CN101209955A - Methyl acetate hydrolysis catalysis reaction rectifying device and realization technique - Google Patents
Methyl acetate hydrolysis catalysis reaction rectifying device and realization technique Download PDFInfo
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- CN101209955A CN101209955A CNA2007100601268A CN200710060126A CN101209955A CN 101209955 A CN101209955 A CN 101209955A CN A2007100601268 A CNA2007100601268 A CN A2007100601268A CN 200710060126 A CN200710060126 A CN 200710060126A CN 101209955 A CN101209955 A CN 101209955A
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Abstract
The invention relates to a rectification device of catalyzed hydrolysis reaction of methyl acetate and a process method thereof, which comprises a reboiler, a catalysis rectifying tower, a condenser, a fixed bad reactor and pipe-lines. The catalysis rectifying tower consists of an upper segment, a middle segment and a lower segment. By making use of the process of combining the catalysis rectifying tower with the fixed bed reactor, the catalysis rectifying tower is divided into a mixing and preheating segment of methyl acetate and water, a catalysis rectifying segment and a methyl acetate stripping segment; after mixing and preheating in upper segment of tower, part of the methyl acetate, water and backflow liquid, is leaded out of the tower, and part thereof continuously flows to the rectifying segment of catalysis; the lead-out part is sent into the upper part of stripping segment after being sent to the fixed bed reactor for hydrolysis reaction; under the rectifying function in the lower segment and after the concentration of methyl acetate is increased, the obtained material is sent into the rectifying segment of the catalysis; the hydrolyzed material is taken out from the tower, and the content of methyl acetate in the material is extremely low; therefore, hydrolysis rate of methyl acetate is enhanced. The hydrolysis rate of methyl acetate of the invention can reach 60-99.9 percent; besides, the difficulty of catalyzer loading and regeneration is also solved.
Description
Technical field
The present invention relates to a kind of methyl acetate hydrolysis catalysis reaction rectifying device and realize processing method.
Background technology
In polyvinyl alcohol (PVA) production process, to produce a large amount of ritalin by products, 1000 kilograms of PVA of every production just produce 1500 kilograms of ritalins, how to make ritalin become basic raw material acetic acid and the methyl alcohol of producing PVA, just become the key in the PVA production.All adopt fixed-bed reactor to be hydrolyzed at present both at home and abroad, percent hydrolysis is generally 23-27%, and a large amount of undecomposed ritalins need to return reactor after rectifying separation, and have azeotrope to exist in the hydrolyzed solution, so equipment is numerous and jumbled and energy consumption is very high.
(CA 96164550n), makes fibrous being wrapped on the sticking plaster to ion-exchange resin catalyst, then is seated in the tower for Japanese Patent (8207.259) and document; Or cylindrical being molded under ion exchange resin and the high density polyethylene(HDPE) heating and melting, then be filled in the tower, make trouble, catalyzer easily comes off, and reclaims difficulty.Chinese patent (CN1163259A) is inserted in the tower with 5 catalyst structure unit vertical interlaceds of tying up packet mode formation at least, and also there is the problem that catalyst elements is complicated and the life-time service catalyzer comes off in this method.Chinese patent (CN 1343649A) is designed to the ritalin reaction tower to have a plurality of rectifying sections and the catalyst reaction section of indirect arrangement, rectifying section uses column plate, catalyst reaction section is equipped with catalyzer, this method combines rectifying and reaction process, but rectifying and reaction process segmentation are carried out, the superiority of catalytic reaction rectification is difficult to demonstrate fully, be to lean on the gravity natural back flow between the rectifying section conversion zone, need occupy certain tower height, thereby can not too much segmentation, also there is the problem of catalyst regeneration difficulty.
Summary of the invention
The object of the present invention is to provide a kind of methyl acetate hydrolysis catalysis reaction rectifying device and realize processing method, utilize the technical process of catalytic rectifying tower in conjunction with fixed-bed reactor, the methyl acetate catalysis reactive distillation processes is carried out continuously, also solved the problem of catalyst loading and regeneration difficulty simultaneously.
The invention provides methyl acetate hydrolysis catalysis reaction rectifying device and comprise supplementary units such as reboiler, catalytic rectifying tower, condenser fixed-bed reactor and pipeline.Pipeline comprises: pipeline 8, pipeline 9, pipeline 10, pipeline, 11 pipelines 12 and pipeline 15.Catalytic rectifying tower 2 is formed by three sections: epimere 7, stage casing 6 and hypomere 5.
Described epimere is ritalin-water mixing preheating section, is formed or is made up of the various fillers of certain altitude by 1 to 15 layer of column plate.
Described stage casing is the catalytic reaction rectification section, and this section stage number can be 10 to 50 layers of catalytic rectifying tower plate, also can be the filler of various loading catalysts.The number of plies of column plate can be 10 to 50 layers, by the three-dimensional catalytic rectifying tower plate that catalyst basket is formed is installed between the calotte of combined trapezoid spray tray, utilize the characteristics of combined trapezoid spray tray liquid lifting capacity big (5-12kg liquid/kg gas), repeatedly flow through catalyzer when making liquid by column plate, assurance reaction and rectifying are efficiently carried out simultaneously; Described catalyst basket adds wire cloth by the porous gabion and constitutes, and is placed in the liquid, there is no gas phase in the catalyst basket and passes through, and can guarantee that therefore catalyzer can be not broken; Also can constitute by the catalytic rectifying tower plate or the filler of other form.
Hypomere is the ritalin stripping section, and this section is made up of 5 to 25 layers of column plate or the various fillers of certain altitude are formed.
Fixed-bed reactor among the present invention can be 1 to 10 parallel operations, these fixed-bed reactor can be just the same with the methyl acetate hydrolysis tower structure in the present PVA production process, even can directly use the present equipment of usefulness again, can save a large amount of facility investments on the one hand, on the other hand, the filling of catalyzer, regeneration can be identical with present method, can guarantee that fully the methyl acetate hydrolysis rate maintains high level in the whole production cycle.
The step of processing method of the present invention is:
1) ritalin enters top of tower from pipeline, and outside pipeline was drawn tower, part continued to flow into tower catalytic reaction rectification section through tower epimere mixing preheating rear section.
2) part of drawing ritalin enters fixed-bed reactor and is hydrolyzed after the reaction, enters a certain position at this tower methyl esters stripping section top to middle part of reactive distillation section from pipeline; Flow into the ritalin and the water of catalytic reaction rectification section, hydrolysis reaction and rectifying carry out simultaneously on every layer of column plate of this section.
3) material that flows down from the stage casing with through after the reacted mixing of materials of fixed-bed reactor, refinery distillation through the ritalin stripping section, make the raising of ritalin concentration and enter the catalytic reaction rectification section, the ritalin content that flows in the reboiler material is reduced so that trace.
4) partial hydrolysis reaction product is by the pipeline extraction.
In this technical process, the ritalin for the treatment of hydrolysis can be 92% methyl esters (being the overhead product of extractive distillation column), also can be the charging of this extractive distillation column, can save the extractive distillation column of present use when promptly using this flow process.(an indispensable tower in the PVA production technique recycle section at present)
The filler of described catalytic reaction rectification section can be Zeo-karb (for example, 001x7 type storng-acid cation exchange resin or C100/6100H type cation exchange resin catalyst etc.), also can be the various fillers that include Zeo-karb.
The present invention utilizes the technical process of three-dimensional catalytic rectifying tower in conjunction with fixed-bed reactor, the methyl acetate catalysis reactive distillation processes is carried out continuously, very low even micro-by ritalin content in the material after the tower still extraction hydrolysis, improve the methyl acetate hydrolysis rate, can make the methyl acetate hydrolysis rate reach 60% to 99.9%.Also solved simultaneously the problem of catalyst loading and regeneration difficulty.
Description of drawings
Fig. 1 is the methyl acetate hydrolysis catalysis reaction rectifying device synoptic diagram.
Embodiment
The present invention can illustrate by example
As shown in the figure, the present invention includes: reboiler 1, catalytic rectifying tower 2, condenser 3, fixed-bed reactor 4, pipeline 8, pipeline 9, pipeline 10, pipeline, 11 pipelines 12 and pipeline 15 and other supplementary unit.Catalytic rectifying tower 2 is formed by three sections: epimere 7, stage casing 6 and hypomere 5.
The concrete processing method of the present invention is: epimere 7 is ritalin-water mixing preheating section; Stage casing 6 is the catalytic reaction rectification section; Hypomere 5 is the ritalin stripping section.Ritalin enters top of tower from pipeline 9, phegma from pipeline 10 from pipeline 8, water, through tower epimere mixing preheating rear section from pipeline 11 draw outside the tower, part continues to flow into tower catalytic reaction rectification section.Extension enters fixed-bed reactor 4 and is hydrolyzed after the reaction, enters a certain position at this tower methyl esters stripping section 5 tops to middle part of reactive distillation section 6 from pipeline 12.Flow into the ritalin and the water of catalytic reaction rectification section, hydrolysis reaction and rectifying carry out simultaneously on every layer of column plate of this section.The material that flows down from stage casing 6 with through after the fixed-bed reactor 4 reacted mixing of materials, refinery distillation through ritalin stripping section 5, make the raising of ritalin concentration and enter the catalytic reaction rectification section, the ritalin content that flows in reboiler 1 material is reduced so that trace, and a part as the extraction of hydrolysis reaction product, can make the methyl acetate hydrolysis rate reach 60% to 99.9% by pipeline 15 like this.
The epimere ritalin of the catalytic rectifying tower among the present invention-water mixing preheating section can be made up of 1 to 15 layer of column plate, also can be made up of the various fillers of certain altitude.
The stage casing is the catalytic reaction rectification section, can be by the three-dimensional catalytic rectifying tower plate that catalyst basket is formed is installed between the calotte of combined trapezoid spray tray, utilize the characteristics of combined trapezoid spray tray liquid lifting capacity big (5-12kg liquid/kg gas), repeatedly flow through catalyzer when making liquid by column plate, assurance reaction and rectifying are efficiently carried out simultaneously, catalyst basket adds wire cloth by the porous gabion and constitutes, be placed in the liquid, there is no gas phase in the catalyst basket passes through, therefore can guarantee that catalyzer can be not broken, also can be made of the catalytic rectifying tower plate or the filler of other form, the number of plies of this section column plate can be 10 to 50 layers.
Hypomere is the ritalin stripping section, and this section can be made up of 5 to 25 layers of column plate, also can be made up of the various fillers of certain altitude.
In this technical process, the ritalin for the treatment of hydrolysis can be 92% methyl esters (being the overhead product of extractive distillation column), also can be the charging of this extractive distillation column, can save the extractive distillation column of present use when promptly using this flow process.
Designed catalytic rectifying tower is characterized in that being divided into three sections: epimere is ritalin-water mixing preheating section, and this section can be made up of 1 to 15 layer of column plate, also can be made up of the various fillers of certain altitude; The stage casing is the catalytic reaction rectification section, and this section stage number can be 10 to 50 layers of catalytic rectifying tower plate, also can be the filler of various loading catalysts; Hypomere is the ritalin stripping section, and this section can be made up of 5 to 25 layers of column plate, also can be made up of the various fillers of certain altitude.
Fixed-bed reactor among the present invention can be 1 to 10 parallel operations, these fixed-bed reactor can be just the same with the methyl acetate hydrolysis tower structure in the present PVA production process, even can directly use the present equipment of usefulness again, can save a large amount of facility investments on the one hand, on the other hand, the filling of catalyzer, regeneration can be identical with present method.
Application example 1
Reaction fractionating tower is formed by three sections: 6 layers of column plate of epimere (ritalin-water mixing preheating section); The 30 layers of Reactive Stage in stage casing (catalytic reaction rectification section); 12 layers of column plate of hypomere (ritalin stripping section), tower diameter 1.2m.The water ester mol ratio of feed water and charging ritalin be respectively 2.0,3.0,4.0,6.0 stable after, tower still acetate concentration is 49.2%, 41.8%, 40.7%, 31.99%, hydrolysis conversion is respectively 63%, 68%, 85%, 98.9%.
Application example 2
Reaction fractionating tower is formed by three sections: 4 layers of column plate of epimere (ritalin-water mixing preheating section); Stage casing (catalytic reaction rectification section) 16m filler (the catalytic reaction rectification filler contains 001x7 type storng-acid cation exchange resin); 10 layers of column plate of hypomere (ritalin stripping section), tower diameter 2.4m.The water ester mol ratio of feed water and charging ritalin is 4.0, stable after, tower still acetate concentration is 35%, hydrolysis conversion is 70%.
Application example 3
Reaction fractionating tower is formed by three sections: 4 layers of column plate of epimere (ritalin-water mixing preheating section); Stage casing (catalytic reaction rectification section) 16m filler (the catalytic reaction rectification filler contains C100/6100H type cation exchange resin catalyst); Hypomere (ritalin stripping section) 5m Mellapak packing, tower diameter 2.4m.The water ester mol ratio of feed water and charging ritalin is 2.0, stable after, tower still acetate concentration is 49.2%, hydrolysis conversion is 61.7%.
Claims (10)
1. methyl acetate hydrolysis catalysis reaction rectifying device, it is characterized in that it comprises reboiler, catalytic rectifying tower, condenser, fixed-bed reactor and pipeline, reboiler, catalytic rectifying tower, condenser and fixed-bed reactor are connected by pipeline successively, and catalytic rectifying tower is made up of for three sections epimere, stage casing and hypomere.
Described epimere is ritalin-water mixing preheating section, and the stage casing is the catalytic reaction rectification section, and hypomere is the ritalin stripping section.
2. rectifier unit according to claim 1 is characterized in that described ritalin-water mixing preheating section formed or be made up of various fillers by 1 to 15 layer of column plate.
3. rectifier unit according to claim 1, the number of plies that it is characterized in that the column plate of described catalytic reaction rectification section are 10 to 50 layers.
4. rectifier unit according to claim 3 is characterized in that described column plate is that the three-dimensional catalytic rectifying tower plate that catalyst basket is formed is installed between the calotte of combined trapezoid spray tray.
5. rectifier unit according to claim 4 is characterized in that described catalyst basket is added by the porous gabion that wire cloth constitutes or the filler of other form.
6. rectifier unit according to claim 1 is characterized in that described ritalin stripping section is made up of 5 to 25 layers of column plate or various filler is formed.
7. rectifier unit according to claim 1 is characterized in that described fixed-bed reactor are 1 to 10 parallel operations.
8. realization processing method of utilizing the described methyl acetate hydrolysis catalysis reaction rectifying device of claim 1 is characterized in that the step that comprises is:
1) ritalin enters top of tower from pipeline, and outside pipeline was drawn tower, part continued to flow into tower catalytic reaction rectification section through tower epimere mixing preheating rear section.
2) part of drawing ritalin enters fixed-bed reactor and is hydrolyzed after the reaction, enters a certain position at this tower methyl esters stripping section top to middle part of reactive distillation section from pipeline; Flow into the ritalin and the water of catalytic reaction rectification section, hydrolysis reaction and rectifying carry out simultaneously on every layer of column plate of this section or in the filler of cation exchange resin catalyst.
3) material that flows down from the stage casing with through after the reacted mixing of materials of fixed-bed reactor, through the rectifying of ritalin stripping section;
4) partial hydrolysis reaction product is by the pipeline extraction.
9. method according to claim 8, the filler that it is characterized in that described catalytic reaction rectification section are Zeo-karb or the various fillers that include Zeo-karb.
10. method according to claim 8 is characterized in that described cat head treats that the ritalin of hydrolysis is 92% the methyl esters or the charging of this extractive distillation column.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CNA2007100601268A CN101209955A (en) | 2007-12-24 | 2007-12-24 | Methyl acetate hydrolysis catalysis reaction rectifying device and realization technique |
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| CNA2007100601268A CN101209955A (en) | 2007-12-24 | 2007-12-24 | Methyl acetate hydrolysis catalysis reaction rectifying device and realization technique |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012164573A2 (en) | 2011-05-27 | 2012-12-06 | Reliance Industries Ltd., | Hydrolysis and esterification with acid catalysts |
| 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 |
| CN110559678A (en) * | 2019-10-21 | 2019-12-13 | 无锡赫利邦化工科技有限公司 | rectifying tower for synthesizing and separating polymethoxy dimethyl ether and use method thereof |
| CN111072465A (en) * | 2019-12-27 | 2020-04-28 | 江苏兄弟维生素有限公司 | Esterification hydrolysis process, esterification hydrolysis reactor and application |
| CN111662319A (en) * | 2020-07-24 | 2020-09-15 | 浙江皇马科技股份有限公司 | Preparation method of low-color 3-isocyanatopropyl trimethoxy silane |
| CN114057563A (en) * | 2020-08-06 | 2022-02-18 | 天津华信化工技术有限公司 | Method for rectifying and hydrolyzing organic acid ester by slurry catalytic reaction |
| CN114904462A (en) * | 2022-06-30 | 2022-08-16 | 中国天辰工程有限公司 | Method and system for continuously producing allyl alcohol |
-
2007
- 2007-12-24 CN CNA2007100601268A patent/CN101209955A/en active Pending
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2012164573A2 (en) | 2011-05-27 | 2012-12-06 | Reliance Industries Ltd., | Hydrolysis and esterification with acid catalysts |
| 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 |
| 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 |
| CN110559678A (en) * | 2019-10-21 | 2019-12-13 | 无锡赫利邦化工科技有限公司 | rectifying tower for synthesizing and separating polymethoxy dimethyl ether and use method thereof |
| CN110559678B (en) * | 2019-10-21 | 2024-02-27 | 无锡赫利邦化工科技有限公司 | Rectifying tower for synthesizing and separating polymethoxy dimethyl ether and application method thereof |
| CN111072465A (en) * | 2019-12-27 | 2020-04-28 | 江苏兄弟维生素有限公司 | Esterification hydrolysis process, esterification hydrolysis reactor and application |
| CN111662319A (en) * | 2020-07-24 | 2020-09-15 | 浙江皇马科技股份有限公司 | Preparation method of low-color 3-isocyanatopropyl trimethoxy silane |
| CN114057563A (en) * | 2020-08-06 | 2022-02-18 | 天津华信化工技术有限公司 | Method for rectifying and hydrolyzing organic acid ester by slurry catalytic reaction |
| CN114904462A (en) * | 2022-06-30 | 2022-08-16 | 中国天辰工程有限公司 | Method and system for continuously producing allyl alcohol |
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Open date: 20080702 |