 ℃, and dilute acetic acid and sec-butyl acetate feed volume throughput ratio are 1:(1～3).
The processing condition of described azeotropy rectification column are: atmospheric operation, bed stuffing height are equivalent to 45～55 theoretical stages, and the volume flow ratio that enters the sec-butyl acetate of the dilute acetic acid of azeotropy rectification column and azeotropy rectification column trim the top of column is: 1:(1～7).
Described extraction tower cat head obtains containing the extraction phase of sec-butyl acetate, acetic acid and less water, and wherein the concentration of acetic acid is 7%～15%.
The first half that the extraction phase of described extraction tower is sent into azeotropy rectification column is further carried dense, and the height that enters azeotropy rectification column is the 23rd～27 theoretical stage.
The height that described another strand dilute acetic acid solution adds azeotropic distillation Tata middle part is the 28th～32 theoretical stage.
The percentage extraction of described extraction tower 〉=95%, described azeotropic distillation column overhead distillates the mixed solution that contains sec-butyl acetate, water and acetic acid, and wherein the mass concentration of acetic acid is below 0.5%, and the described oil phase that returns azeotropy rectification column is mainly sec-butyl acetate.
Extracting phase that described extraction Tata still comes out and azeotropy rectification column cat head come out to enter solvent recovery tower jointly through the water after the layering and reclaim solvent; The rate of recovery of described extraction-azeotropic distillation technology acetic acid is higher than 95%, and the concentration of the acetic acid of the aqueous phase after the extracting phase of extraction tower, the layering of azeotropic distillation column overhead is less than 0.5%.
Advantage of the present invention is: liquid-liquid extraction-azeotropic distillation integrated process that the present invention adopts, the used extraction agent sec-butyl acetate of extraction tower is again the entrainer of azeotrope column simultaneously.Extraction-azeotropic distillation combined process is compared with the azeotropic rectifying, makes full use of the dewatering of extraction process, thereby has reduced the load of azeotropy rectification column dehydration, has saved the required heat of rectifying.And, the conventional solvent such as n-propyl acetate, Iso Butyl Acetate, n-butyl acetate, isobutyl acetate that is different from available technology adopting, the sec-butyl acetate that the present invention adopts is the isomers of n-butyl acetate, isobutyl acetate, be a kind of environment-friendly type solvent, have the strong characteristics of band outlet capacity equally.Compare with isobutyl acetate with n-butyl acetate, the district of dissolving each other of acetic acid-sec-butyl acetate-water is bigger, this is favourable for extraction separation process, simultaneously as entrainer, the ability of its water entrainment is big, and sec-butyl acetate also has advantages such as energy consumption is low, cost performance is high, the entrainer loss is little, toxicity is low, replacement technology is simple simultaneously.Use sec-butyl acetate can reduce enterprise's production cost greatly, for enterprise brings economic benefit significantly.
Description of drawings
Fig. 1 is the schematic flow sheet of technology of the present invention.
Wherein: T1 is extraction tower (packed height is equivalent to 20～30 theoretical stages), and T2 is azeotropy rectification column (packed height is equivalent to 45～55 theoretical stages), and T3 is solvent recovery tower (being equivalent to 25～35 theoretical stages).E1 is the azeotropy rectification column overhead condenser, and E2 is an azeotropic distillation Tata still reboiler, and V1 is an azeotropic distillation column overhead quantizer, and V2 is the sec-butyl acetate storage tank, and E3 is the solvent recovery tower overhead condenser.The part of dilute acetic acid (stream strand 1) adds from the top of extraction tower T1, and the sec-butyl acetate that comes out from storage tank V2 adds the bottom of extraction tower T1 through pump P1 supercharging by pipeline 2, realizes extracting and separating in extraction tower T1.Send into the 23rd～27 theoretical stage of azeotropy rectification column from the extraction phase (stream thigh 3) that the extraction tower cat head comes out, the extracting phase that the tower still comes out (stream thigh 5) is sent into solvent recovery tower T3 recovery solvent wherein.The sec-butyl acetate that comes out from storage tank V2 passes through pump P1 supercharging adds azeotropy rectification column T2 by pipeline 6 top.Another part dilute acetic acid (stream thigh 4) is from the 28th～32 column plate charging of azeotropy rectification column, the sec-butyl acetate that comes out from storage tank V2 passes through pump P1 supercharging adds azeotropy rectification column T2 by pipeline 6 top, in azeotrope column, realize azeotropic distillation, the steam that comes out from the azeotropic distillation column overhead (stream strand 7) is sent into the V1 quantizer and is carried out layering after condenser E1 condensation, oil reservoir in the quantizer (stream thigh 8) is sent into storage tank V2, and water layer (stream thigh 9) is sent into solvent recovery tower T3 recovery solvent wherein.Fresh sec-butyl acetate adds storage tank V2 by pipeline 10.Obtain acetate concentration from azeotropic distillation Tata still and be higher than 99% solution.Enter solvent recovery tower recovery solvent from extracting Tata still extracting phase (flowing thigh 5) that comes out and the water that comes out from azeotropic distillation column overhead quantizer (stream thigh 9), the mixed solution that comes out from the solvent recuperation column overhead (stream strand 14) passes back into the T3 column overhead through a part after the solvent recovery tower overhead condenser E3 condensation (stream strand 15), another part (stream strand 16) with send into quantizer V1 after the phlegma that comes out from azeotropy rectification column T2 overhead condenser E1 mixes.
Fig. 2 is each parameter of extraction tower T1 among the embodiment 1,20～25 ℃ of T1 tower service temperatures.
Fig. 3 is each parameter of azeotrope column T2 among the embodiment 1,98.7 ℃ of T2 cat head temperature, 118.0 ℃ of still temperature, reboiler energy consumption: 9854.7kW.
Fig. 4 is each parameter of solvent recovery tower T3 among the embodiment 1,81.1 ℃ of T3 cat head temperature, 100.0 ℃ of still temperature, reboiler energy consumption: 755.7kW.
Fig. 5 is each parameter of extraction tower T1 among the embodiment 2,20～25 ℃ of T1 tower service temperatures.
Fig. 6 is each parameter of azeotrope column T2 among the embodiment 2,91.3 ℃ of T2 cat head temperature, 117.9 ℃ of still temperature, reboiler energy consumption: 6203.4kW.
Fig. 7 is each parameter of solvent recovery tower T3 among the embodiment 2,59.9 ℃ of T3 cat head temperature, 100.0 ℃ of still temperature, reboiler energy consumption: 2144.4kW.
Embodiment
Sec-butyl acetate in a kind of method of sec-butyl acetate extraction-azeotropic distillation recovery dilute acetic acid is the extraction agent of extraction tower and the entrainer of azeotropy rectification column; A part that with mass concentration is 10%～35% dilute acetic acid is sent into the filler extraction top of tower, and the trim the top of column liquid of azeotropy rectification column divides a small gangs of to deliver to the bottom of extraction tower as extraction agent, carries out the extraction of normal temperature counter current contact with dilute acetic acid; The extraction tower cat head obtains containing the extraction phase of sec-butyl acetate, acetic acid and less water; It is the water that contains acetate in minute that the tower still obtains extracting phase, and extracting phase enters solvent recovery tower;
The extraction phase of extraction tower is sent into the first half of azeotropy rectification column and is further carried dense, another part sec-butyl acetate is sent into the azeotropic distillation column overhead, another strand dilute acetic acid solution adds azeotropic distillation Tata middle part simultaneously, through azeotropic distillation, cat head obtains the two-phase mixture of sec-butyl acetate and water, contain the secondary butyl ester of small amount of acetic acid through the water after the phase splitter layering, water enters solvent recovery tower after the cat head extraction, and oil phase returns azeotropy rectification column.
The packed height of described packed extraction tower is equivalent to 20～30 theoretical stages, and the extraction tower operational condition is: atmospheric operation, extraction temperature are 20～25 ℃, and dilute acetic acid and sec-butyl acetate feed volume throughput ratio are 1:(1～3).
The processing condition of described azeotropy rectification column are: atmospheric operation, bed stuffing height are equivalent to 45～55 theoretical stages, and the volume flow ratio that enters the sec-butyl acetate of the dilute acetic acid of azeotropy rectification column and azeotropy rectification column trim the top of column is: 1:(1～7).
The concentration that described extraction tower cat head obtains containing acetic acid in the extraction phase of sec-butyl acetate, acetic acid and less water is 7%～15%.
The first half that the extraction phase of described extraction tower is sent into azeotropy rectification column is further carried dense, and the height that enters azeotropy rectification column is the 23rd～27 theoretical stage.
The entrainer sec-butyl acetate of described azeotropy rectification column is added by the 1st block of column plate of cat head.
The height that described another strand dilute acetic acid solution adds azeotropic distillation Tata middle part is the 28th～32 theoretical stage.
The percentage extraction of described extraction tower 〉=95%, described azeotropic distillation column overhead distillates the mixed solution that contains sec-butyl acetate, water and acetic acid, and wherein the mass concentration of acetic acid is below 0.5%, and the described oil phase that returns azeotropy rectification column is mainly sec-butyl acetate.
Extracting phase that described extraction Tata still comes out and azeotropy rectification column cat head come out to enter solvent recovery tower jointly through the water after the layering and reclaim solvent; The rate of recovery of described extraction-azeotropic distillation technology acetic acid is higher than 95%, and the concentration of the acetic acid of the aqueous phase in the extracting phase of extraction tower, after the layering of azeotropic distillation column overhead is less than 0.5%.
Embodiment 1
As shown in Figure 1, sending into flow by pipeline 1 to the extraction tower top is 6m
3/ h, acetic acid concentration are 26.54% dilute acetic acid solution, and sending into flow from pipeline 2 to the extraction tower bottom is 17.5m
3/ h, concentration are 97.87% sec-butyl acetate, and behind the counter-current extraction, cat head extraction phase flow is 1.851 m in extraction tower T1
3/ h, contain acetate 9.077%, tower still extracting phase flow is 4.008m
3/ h contains acetic acid concentration 0.7%.Send into the 25th theoretical stage of azeotropy rectification column from the extraction phase (stream thigh 3) that the extraction tower cat head comes out, the extracting phase that the tower still comes out (stream thigh 5) is sent into solvent recovery tower T3 recovery solvent wherein.Adding inbound traffics by pipeline 6 to azeotropy rectification column T2 cat head is 69.0 m
3/ h, concentration are 97.87% sec-butyl acetate.Another concentration is 26.54%, flow is 6m
3The dilute acetic acid of/h (stream thigh 4) is from the 30th column plate charging of azeotropy rectification column, in azeotrope column, realize azeotropic distillation, from the come out mixed solution of sec-butyl acetate and water of azeotropy rectification column 2 cats head, after the quantizer layering, recovery obtains the secondary butyl ester of solvent acetic acid, and the aqueous phase acetic acid content is sent into solvent recovery tower T3 recovery solvent wherein less than 0.4%.The tower still comes out to be flow 3m
3/ h concentration is greater than 99% acetic acid.Concrete data are seen Fig. 2～4.
Embodiment 2
As shown in Figure 1, sending into flow by pipeline 1 to the extraction tower top is 6m
3/ h, acetic acid concentration are 10% dilute acetic acid solution, and sending into flow from pipeline 2 to the extraction tower bottom is 17.5m
3/ h, concentration are 97.79% sec-butyl acetate, and behind the counter-current extraction, cat head extraction phase flow is 17.935 m in extraction tower T1
3/ h, contain acetate 3.6%, tower still extracting phase flow is 5.255m
3/ h contains acetic acid concentration 0.3%.Send into the 25th theoretical stage of azeotropy rectification column from the extraction phase (stream thigh 3) that the extraction tower cat head comes out, the extracting phase that the tower still comes out (stream thigh 5) is sent into solvent recovery tower T3 recovery solvent wherein.Adding inbound traffics by pipeline 6 to azeotropy rectification column T2 cat head is 31.5m
3/ h, concentration are 97.79% sec-butyl acetate.Another part concentration is 26.54%, flow is 6m
3The dilute acetic acid of/h (stream thigh 6) is from the 30th column plate charging of azeotropy rectification column, in azeotrope column, realize azeotropic distillation, from the come out mixed solution of sec-butyl acetate and water of azeotropy rectification column 2 cats head, after the quantizer layering, recovery obtains the secondary butyl ester of solvent acetic acid, and the aqueous phase acetic acid content is sent into solvent recovery tower T3 recovery solvent wherein less than 0.3%.The tower still comes out to be flow 3m
3/ h concentration is greater than 99% acetic acid.Concrete data are seen Fig. 5～7..
The above only is preferred embodiment of the present invention, and all equalizations of being done according to the present patent application claim change and modify, and all should belong to covering scope of the present invention.
Claims (8)
1. a sec-butyl acetate extraction-azeotropic distillation reclaims the method for dilute acetic acid, and it is characterized in that: the sec-butyl acetate in the described method is the extraction agent of extraction tower and the entrainer of azeotropy rectification column; Part dilute acetic acid is sent into the filler extraction top of tower, and the trim the top of column liquid of azeotropy rectification column divides a small gangs of to deliver to the bottom of extraction tower as extraction agent, carries out the extraction of normal temperature counter current contact with dilute acetic acid; The extraction tower cat head obtains containing the extraction phase of sec-butyl acetate, acetic acid and less water; The extracting phase that the tower still obtains is the water that contains acetate in minute, and extracting phase enters solvent recovery tower;
The extraction phase of extraction tower is sent into the first half of azeotropy rectification column and is further carried dense, another part sec-butyl acetate is sent into the azeotropic distillation column overhead, another strand dilute acetic acid solution adds azeotropic distillation Tata middle part simultaneously, through azeotropic distillation, the cat head of azeotropy rectification column distillates the two-phase mixture that comprises sec-butyl acetate, water and minute quantity acetic acid, contain the secondary butyl ester of small amount of acetic acid through the water after the phase splitter layering, water enters solvent recovery tower after the cat head extraction, oil phase returns azeotropy rectification column, and azeotropic distillation Tata stilling goes out mass content greater than 95% acetic acid.
2. a kind of sec-butyl acetate extraction-azeotropic distillation according to claim 1 reclaims the method for dilute acetic acid, it is characterized in that: the packed height of described packed extraction tower is equivalent to 20～30 theoretical stages, the extraction tower operational condition is: atmospheric operation, extraction temperature is 20～25 ℃, and dilute acetic acid and sec-butyl acetate feed volume throughput ratio are 1:(1～3).
3. a kind of sec-butyl acetate extraction-azeotropic distillation according to claim 1 reclaims the method for dilute acetic acid, it is characterized in that: the processing condition of described azeotropy rectification column are: atmospheric operation, bed stuffing height is equivalent to 45～55 theoretical stages, and the volume flow ratio that enters the sec-butyl acetate of the dilute acetic acid of azeotropy rectification column and azeotropy rectification column trim the top of column is: 1:(1～7).
4. a kind of sec-butyl acetate extraction-azeotropic distillation according to claim 1 reclaims the method for dilute acetic acid, and it is characterized in that: described extraction tower cat head obtains containing the extraction phase of sec-butyl acetate, acetic acid and less water, and wherein the concentration of acetic acid is 7%～15%.
5. a kind of sec-butyl acetate extraction-azeotropic distillation according to claim 1 reclaims the method for dilute acetic acid, it is characterized in that:
The first half that the extraction phase of described extraction tower is sent into azeotropy rectification column is further carried dense, and the position that enters azeotropy rectification column is the 23rd～27 theoretical stage.
6. a kind of sec-butyl acetate extraction-azeotropic distillation according to claim 1 reclaims the method for dilute acetic acid, it is characterized in that: the height that described another strand dilute acetic acid solution adds azeotropic distillation Tata middle part is the 28th～32 theoretical stage.
7. a kind of sec-butyl acetate extraction-azeotropic distillation according to claim 1 reclaims the method for dilute acetic acid, it is characterized in that: the percentage extraction of described extraction tower 〉=95%, described azeotropic distillation column overhead distillates the mixed solution that contains sec-butyl acetate, water and acetic acid, wherein the mass concentration of acetic acid is below 0.5%, and the described oil phase that returns azeotropy rectification column is mainly sec-butyl acetate.
8. a kind of sec-butyl acetate extraction-azeotropic distillation according to claim 1 reclaims the method for dilute acetic acid, it is characterized in that: extracting phase that described extraction Tata still comes out and azeotropy rectification column cat head come out to enter solvent recovery tower jointly through the water after the layering and reclaim solvent; The rate of recovery of described extraction-azeotropic distillation technology acetic acid is higher than 95%, and the concentration of the acetic acid of the aqueous phase after the extracting phase of extraction tower, the layering of azeotropic distillation column overhead is less than 0.5%.
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| CN102432453A (en) * | 2011-10-31 | 2012-05-02 | 安丘市鲁安药业有限责任公司 | Process and equipment for purifying dilute acetic acid solution |
| 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 |
| CN105272845A (en) * | 2014-07-24 | 2016-01-27 | 中国石化扬子石油化工有限公司 | Acetic acid and water separation method in aromatic carboxylic acid production |
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Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
-
2011
- 2011-02-28 CN CN2011100472738A patent/CN102153458A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| 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 |
Non-Patent Citations (1)
| Title |
|---|
| 胡云光: "醋酸仲丁酯的应用及其正丁烯法生产技术", 《精细石油化工》 * |
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| CN102432453A (en) * | 2011-10-31 | 2012-05-02 | 安丘市鲁安药业有限责任公司 | Process and equipment for purifying dilute acetic acid solution |
| 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 |
| CN102746135B (en) * | 2012-08-01 | 2015-03-25 | 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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Application publication date: 20110817 |