CN104744423A - Method for continuously producing vinylene carbonate - Google Patents
Method for continuously producing vinylene carbonate Download PDFInfo
- Publication number
- CN104744423A CN104744423A CN201510114056.4A CN201510114056A CN104744423A CN 104744423 A CN104744423 A CN 104744423A CN 201510114056 A CN201510114056 A CN 201510114056A CN 104744423 A CN104744423 A CN 104744423A
- Authority
- CN
- China
- Prior art keywords
- vinylene carbonate
- tower
- triethylamine
- solid
- equipment
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
- Granted
Links
Classifications
-
- C—CHEMISTRY; METALLURGY
- C07—ORGANIC CHEMISTRY
- C07D—HETEROCYCLIC COMPOUNDS
- C07D317/00—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms
- C07D317/08—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3
- C07D317/10—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings
- C07D317/32—Heterocyclic compounds containing five-membered rings having two oxygen atoms as the only ring hetero atoms having the hetero atoms in positions 1 and 3 not condensed with other rings with hetero atoms or with carbon atoms having three bonds to hetero atoms with at the most one bond to halogen, e.g. ester or nitrile radicals, directly attached to ring carbon atoms
- C07D317/34—Oxygen atoms
- C07D317/40—Vinylene carbonate; Substituted vinylene carbonates
Landscapes
- Chemical & Material Sciences (AREA)
- Organic Chemistry (AREA)
- Organic Low-Molecular-Weight Compounds And Preparation Thereof (AREA)
Abstract
The invention discloses a method for continuously producing vinylene carbonate. The method is characterized by comprising a production device and a production method, wherein the production device comprises a tubular reactor (1), a solid-liquid separating device (2), a separating tower (3), a fractional condenser (4), a condenser (5), a secondary solid-liquid separating device (6), connecting pipelines of equipment, a display and control instruments as well as accessories. The production method comprises the following steps: continuously introducing raw materials monochloroethylene carbonate and triethylamine into the tubular reactor (1) in proportion; introducing a solid phase which is generated by removing a reaction liquid through the solid-liquid separating device (2) into the separating tower (3); introducing un-reacted triethylamine which is distilled off on the tower top and a vinylene carbonate gas mixture which is generated by reaction into the fractional condenser (4); performing primary condensation to obtain vinylene carbonate, wherein one part of the vinylene carbonate is used as a reflux fluid for being returned to the separating tower (3), and the other part of the vinylene carbonate is used as a product; introducing triethylamine into the condenser (5), circulating and returning to the system to participate in reaction again after condensing; and returning tower-kettle liquid of the separating tower (3) to the system to participate in reaction again.
Description
Technical field
The present invention relates to a kind of preparation method of Chemicals, particularly relate to a kind of method of continuous prodution vinylene carbonate.
Background technology
Vinylene carbonate is a kind of important lithium-ion battery electrolytes additive.Chlorocarbonic acid vinyl acetate can generate vinylene carbonate with triethylamine generation elimination reaction; In this reaction process, the hydrogenchloride generated can react with the triethylamine existed in a large number and generate triethylamine hydrochloride, vinylene carbonate is the ester class that a kind of activity is strong, a kind of dark thick shape material being difficult to be separated can be mixed to form with the triethylamine hydrochloride that dehydrochlorination reaction generates by polymerization reaction take place under high temperature, object product vinylene carbonate is surrounded by sticky mass, is unfavorable for that later separation is more and acquires high-purity product.For obtaining high purity vinylene carbonate as much as possible, people add solvent and are easy to be separated to make product in reaction system; Add stopper to be polymerized to suppress product.
At present, the production process that chlorocarbonic acid vinyl acetate produces methyl ethyl carbonate alkene ester with triethylamine reaction is the periodical operation of autoclave dropwise reaction, and production efficiency is low, and quality product not easily ensures, raw material availability is not high.Develop a kind of method of continuous prodution vinylene carbonate, enhance productivity, improve the quality of products, improve raw material availability significant.
Summary of the invention
The object of this invention is to provide a kind of method being raw material continuous prodution vinylene carbonate with chlorocarbonic acid vinyl acetate and triethylamine, the method adopts the tubular reactor establishing turbulent element in peripheral hardware chuck, and mass-and heat-transfer is effective, and reaction mass contact fully, speed of response is fast, good product quality; The process implementation continuous prodution producing vinylene carbonate with chlorocarbonic acid vinyl acetate and triethylamine reaction can be made.
Technical scheme of the present invention is as follows:
A method for continuous prodution vinylene carbonate, comprises following production equipment and production method:
Production equipment comprises: tubular reactor, equipment for separating liquid from solid, knockout tower, partial condenser, condenser, equipment room connection line, display and control instruments and annex; Tubular reactor 1 be with or without the blank pipe of chuck or in pipe continuously or interruption dynamic and static hybrid element material being played to perturbation action is set;
B. production method comprises: a) raw material chlorocarbonic acid vinyl acetate and triethylamine and stopper enter tubular reactor continuously by regulation mol ratio, control the Axial Temperature Distribution in reactor by tubular reactor chuck transferring heat, make the temperature out of reactor lower than the boiling point (time in tubular reactor outlet material containing unconverted triethylamine) of triethylamine or lower than vinylene carbonate boiling temperature; B) reaction solution going out tubular reactor enters equipment for separating liquid from solid, isolates the reaction solution after solid phase and enters knockout tower; C) knockout tower tower top distillates vinylene carbonate and triethylamine mixing steam, and obtain vinylene carbonate through a condensation, a part makes phegma, and another part does product; Knockout tower overhead vapours time condensation obtains triethylamine retrieval system and again participates in reaction; D) knockout tower tower bottoms circulation retrieval system continues to participate in reaction.
The method of described a kind of continuous prodution vinylene carbonate, feedstock mol ratio preferably adopts chlorocarbonic acid vinyl acetate excessive, makes without triethylamine in pipe reactor outlet material, again participates in the operation of reacting without raw material triethylamine circulation retrieval system;
The method of described a kind of continuous prodution vinylene carbonate, isolate the reaction solution of solid phase preferably by the charging of knockout tower tower reactor, both preferable separation tower only had rectifying section, did not establish stripping section;
The method of described a kind of continuous prodution vinylene carbonate, in knockout tower tower reactor, liquid storage unconverted chlorocarbonic acid vinyl acetate has allowed a certain proportion of vinylene carbonate;
The method of described a kind of continuous prodution vinylene carbonate, before or after equipment for separating liquid from solid is arranged on knockout tower, or all arranges equipment for separating liquid from solid before and after knockout tower;
The method of described a kind of continuous prodution vinylene carbonate, arranges between tubular reactor and equipment for separating liquid from solid or does not arrange reaction solution tundish; Arrange between equipment for separating liquid from solid and knockout tower or parting liquid tundish are not set;
The method of described a kind of continuous prodution vinylene carbonate, the combination that equipment for separating liquid from solid used can be centrifugal separating device, filtering separation device, settling separation device are not limited to these devices and these devices;
The method of described a kind of continuous prodution vinylene carbonate, can adopt double tower to operate from the reaction solution removing solid phase, isolate unconverted raw material triethylamine and reaction product vinylene carbonate;
The method of described a kind of continuous prodution vinylene carbonate, the available solvent not participating in reacting carries out pre-mixing to one raw material or continuously enters tubular reactor after carrying out pre-mixing to two strands of raw materials simultaneously;
advantage of the present invention is:
1. can make the process implementation continuous prodution producing vinylene carbonate with chlorocarbonic acid vinyl acetate and triethylamine reaction;
2. do not pursue a transformation efficiency of raw material, unconverted raw material retrieval system participates in reaction again, and turndown ratio is large;
3. adopt the tubular reactor establishing turbulent element in peripheral hardware chuck, mass-and heat-transfer is effective, and fully, speed of response is fast, good product quality in reaction mass contact;
4. reactants separate adopts tower charging, only has distillation operation, heats up in a steamer without carrying the purity that operation preferentially can ensure overhead product.
Accompanying drawing explanation
The production equipment sketch that Fig. 1 is is raw material continuous prodution vinylene carbonate with chlorocarbonic acid vinyl acetate and triethylamine.
Embodiment
Below in conjunction with accompanying drawing embodiment, the present invention is described in detail.
Embodiment 1
Continuous prodution vinylene carbonate production equipment comprises: tubular reactor 1, equipment for separating liquid from solid 2, knockout tower 3, partial condenser 4, condenser 5, secondary equipment for separating liquid from solid 6, equipment room connection line, control instruments and annex; Tubular reactor 1 straight length is commercially available static mixer, and curved tube section is blank pipe.
Continuous prodution vinylene carbonate production method comprises: raw material chlorocarbonic acid vinyl acetate and triethylamine enter the flowing of tubular reactor limit, limit mixing, limit reaction, limit heat transfer by theoretical mol ratio; The material going out tubular reactor enters the triethylamine hydrochloride that equipment for separating liquid from solid deviates from generation, takes off the liquid phase admittedly and enters knockout tower by tower reactor; Tower top distillates the vinylene carbonate mixing steam of unreacted triethylamine and reaction generation, and a condensation obtains vinylene carbonate in order, and a part is as knockout tower trim the top of column, and another part is as thick product; Time condensation obtains triethylamine retrieval system and again participates in reaction; Knockout tower tower bottoms is unconverted chlorocarbonic acid vinyl acetate and part vinylene carbonate and a small amount of triethylamine hydrochloride, and retrieval system participates in reaction again.
Embodiment 2
Embodiment 2 is substantially the same manner as Example 1, and difference is in raw material chlorocarbonic acid vinyl acetate (or triethylamine), to add stopper in advance, then converges with triethylamine (or chlorocarbonic acid vinyl acetate) and enters tubular reactor.
Embodiment 3
Embodiment 3 is substantially the same manner as Example 1, difference is that one raw material is first mixed into the solvent of regulation ratio before entering the reactor, another strand of raw material is mixed into stopper before entering the reactor in advance, isolate after solid phase through equipment for separating liquid from solid after two strands of raw materials enter reactor reaction, increase solvent recovery operation, the reaction solution taken off after solid and recycling design enters knockout tower.
Embodiment 4
Embodiment 4 is substantially the same manner as Example 1, and difference is all to fill chemical filler in tubular reactor straight length and curved tube section.
Claims (9)
1. a method for continuous prodution vinylene carbonate, is characterized in that, described method comprises production equipment and production method:
A. production equipment comprises: tubular reactor (1), equipment for separating liquid from solid (2), knockout tower (3), partial condenser (4), condenser (5), secondary equipment for separating liquid from solid (6), equipment room connection line, control instruments and annex; Tubular reactor (1) be with or without the blank pipe of chuck or in pipe continuously or interruption dynamic and static perturbation element material being played to perturbation action is set;
B. production method comprises: a) raw material chlorocarbonic acid vinyl acetate and triethylamine and stopper enter tubular reactor (1) continuously by regulation mol ratio, control the Axial Temperature Distribution in reactor by tubular reactor chuck transferring heat, make the temperature out of reactor lower than the boiling point (time in tubular reactor (1) outlet material containing unconverted triethylamine) of triethylamine or lower than vinylene carbonate boiling temperature; B) reaction solution going out tubular reactor (1) enters equipment for separating liquid from solid (2), isolates the reaction solution after solid phase and enters knockout tower (3); C) knockout tower (3) tower top distillates vinylene carbonate and triethylamine mixing steam, and obtain vinylene carbonate through a condensation, a part makes phegma, and another part does product; Knockout tower (3) overhead vapours time condensation obtains triethylamine retrieval system and again participates in reaction; D) knockout tower (3) tower bottoms circulation retrieval system continues to participate in reaction.
2. the method for a kind of continuous prodution vinylene carbonate according to claim 1, it is characterized in that, described feedstock mol ratio preferably adopts chlorocarbonic acid vinyl acetate excessive, make without triethylamine in pipe reactor (1) outlet material, again participate in the operation of reacting without raw material triethylamine circulation retrieval system.
3. the method for a kind of continuous prodution vinylene carbonate according to claim 1, is characterized in that, described in isolate the reaction solution of solid phase preferably by knockout tower (3) tower reactor charging, both preferable separation tower (3) only had rectifying section, did not establish stripping section.
4. the method for a kind of continuous prodution vinylene carbonate according to claim 1, is characterized in that, in described knockout tower (3) tower reactor, liquid storage unconverted chlorocarbonic acid vinyl acetate has allowed a certain proportion of vinylene carbonate.
5. the method for a kind of continuous prodution vinylene carbonate according to claim 1, is characterized in that, before or after described equipment for separating liquid from solid (2) is arranged on knockout tower (3), or all arranges equipment for separating liquid from solid before and after knockout tower (3).
6. the method for a kind of continuous prodution vinylene carbonate according to claim 1, is characterized in that, arranges or do not arrange reaction solution tundish between described tubular reactor (1) and equipment for separating liquid from solid (2); Arrange between equipment for separating liquid from solid (2) and knockout tower (3) or parting liquid tundish are not set.
7. the method for a kind of continuous prodution vinylene carbonate according to claim 1, it is characterized in that, described equipment for separating liquid from solid is centrifugal separating device or filtering separation device or settling separation device, is not limited to the combination of these devices and these devices.
8. the method for a kind of continuous prodution vinylene carbonate according to claim 1, is characterized in that, described method can adopt double tower to operate from the reaction solution removing solid phase, isolate unconverted raw material triethylamine and reaction product vinylene carbonate.
9. the method for a kind of continuous prodution vinylene carbonate according to claim 1, it is characterized in that, described method can adopt the solvent not participating in reacting carry out pre-mixing to one raw material or continuously enter tubular reactor (2) after carrying out pre-mixing to two strands of raw materials simultaneously.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510114056.4A CN104744423B (en) | 2015-03-17 | 2015-03-17 | A kind of process of continuous prodution vinylene carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201510114056.4A CN104744423B (en) | 2015-03-17 | 2015-03-17 | A kind of process of continuous prodution vinylene carbonate |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN104744423A true CN104744423A (en) | 2015-07-01 |
| CN104744423B CN104744423B (en) | 2017-03-01 |
Family
ID=53584767
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201510114056.4A Active CN104744423B (en) | 2015-03-17 | 2015-03-17 | A kind of process of continuous prodution vinylene carbonate |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN104744423B (en) |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174928A (en) * | 2020-11-02 | 2021-01-05 | 浙江天硕氟硅新材料科技有限公司 | Novel vinylene carbonate synthesis preparation method |
| CN112397781A (en) * | 2020-11-17 | 2021-02-23 | 徐文忠 | Lithium battery car electrolyte additive |
| CN112436187A (en) * | 2020-11-24 | 2021-03-02 | 徐文忠 | Gel electrolyte for lithium battery |
| CN114749136A (en) * | 2022-04-14 | 2022-07-15 | 山东惟普新能源有限公司 | Tubular reactor and system device for continuously preparing vinylene carbonate |
| CN115716815A (en) * | 2022-12-22 | 2023-02-28 | 青岛科技大学 | Method and system for continuously preparing vinylene carbonate |
| CN116003374A (en) * | 2022-12-16 | 2023-04-25 | 山东惟普新能源有限公司 | Method for synthesizing immediately separated vinylene carbonate |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN200998645Y (en) * | 2006-09-29 | 2008-01-02 | 沈阳化工学院 | Pipe fluid destabilization device capable of reinforcing mass transfer and heat transfer |
| CN104327037A (en) * | 2014-10-16 | 2015-02-04 | 荣成青木高新材料有限公司 | Vinylene carbonate preparation method |
-
2015
- 2015-03-17 CN CN201510114056.4A patent/CN104744423B/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN200998645Y (en) * | 2006-09-29 | 2008-01-02 | 沈阳化工学院 | Pipe fluid destabilization device capable of reinforcing mass transfer and heat transfer |
| CN104327037A (en) * | 2014-10-16 | 2015-02-04 | 荣成青木高新材料有限公司 | Vinylene carbonate preparation method |
Cited By (10)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112174928A (en) * | 2020-11-02 | 2021-01-05 | 浙江天硕氟硅新材料科技有限公司 | Novel vinylene carbonate synthesis preparation method |
| CN112397781A (en) * | 2020-11-17 | 2021-02-23 | 徐文忠 | Lithium battery car electrolyte additive |
| CN112397781B (en) * | 2020-11-17 | 2022-06-07 | 徐文忠 | Preparation method of vinylene carbonate additive for lithium battery car electrolyte |
| CN112436187A (en) * | 2020-11-24 | 2021-03-02 | 徐文忠 | Gel electrolyte for lithium battery |
| CN112436187B (en) * | 2020-11-24 | 2022-12-02 | 徐文忠 | Gel electrolyte for lithium battery |
| CN114749136A (en) * | 2022-04-14 | 2022-07-15 | 山东惟普新能源有限公司 | Tubular reactor and system device for continuously preparing vinylene carbonate |
| CN116003374A (en) * | 2022-12-16 | 2023-04-25 | 山东惟普新能源有限公司 | Method for synthesizing immediately separated vinylene carbonate |
| CN116003374B (en) * | 2022-12-16 | 2024-03-29 | 山东惟普新能源有限公司 | Method for synthesizing immediately separated vinylene carbonate |
| CN115716815A (en) * | 2022-12-22 | 2023-02-28 | 青岛科技大学 | Method and system for continuously preparing vinylene carbonate |
| CN115716815B (en) * | 2022-12-22 | 2024-03-29 | 青岛科技大学 | Method and system for continuously preparing vinylene carbonate |
Also Published As
| Publication number | Publication date |
|---|---|
| CN104744423B (en) | 2017-03-01 |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN104744423A (en) | Method for continuously producing vinylene carbonate | |
| CN102675093B (en) | A kind of process of n-butyl acetate synthesis | |
| Banchero et al. | Reactive distillation in the intensification of oleic acid esterification with methanol–A simulation case-study | |
| CN102875493A (en) | Method for preparing epoxidized fatty acid methyl esters in continuous flow microchannel reactor | |
| CN106414422A (en) | Apparatus and method for producing cyclic carbonate | |
| WO2017155441A1 (en) | Production equipment for production of caprolactone | |
| CN204661588U (en) | A kind of device of continuous prodution vinylene carbonate | |
| JP2012201684A (en) | Reactive distillation process and plant for obtaining acetic acid and alcohol from hydrolysis of methyl acetate | |
| He et al. | Two-stage continuous flow synthesis of epoxidized fatty acid methyl esters in a micro-flow system | |
| CN106397123B (en) | Method for producing dichloropropanol and method for producing epichlorohydrin | |
| CN105801408B (en) | A kind of reaction and rectification device producing high purity acrylic acid N-butyl and method | |
| CN106242970A (en) | A kind of Apparatus and method for producing dimethyl adipate | |
| CN108864178A (en) | A kind of synthesis tricresyl phosphate（2- chloropropyl）The micro- reaction method and device of ester | |
| CN207468571U (en) | The equipment that aliphatic acid is prepared by ester hydrolysis | |
| CN105777543A (en) | Chain-shaped carbonate ester preparing and dihydric alcohol coproduction method and technology system | |
| CN109305893B (en) | Synthesis method and synthesis device of 1, 2-difluoroethylene trifluoromethyl ether | |
| CN103288584B (en) | Reformed arene C 10the processing method of middle extraction high-purity beta-methylnaphthalene | |
| CN102600627B (en) | Cyclone-flash cloth-film-reboiling-type heat-pipe distiller | |
| CN106588958A (en) | Production system and method for continuously preparing alkynol di-Grignard reagent | |
| CN104447230A (en) | Method for preparing 4-methoxystyrene | |
| CN106397122B (en) | Method for preparing dichloropropanol and epichlorohydrin by using glycerol as raw material | |
| CN104693089B (en) | Continuous preparation process method of N-acetate pyrrolidone | |
| CN105968007A (en) | High-purity methyl acetate production process device and method | |
| CN113710640A (en) | Diester-based material production unit and diester-based material production system comprising same | |
| CN110204514A (en) | A kind of production technology of epoxidized vegetable oil |
Legal Events
| Date | Code | Title | Description |
|---|---|---|---|
| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| GR01 | Patent grant | ||
| GR01 | Patent grant |