CN102190556A - Method for hydrolyzing methyl acetate - Google Patents
Method for hydrolyzing methyl acetate Download PDFInfo
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- CN102190556A CN102190556A CN2010101162984A CN201010116298A CN102190556A CN 102190556 A CN102190556 A CN 102190556A CN 2010101162984 A CN2010101162984 A CN 2010101162984A CN 201010116298 A CN201010116298 A CN 201010116298A CN 102190556 A CN102190556 A CN 102190556A
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Abstract
The invention relates to a method for hydrolyzing methyl acetate, which mainly solves the problems that the conventional methyl acetate hydrolysis reaction distillation process is implemented by a reaction distillation tower and a product separation tower, the flow is complex and the energy consumption is high. The method comprises the following steps of: making methyl acetate and water enter a reaction section of a reaction distillation separation tower, fully refluxing on a feed side tower top, extracting methanol on an extraction side tower top of the reaction distillation separation tower, and obtaining aqueous solution of acetic acid at the tower bottom, wherein the reaction distillation separation tower comprises a reaction distillation separation tower body, a feed side overhead condenser, an extraction side overhead condenser and a reboiler; and the reaction distillation separation tower body comprises a raw material feed hole, a feed side tower top feed hole, a feed side tower top discharging hole, an extraction side tower top feed hole, an extraction side tower top discharging hole, a tower bottom feed hole, a tower bottom discharging hole, a division plate, a reaction section, an extraction side rectifying section and a public stripping section. The technical scheme better solves the problems, and the method can be used for industrial production for recovering a byproduct, namely methyl acetate, in the polyvinyl alcohol production process.
Description
Technical field
The present invention relates to a kind of method of methyl acetate hydrolysis.
Background technology
A large amount of by-product methyl acetates is arranged in the polyvinyl alcohol production process, and according to estimates, 1 ton of polyvinyl alcohol of every production is with the ritalin of 1.5～1.7 tons of by-products.Because the ritalin industrial use is little, need it is hydrolyzed into acetic acid and methyl alcohol, behind separation and purification, methyl alcohol is used for vinyl acetate between to for plastic polymerization workshop section, and it is synthetic that acetic acid is used for vinyl acetate between to for plastic.It is the fixed bed hydrolysis process of methyl acetate of catalyzer that domestic and international in the past each manufacturer all adopts with ion exchange resin.The shortcoming of this technology is per pass conversion low (percent hydrolysis can only reach 23%～24%), and a large amount of unreacted ritalins need reclaim circulation, and equipment is huge, energy consumption height, and the separation process complexity of hydrolysate.In recent years, catalytic distillation hydrolysis ritalin technical study is achieved success, and progressively is applied to suitability for industrialized production.Owing to adopted reaction rectification technique, reaction mass is separated in rectifying, and product is in time removed from reaction zone, reaction process always is under the higher ritalin concentration, thereby has improved percent hydrolysis.Industrial applications shows: the methyl acetate hydrolysis rate reaches 53%～57%, compares with the fixed bed hydrolysis process, has enlarged the processing power of equipment, has reduced catalyst consumption and has reduced energy consumption.However, still exist sepn process complexity and a large amount of unhydrolysed ritalins to need the round-robin problem.
Chinese patent literature CN1380273A has introduced present methyl acetate catalysis rectification hydrolysis technique, and the domestic full scale plant that adopts methyl acetate catalysis rectification hydrolysis technique the earliest built up and goes into operation in Fujian textile chemical fiber Group Co.,Ltd in 2000.This technology is mainly by catalytic rectifying tower, extractive distillation column, dealcoholize column, degreasing tower and azeotropy rectification column are formed, ritalin enters extractive distillation column with the ritalin that loops back from the degreasing tower, overhead distillate is a ritalin, obtain methanol aqueous solution at the bottom of the tower, methanol aqueous solution enters dealcoholize column, overhead distillate is a methyl alcohol, obtain water at the bottom of the tower, loop back extractive distillation column and make solvent, ritalin and water are mixed into catalytic rectifying tower, the cat head total reflux, discharging enters the degreasing tower at the bottom of the tower, and overhead distillate is ritalin and carbinol mixture, obtain aqueous acetic acid at the bottom of the tower, aqueous acetic acid enters azeotropy rectification column, and overhead distillate is the water that removes, and obtains acetic acid at the bottom of the tower.Because the extractive distillation column methyl acetate hydrolysis is still incomplete in the technology, follow-up flow process must be recycled by the Dichlorodiphenyl Acetate methyl esters, and ritalin, first alcohol and water form ternary azeotrope, make itself and methyl alcohol and water sepn difficulty, needing to increase extractive distillation column realizes separating, therefore there is the flow process complexity in this technology, the problem that energy consumption is high.
Summary of the invention
Technical problem to be solved by this invention is in methyl acetate hydrolysis reaction distillation arts demand reactive distillation column and product knockout tower two towers realization at present, there is the complicated and high problem of energy consumption of flow process, a kind of method of new methyl acetate hydrolysis is provided, and this method has the simple and characteristic of low energy consumption of flow process.
For solving the problems of the technologies described above, the technical solution used in the present invention is as follows, a kind of method of methyl acetate hydrolysis, ritalin and water enter the conversion zone that reaction distillation is separated tower, the total reflux of feeding side cat head, and reaction distillation is separated tower extraction side cat head extraction methyl alcohol, obtain aqueous acetic acid at the bottom of the tower, reaction distillation is separated tower and is comprised reaction distillation separation tower body, feeding side overhead condenser, extraction side overhead condenser, and reboiler, wherein reaction distillation is separated tower body and is comprised material inlet, feeding side cat head opening for feed, feeding side cat head discharge port, extraction side cat head opening for feed, extraction side cat head discharge port, opening for feed at the bottom of the tower, discharge port at the bottom of the tower, division plate, conversion zone, extraction side rectifying section, and public stripping section.
In technique scheme, reaction distillation is separated the interior division plate of tower and tower body is separated into the feeding side rectifying section, conversion zone, feeding side stripping section, extraction side rectifying section, and public stripping section; The feeding side of division plate is a conversion zone, and the extraction side of division plate is an extraction side rectifying section; At the bottom of division plate bottom and the tower between the feed inlet and outlet zone be public stripping section; Material inlet is at least one; Material inlet is positioned at conversion zone, and division plate is until separating column overhead; Conversion zone is filled with the gel type cation exchange resin, and temperature of reaction is 40～80 ℃; The feeding side overhead condenser connects feeding side cat head feed inlet and outlet, behind the tower top outlet vapor condensation, all as refluxing; Extraction side overhead condenser connects extraction side cat head feed inlet and outlet, behind the tower top outlet vapor condensation, first part sends into the cat head import, the second section extraction is as product, the weight ratio of first part and second section material is 1～10: 1, and the controlled temperature that reaction distillation is separated tower extraction side cat head is 64.3～64.7 ℃; Tower bottom reboiler with tower at the bottom of feed inlet and outlet connect, tower bottom outlet liquid first part enters and sends into import at the bottom of the tower after the reboiler vaporization, the second section extraction is as product; Conversion zone is filled with at least a in sulfonate sodium type ion exchange resin or the gel-type polystyrene strong acid sodium ion exchange resin, and temperature of reaction is preferably 45～60 ℃; The raw material ritalin can contain methyl alcohol 0～30 weight %; Ritalin is complete reaction in reaction distillation is separated tower; Water and ritalin mol ratio 1～10: 1; It is 10～80 that conversion zone is equivalent to number of theoretical plate, and extraction side theoretical number of plates of rectifying section is 10～80, and public stripping section number of theoretical plate is 10～50; Water and ritalin raw materials components mole ratio preferred 2～6: 1; Conversion zone is equivalent to number of theoretical plate and is preferably 20～50, and extraction side theoretical number of plates of rectifying section is preferably 20～50, and public stripping section number of theoretical plate is preferably 15～30; Reaction distillation is separated the first part of tower extraction side condenser and the weight ratio of second section material is preferably 3～6: 1.
Produce in the technological process of acetic acid and methyl alcohol at methyl acetate hydrolysis, reactive distillation column is only realized the response function of methyl acetate hydrolysis in essence, the cat head total reflux, ritalin is complete hydrolysis in reactive distillation column, the problem that does not exist ritalin to reclaim, and product methyl alcohol and acetic acid separated must realize in the product knockout tower.So classical inverse answers distil process to be necessary for the combined process flow of reactive distillation column and product knockout tower.Reaction distillation separation tower can be finished reaction distillation and product sepn process separately among the present invention, realizes the effect of two towers unification, compares with traditional technology, and flow process is simple, and promptly reaction distillation is separated tower alternative reaction distillation tower and product knockout tower.Using the present invention is that total energy consumption saving 13.7% has obtained better technical effect under the identical situation of operational conditions such as 50～60 ℃, number of theoretical plate 58 in water and ritalin mol ratio 3.0, temperature of reaction.
Description of drawings
Fig. 1 is the process schematic representation of methyl acetate hydrolysis.
Among Fig. 1,1 is reaction distillation separation tower body, and 2 is material inlet, 3 feeding side cat head discharge ports, 4 is feeding side cat head opening for feed, and 5 are discharge port at the bottom of the extraction side tower, and 6 are opening for feed at the bottom of the extraction side tower, 7 is discharge port at the bottom of the tower, and 8 is opening for feed at the bottom of the tower, and 9 is conversion zone, 10 is public stripping section, and 11 are extraction side rectifying section, and 12 is division plate, 13 is the feeding side overhead condenser, and 14 are extraction side overhead condenser, and 15 is tower bottom reboiler, 16 is raw material, and 17 for the extraction of extraction side cat head, and 18 is extraction at the bottom of the tower.
As shown in Figure 1, raw material 16 enters the material inlet 2 that reaction distillation is separated tower 1, the feeding side overhead vapours enters feeding side overhead condenser 13 from feeding side cat head discharge port 3, all reflux after the condensation and enter feeding side cat head opening for feed 4, extraction side overhead vapours enters extraction side overhead condenser 14 from extraction side cat head discharge port 5, after the condensation, a part enters cat head opening for feed 6, part cat head extraction 17, discharge port 7 dischargings at the bottom of the tower at the bottom of the tower, a part is sent into and is entered opening for feed 8 at the bottom of the tower after tower bottom reboiler 15 evaporation, and a part is as extraction at the bottom of the tower 18.
The present invention is further illustrated below by specific embodiment, and still, scope of the present invention has more than and is limited to the scope that embodiment covers.
Embodiment
[embodiment 1]
By hydrolysis process of methyl acetate shown in Figure 1, public stripping section number of theoretical plate is 15, and it is 18 that the conversion zone separation efficiency is equivalent to number of theoretical plate, and extraction side theoretical number of plates of rectifying section is 25.The catalyzer of conversion zone filling is a sulfonate sodium type ion exchange resin, water enters the 1st theoretical stage separating the tower conversion zone with 2.32 gram/minute flows and (counts from top to bottom, as follows), ritalin enters from separating tower conversion zone bottom with 3.00 gram/minute flows, control conversion zone temperature is 50～60 ℃, it is 64.5 ℃ that tower extraction side tower top temperature is separated in control, the weight ratio of first part and second section material is 4: 1 after the condensation, extraction side cat head produced quantity is 1.30 gram/minute, behind the stable operation, the gained result is 99.97 weight % for extraction side cat head methanol content, acetic acid content is 60.45 weight % at the bottom of the tower, feeding side overhead condenser energy consumption, extraction side overhead condenser and tower bottom reboiler energy consumption, and compare with comparative example and to save energy consumption and see Table 1.
[embodiment 2]
By hydrolysis process of methyl acetate shown in Figure 1, public stripping section number of theoretical plate is 10, and it is 10 that the conversion zone separation efficiency is equivalent to number of theoretical plate, and extraction side theoretical number of plates of rectifying section is 10.The catalyzer of conversion zone filling is a sulfonate sodium type ion exchange resin, water enters the 1st theoretical stage separating the tower conversion zone with 7.25 gram/minute flows and (counts from top to bottom, as follows), ritalin enters from separating tower conversion zone bottom with 3.00 gram/minute flows, control conversion zone temperature is 53～62 ℃, it is 64.3 ℃ that tower extraction side tower top temperature is separated in control, the weight ratio of first part and second section material is 10: 1 after the condensation, the cat head produced quantity is 1.30 gram/minute, behind the stable operation, the gained result is 99.92 weight % for extraction side cat head methanol content, acetic acid content is 27.15 weight % at the bottom of the tower, feeding side overhead condenser energy consumption, extraction side overhead condenser and tower bottom reboiler energy consumption, and compare with comparative example and to save energy consumption and see Table 1.
[embodiment 3]
By hydrolysis process of methyl acetate shown in Figure 1, public stripping section number of theoretical plate is 50, and it is 80 that the conversion zone separation efficiency is equivalent to number of theoretical plate, and extraction side theoretical number of plates of rectifying section is 80.The catalyzer of conversion zone filling is a sulfonate sodium type ion exchange resin, water enters the 1st theoretical stage separating the tower conversion zone with 1.10 gram/minute flows and (counts from top to bottom, as follows), ritalin enters from separating tower conversion zone bottom with 3.00 gram/minute flows, control conversion zone temperature is 41～51 ℃, it is 64.5 ℃ that tower extraction side tower top temperature is separated in control, the weight ratio of first part and second section material is 1: 1 after the condensation, extraction side cat head produced quantity is 1.30 gram/minute, behind the stable operation, the gained result is 99.98 weight % for extraction side cat head methanol content, acetic acid content is 86.79 weight % at the bottom of the tower, feeding side overhead condenser energy consumption, extraction side overhead condenser and tower bottom reboiler energy consumption, and compare with comparative example and to save energy consumption and see Table 1.
[embodiment 4]
By hydrolysis process of methyl acetate shown in Figure 1, public stripping section number of theoretical plate is 20, and it is 30 that the conversion zone separation efficiency is equivalent to number of theoretical plate, and extraction side theoretical number of plates of rectifying section is 30.The catalyzer of conversion zone filling is a gel-type polystyrene strong acid sodium ion exchange resin, water enters the 1st theoretical stage separating the tower conversion zone with 5.28 gram/minute flows and (counts from top to bottom, as follows), ritalin enters from separating tower conversion zone bottom with 3.00 gram/minute flows, control conversion zone temperature is 68～78 ℃, it is 64.6 ℃ that tower extraction side tower top temperature is separated in control, the weight ratio of first part and second section material is 2: 1 after the condensation, extraction side cat head produced quantity is 1.30 gram/minute, behind the stable operation, the gained result is 99.96 weight % for extraction side cat head methanol content, acetic acid content is 34.81 weight % at the bottom of the tower, feeding side overhead condenser energy consumption, extraction side overhead condenser and tower bottom reboiler energy consumption, and compare with comparative example and to save energy consumption and see Table 1.
[embodiment 5]
By hydrolysis process of methyl acetate shown in Figure 1, public stripping section number of theoretical plate is 20, and it is 30 that the conversion zone separation efficiency is equivalent to number of theoretical plate, and extraction side theoretical number of plates of rectifying section is 30.The catalyzer of conversion zone filling is a gel-type acrylic strong acid sodium ion exchange resin, water enters the 1st theoretical stage separating the tower conversion zone with 3.19 gram/minute flows and (counts from top to bottom, as follows), ritalin and carbinol mixture (methyl alcohol contains 25 weight %) enter from separating tower conversion zone bottom with 4.00 gram/minute flows, control conversion zone temperature is 55～64 ℃, it is 64.7 ℃ that tower extraction side tower top temperature is separated in control, the weight ratio of first part and second section material is 8: 1 after the tower condensation, the top produced quantity is 2.30 gram/minute, behind the stable operation, the gained result is 99.96 weight % for extraction side cat head methanol content, acetic acid content is 49.69 weight % at the bottom of the tower, feeding side overhead condenser energy consumption, extraction side overhead condenser and tower bottom reboiler energy consumption, and compare with comparative example and to save energy consumption and see Table 1.
The energy consumption result of each embodiment of table 1
| Embodiment | Feeding side cat head/kilojoule/hour | Extraction side cat head/kilojoule/hour | At the bottom of the tower // kilojoule/hour | Total energy consumption reduction/% |
| 1 | -1.17 | -0.46 | ?2.34 | 13.7 |
| 2 | -1.26 | -0.49 | ?2.52 | 7.2 |
| 3 | -1.08 | -0.43 | ?2.17 | 20.0 |
| 4 | -1.20 | -0.47 | ?2.49 | 9.6 |
| 5 | -1.18 | -0.45 | ?2.43 | 11.7 |
[comparative example 1]
Traditionally, flow process is that reactive distillation column and product knockout tower two towers are formed.The reactive distillation column number of theoretical plate is 18 for the conversion zone separation efficiency is equivalent to number of theoretical plate, and the stripping section number of theoretical plate is 15, and product knockout tower theoretical number of plates of rectifying section is 15, and the stripping section number of theoretical plate is 15.Water (is counted from top to bottom with the 1st theoretical stage that 2.32 gram/minute flows enter the reactive distillation column conversion zone, as follows), ritalin enters from reactive distillation column conversion zone bottom with 3.00 gram/minute flows, the cat head total reflux, full extraction at the bottom of the tower, control conversion zone temperature is 50～60 ℃, extraction liquid enters product knockout tower middle part at the bottom of the tower, control product knockout tower tower top temperature is 64.5 ℃, the cat head produced quantity is 1.30 gram/minute, behind the stable operation, the gained result is 99.98 weight % for extraction side cat head methanol content, and acetic acid content is 60.47 weight % at the bottom of the tower, reactive distillation column overhead condenser energy consumption-1.34 kilojoule/hour, tower bottom reboiler energy consumption 1.89 kilojoules/hour, product knockout tower overhead condenser energy consumption-0.55 kilojoule/hour, tower bottom reboiler energy consumption 0.82 kilojoule/hour.
Claims (10)
1. the method for a methyl acetate hydrolysis, it is characterized by ritalin and water and enter the conversion zone that reaction distillation is separated tower, the total reflux of feeding side cat head, reaction distillation is separated tower extraction side cat head extraction methyl alcohol, obtain aqueous acetic acid at the bottom of the tower, reaction distillation is separated tower and is comprised reaction distillation separation tower body, feeding side overhead condenser, extraction side overhead condenser, and reboiler, wherein reaction distillation is separated tower body and is comprised material inlet, feeding side cat head opening for feed, feeding side cat head discharge port, extraction side cat head opening for feed, extraction side cat head discharge port, opening for feed at the bottom of the tower, discharge port at the bottom of the tower, division plate, conversion zone, extraction side rectifying section, and public stripping section.
2. according to the method for the described methyl acetate hydrolysis of claim 1, it is characterized in that division plate is separated into the feeding side rectifying section with tower body, conversion zone, feeding side stripping section, extraction side rectifying section, and public stripping section in the reaction distillation separation tower; The feeding side of division plate is a conversion zone, and the extraction side of division plate is an extraction side rectifying section; At the bottom of division plate bottom and the tower between the feed inlet and outlet zone be public stripping section.
3. according to the method for claim 1 and 2 described methyl acetate hydrolysis, it is characterized in that material inlet is at least one; Material inlet is positioned at conversion zone, and division plate is until separating column overhead.
4. according to the method for the described methyl acetate hydrolysis of claim 1, it is characterized in that conversion zone is filled with the gel type cation exchange resin, temperature of reaction is 40～80 ℃.
5. according to the method for the described methyl acetate hydrolysis of claim 1, it is characterized in that the feeding side overhead condenser connects feeding side cat head feed inlet and outlet, behind the tower top outlet vapor condensation, all as refluxing; Extraction side overhead condenser connects extraction side cat head feed inlet and outlet, behind the tower top outlet vapor condensation, first part sends into the cat head import, the second section extraction is as product, the weight ratio of first part and second section material is 1～10: 1, and the controlled temperature that reaction distillation is separated tower extraction side cat head is 64.3～64.7 ℃; Tower bottom reboiler with tower at the bottom of feed inlet and outlet connect, tower bottom outlet liquid first part enters and sends into import at the bottom of the tower after the reboiler vaporization, the second section extraction is as product.
6. according to the method for the described methyl acetate hydrolysis of claim 4, it is characterized in that conversion zone is filled with at least a in sulfonate sodium type ion exchange resin or the gel-type polystyrene strong acid sodium ion exchange resin, temperature of reaction is 45～60 ℃.
7. according to the method for the described methyl acetate hydrolysis of claim 1, it is characterized in that the raw material ritalin can contain methyl alcohol 0～30 weight %.
8. according to the method for the described methyl acetate hydrolysis of claim 1, it is characterized in that ritalin complete reaction in reaction distillation is separated tower.
9. according to the method for the described methyl acetate hydrolysis of claim 1, it is characterized in that water and ritalin mol ratio 1～10: 1; It is 10～80 that conversion zone is equivalent to number of theoretical plate, and extraction side theoretical number of plates of rectifying section is 10～80, and public stripping section number of theoretical plate is 10～50.
10. according to the method for the described methyl acetate hydrolysis of claim 9, it is characterized in that water and ritalin raw materials components mole ratio 2～6: 1; It is 20～50 that conversion zone is equivalent to number of theoretical plate, and extraction side theoretical number of plates of rectifying section is 20～50, and public stripping section number of theoretical plate is 15～30.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102690186A (en) * | 2012-06-12 | 2012-09-26 | 天津大学 | Methyl acetate hydrolysis partition reaction rectification column and operating method thereof |
| CN104030921A (en) * | 2013-07-05 | 2014-09-10 | 中石化上海工程有限公司 | Method for separating vinyl acetate |
| 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 |
| WO2020024886A1 (en) * | 2018-08-03 | 2020-02-06 | 天津大学 | Anti-corrosive process and device for methyl acetate hydrolysis and acetic acid refining in polyvinyl alcohol mother liquor recovery process |
| CN111606797A (en) * | 2020-06-12 | 2020-09-01 | 天津大学 | New reaction rectification process for separating methyl acetate hydrolysate by using bulkhead column |
| CN112694405A (en) * | 2019-10-23 | 2021-04-23 | 中国石油化工股份有限公司 | Method and device for recycling vinyl acetate in EVOH production process |
| CN113443990A (en) * | 2021-06-02 | 2021-09-28 | 天津大学 | Methyl acetate dividing wall tower extraction-reaction rectification hydrolysis process and device |
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Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102690186A (en) * | 2012-06-12 | 2012-09-26 | 天津大学 | Methyl acetate hydrolysis partition reaction rectification column and operating method thereof |
| CN104030921A (en) * | 2013-07-05 | 2014-09-10 | 中石化上海工程有限公司 | Method for separating vinyl acetate |
| CN104030921B (en) * | 2013-07-05 | 2016-06-29 | 中石化上海工程有限公司 | The method separating vinyl acetate |
| 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 |
| WO2020024886A1 (en) * | 2018-08-03 | 2020-02-06 | 天津大学 | Anti-corrosive process and device for methyl acetate hydrolysis and acetic acid refining in polyvinyl alcohol mother liquor recovery process |
| CN109467497B (en) * | 2018-08-03 | 2023-11-10 | 内蒙古蒙维科技有限公司 | Recovery process and device for polyvinyl alcohol alcoholysis mother liquor |
| CN112694405A (en) * | 2019-10-23 | 2021-04-23 | 中国石油化工股份有限公司 | Method and device for recycling vinyl acetate in EVOH production process |
| CN111606797A (en) * | 2020-06-12 | 2020-09-01 | 天津大学 | New reaction rectification process for separating methyl acetate hydrolysate by using bulkhead column |
| CN113443990A (en) * | 2021-06-02 | 2021-09-28 | 天津大学 | Methyl acetate dividing wall tower extraction-reaction rectification hydrolysis process and device |
| CN113443990B (en) * | 2021-06-02 | 2022-12-20 | 天津大学 | Methyl acetate dividing wall tower extraction-reaction rectification hydrolysis process and device |
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