CN104327037A - Vinylene carbonate preparation method - Google Patents
Vinylene carbonate preparation method Download PDFInfo
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- CN104327037A CN104327037A CN201410546929.4A CN201410546929A CN104327037A CN 104327037 A CN104327037 A CN 104327037A CN 201410546929 A CN201410546929 A CN 201410546929A CN 104327037 A CN104327037 A CN 104327037A
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- 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
Abstract
The invention relates to a vinylene carbonate preparation method, which comprises the following steps: synthesizing monochloroethylene carbonate (C1EC), adding sulfonyl chloride drop by drop on ethylene carbonate (EC) under existence of an initiator azo, wherein mol ratio of sulfonyl chloride to EC is 1.1-1.2: 1, adding temperature is 55-80 DEG C, adding time is 5-6 hours, insulating for 1 hour, adding trialkylamine for 6-7 hours in a solution of dimethyl carbonate (DMC) and ClEC crude product according to weight ratio of 2.5-2.5: 1, wherein the addition temperature is 50-59 DEG C, insulating for 10-12 hours, wherein weight ratio of trialkylamine to ClEC is 1:1-1.1, and performing vacuum rectification and toluene recrystallization for purifiying VC. According to the invention, EC conversion rate can reach more than 94%, VC yield can reach 44%, and purity can reach more than 99.9%. The method has the advantages of simple process flow, mild technology condition, low reaction temperature and increased production security. In the invention, DMC is especially employed as solvent product which is easy to be separated.
Description
Technical field
The invention belongs to technical field of fine chemical synthesis, be specifically related to a kind of preparation method of vinylene carbonate.
Background technology
Vinylene carbonate (Vinylene carbonate, be called for short VC) be colourless transparent liquid, being a kind of organic synthesis intermediate, is lithium-ion battery electrolytes additive, obviously can extend the cycle life of lithium ion battery, be a kind of nonaqueous electrolytic solution solvent.Can also as top coat component or as the monomer applications preparing polymerized thylene carbonate vinyl acetate, wide market.
The main method of current production vinylene carbonate has following several: NSC 11801 and chlorine are light-initiated lower chloro Formed vinyl acetate (ClEC), use mineral alkali again: sodium hydroxide, potassium hydroxide, sodium carbonate, salt of wormwood, or organic bases: the dehydrochlorination such as DMA, triethylamine produces vinylene carbonate (VC).NSC 11801 under oil-soluble initiator Diisopropyl azodicarboxylate, 2,2'-Azobis(2,4-dimethylvaleronitrile), 2,2'-Azobis(2,4-dimethylvaleronitrile) etc. exist and sulfuryl chloride be obtained by reacting chlorocarbonic acid vinyl acetate (ClEC), then prepare vinylene carbonate (VC) with trialkylamine dehydrochlorination.NSC 11801 and sulfuryl chloride at light-initiated lower generation ClEC, then generate VC with alkali dehydrochlorination.Solvent made by ClEC toluene, and the de-HCl of high temperature (200 ~ 450 DEG C) generates VC.ClEC NSC 11801 (EC) makes solvent, and alkali exists lower de-HCl and generates VC.ClEC methylcarbonate (DMC) makes solvent, and organic bases exists lower de-HCl and generates VC.ClEC ethyl acetate makees solvent, takes off HCl generate VC with trialkylamine.Ethylene carbonate high-temperature dehydrogenation (oxidation) prepares VC.
The document that background technology is quoted from has: Changchun Inst. of Applied Chemistry, Chinese Academy of Sciences Chen Xuesi CN 1733756 (2006); Merck Patent GmbH Germany B matches not top grade people CN 1304935 (calendar year 2001); The little dragon of granary China one chemical science and technology stock company limited king waits people CN102351837A (2012); The quiet CN102532019A of Hubei De Zhou development in science and technology Co., Ltd. Zhang (2012N); Hongbo Chemical Co., Ltd., Zhejiang Kang Hong outstanding person waits people CN1858047 (2006); The people CN1958582A (2007) such as the first snowy peak of Biyadi Co Ltd; Shanxi Inst. of Coal Chemistry, Chinese Academy of Sciences grandson seldom waits people CN1817879 (2006); Guotai Huarong Chemical New Material Co., Ltd., Zhangjiagang City wears the people CN199360 (2005) such as ice dawn.
Above-mentioned prior art describes the method for synthesis VC separately, has all carried out useful experiment, and open thinking, has enriched the natural science treasure-house of fine chemistry industry, but also had deficiency separately.Its Patent CN 1733756 takes off HCl and uses ether to make solvent, and ether washes solid triethylamine hydrochloride, and ether flash-point is low also easily generates superoxide, and be inflammable and explosive substances, operational danger is large.Patent CN 1304935 takes off HCl and uses NSC 11801 (EC) to make solvent, VC and EC is not easily separated, is difficult to obtain highly purified VC.Not solubilizing agent when patent CN102351837A takes off HCl, in still-process, material dispersion difficulty is large, and material is heated not easily even, need adopt the special whipping appts of better performances.Patent CN102532019A is undeclared is the renovation process of strong basicity quarternary ammoniumion exchange resin by what model and resin.Patent CN1858047, chloro, with light-initiated, realize suitability for industrialized production, equipment more complicated, and technology difficulty is comparatively large, and de-HCl solvent for use, as the volatility such as acetone, isopropyl ether, benzene are comparatively large, easily causes atmospheric pollution.Patent CN1958582A takes off HCl alkali metal hydroxide used, the particle that its granularity is less than 3 microns.Its total amount will reach 50%, and extra-fine grinding will solve the problem of the very easily moisture absorption such as NaOH, LiOH, KOH, and equipment and process exists certain difficulty.Patent CN1817879 chlorination employs tetracol phenixin and makes solvent, adds the separating step of solvent, makes solvent again, increase the difficulty that EC with VC is separated, reduce the purity of VC during de-HCl by the NSC 11801 of fusing point up to 37 DEG C.Patent CN199360, adopts light chlorination, suitability for industrialized production, higher to equipment, processing requirement.
Summary of the invention
Technical problem to be solved by this invention overcomes above-mentioned the deficiencies in the prior art, there is provided a kind of processing and fabricating easy, technical process is simple, strong operability, processing condition are gentleer, temperature of reaction is lower, and production security is high, has the preparation method of the vinylene carbonate of environment friendly and practicality.
The technical scheme that the present invention solves the problems of the technologies described above employing is: a kind of preparation method of vinylene carbonate, it is characterized in that comprising the steps:
(1) monochloroethylene carbonate (ClEC) is synthesized: with NSC 11801 (EC) for raw material, azo is initiator, and SULPHURYL CHLORIDE is chlorizating agent; NSC 11801 (EC) is added in reactor, azo is added by oil-soluble initiator azo: EC=2-3:100 (weight ratio), be that 1.1-1.2:1 drips SULPHURYL CHLORIDE by the mol ratio of SULPHURYL CHLORIDE and EC, dropping temperature 55 ~ 80 DEG C, time for adding 5 ~ 6 h, be incubated 1 h again, vacuum purifies tail gas and obtains ClEC crude product;
(2) be added in reactor by solvent methylcarbonate (DMC) and ClEC crude product weight ratio 2.5-3.5:1, trialkylamine is dripped by the weight ratio 1-1.1:1 of trialkylamine and ClEC crude product, time for adding 6 ~ 7 h, dropping temperature 50 ~ 59 DEG C, insulation 10 ~ 12 h; Under methylcarbonate (DMC) exists, the ClEC crude product that step (1) obtains and trialkylamine generation bimolecular elimination reaction, dehydrochlorination, obtains the mixture containing vinylene carbonate (VC);
(3) mixture obtained in step (2) is obtained target product vinylene carbonate (VC) through precipitation, rectification under vacuum, recrystallization, again rectification under vacuum.
Further, described step (1) oil-soluble initiator azo is Diisopropyl azodicarboxylate (AIBN) or 2,2'-Azobis(2,4-dimethylvaleronitrile) (AMBN) or 2,2'-Azobis(2,4-dimethylvaleronitrile) (ABVN), the ABVN of preferred long half time, disposablely joins in reactor.
Further, the add-on of described 2,2'-Azobis(2,4-dimethylvaleronitrile) (ABVN) is ABVN:EC=2.5:100 (weight ratio).
Further, the mol ratio of described SULPHURYL CHLORIDE and EC is 1.15:1.
Further, the weight ratio of described solvent methylcarbonate (DMC) and ClEC crude product is 3:1.
Further, described trialkylamine is triethylamine, and the weight ratio of ClEC crude product and triethylamine is 1:1.
Further, stopper MEHQ is also added with when solvent methylcarbonate (DMC) and the mixing of ClEC crude product in described step (2).
Further, in described step (3), precipitation temperature is 35 ~ 45 DEG C, vacuum tightness-0.03 ~-0.06 MPa.
Further, in described step (3), rectification under vacuum is collected as the cut of 40 ~ 58 DEG C/4 ~ 7 mmHg.
Further, in described step (3), the solvent of recrystallization is toluene, VC: toluene=1:0.5-0.6 (w/v), solvent temperature 45 ~ 50 DEG C, Tc < 0 DEG C.
EC transformation efficiency of the present invention can reach 94 more than %, ClEC yield 78 %, VC yield 44 %, content 99.9 %.VC purity 99.9 more than %.Processing and fabricating of the present invention is easy, and technical process is simple, strong operability, and processing condition are gentleer, and temperature of reaction is lower, production security improves.Particularly adopt DMC to be easy to be separated as solvent product, there is very high practicality and good economic benefit and social benefit.
Accompanying drawing explanation
Fig. 1 is the preparation were established figure of vinylene carbonate of the present invention (VC).
Embodiment
Below in conjunction with embodiment, technical scheme of the present invention is described further.These embodiments are in order to the present invention instead of limitation of the present invention are described.
A preparation method for vinylene carbonate, it comprises the following steps:
(1) monochloroethylene carbonate (ClEC) is synthesized: with NSC 11801 (EC) for raw material, azo is initiator, SULPHURYL CHLORIDE is chlorizating agent, and radical substitution reaction occurs, obtained monochloroethylene carbonate (ClEC).
Principal reaction equation is:
Specifically: NSC 11801 (EC) is added in reactor, azo is added by oil-soluble initiator azo: EC=2-3:100 (weight ratio), be that 1.1-1.2:1 drips SULPHURYL CHLORIDE by the mol ratio of SULPHURYL CHLORIDE and EC, dropping temperature 55 ~ 80 DEG C, time for adding 5 ~ 6 h, be incubated 1 h again, vacuum purifies tail gas and obtains ClEC crude product.
(2) under methylcarbonate (DMC) exists, the ClEC crude product that step (1) is obtained and trialkylamine generation bimolecular elimination reaction (E-2 reaction mechanism), dehydrochlorination, generates vinylene carbonate (VC).
Principal reaction equation is:
Specifically: be added in reactor by solvent methylcarbonate (DMC) and ClEC crude product weight ratio 2.5-3.5:1, trialkylamine is dripped by the weight ratio 1-1.1:1 of trialkylamine and ClEC crude product, time for adding 6 ~ 7 h, dropping temperature 50 ~ 59 DEG C, insulation 10 ~ 12 h, obtain the mixture containing vinylene carbonate (VC).
(3) by the mixture obtained in step (2) through filter press except solids filtrate precipitation, rectification under vacuum, recrystallization, again rectification under vacuum obtain target product vinylene carbonate (VC).
Further, described step (1) oil-soluble initiator azo is Diisopropyl azodicarboxylate (AIBN) or 2,2'-Azobis(2,4-dimethylvaleronitrile) (AMBN) or 2,2'-Azobis(2,4-dimethylvaleronitrile) (ABVN), the ABVN of preferred long half time, disposablely joins in reactor.
Further, the add-on of described 2,2'-Azobis(2,4-dimethylvaleronitrile) (ABVN) is ABVN:EC=2.5:100 (weight ratio).
Further, the mol ratio of described SULPHURYL CHLORIDE and EC is 1.15:1.
Further, the weight ratio of described solvent methylcarbonate (DMC) and ClEC crude product is 3:1.
Further, described trialkylamine is triethylamine, and the weight ratio of ClEC crude product and triethylamine is 1:1.
Further, stopper MEHQ is also added with when solvent methylcarbonate (DMC) and the mixing of ClEC crude product in described step (2).
Further, in described step (3), precipitation temperature is 35 ~ 45 DEG C, vacuum tightness-0.03 ~-0.06 MPa.
Further, in described step (3), rectification under vacuum is collected as the cut of 40 ~ 58 DEG C/4 ~ 7 mmHg.
Further, in described step (3), the solvent of recrystallization is toluene, VC: toluene=1:0.5-0.6 (w/v), solvent temperature 45 ~ 50 DEG C, Tc < 0 DEG C.
EC transformation efficiency of the present invention can reach 94 more than %, ClEC yield 78 %, VC yield 44 %, content 99.9 %.VC purity 99.9 more than %.Processing and fabricating of the present invention is easy, and technical process is simple, and strong operability, processing condition are gentleer, have environment friendly and practicality.
Embodiment 1: by step shown in Fig. 1: (1) adds NSC 11801 (EC) 500 kg (5.68 kmol) to chloro still, be warmed up to 70 ~ 80 DEG C and add Diisopropyl azodicarboxylate (AIBN) 13 kg (2.6% of EC amount), and at 70 ~ 80 DEG C, drip sulfuryl chloride 843 kg (6.25 kmol) in 4.5 ~ 6 h and add AIBN1.3 kg/ time every 30 min simultaneously, add 10 AIBN altogether, after SULPHURYL CHLORIDE drips off, 70 ~ 80 DEG C of insulation 1 h, vacuum purifies tail gas, and cooling obtains monochloroethylene carbonate crude product 668 kg (being roughly equal to 5.45 kmol).By EC to ClEC transformation efficiency 91 %.(2) step (1) gained ClEC crude product 668 kg, methylcarbonate 2000 kg, stopper MEHQ 3.3 kg is added to dehydrochlorination still.Be warmed up to 55 ~ 59 DEG C, drip triethylamine 668 kg (6.6 kmol) in 5 ~ 8 h, drip off insulation 12 h.Obtain the mixture containing vinylene carbonate (VC).(3) mixture obtained in step (2) is removed solids through filter press, filtrate obtains target product vinylene carbonate (VC) through precipitation, rectification under vacuum, recrystallization, again rectification under vacuum.Precipitation temperature is 35 ~ 45 DEG C, vacuum tightness-0.03 ~-0.06 MPa.Rectification under vacuum is collected as the cut of 40 ~ 58 DEG C/4 ~ 7 mmHg.The solvent of recrystallization is toluene, VC: toluene=1:0.5-0.6 (w/v), solvent temperature 45 ~ 50 DEG C, Tc < 0 DEG C.Finally purify and obtain NSC 11801 (VC) 195 kg.Purity 99.9 %, by total recovery 40 % of EC to VC.The stablizer 2,6 di tert butyl 4 methyl phenol (BHT) of output 0.5 % is added with in finished product.
Embodiment 2: shown in Fig. 1: step (1) adds after NSC 11801 (EC) 500 kg (5.68 kmol) is warmed up to 55 ~ 60 DEG C to chlorination tank, disposablely add 2,2'-Azobis(2,4-dimethylvaleronitrile) (ABVN) 12.5 kg, and at 55 ~ 60 DEG C, sulfuryl chloride 882 kg (6.53kmol) is dripped in 4 ~ 5 h, after dripping off, 55 ~ 60 DEG C of insulation 1 h, vacuum purifies tail gas, and cooling obtains monochloroethylene carbonate (ClEC) crude product 675 kg (being roughly equal to 5.51 kmol).By EC to ClEC transformation efficiency 96.3 %.GC analyzes in crude product containing EC 3.7 %, ClEC 87.3 %, dichloro-NSC 11801 Cl
2eC 6.3 %, non-recognizate 2.7 %.Step (2) adds step (1) gained ClEC crude product 675 kg in dehydrochlorination still, adds methylcarbonate 2025 kg, stopper MEHQ 3.4 kg.In 5 ~ 8 h, drip triethylamine 675 kg (6.68 kmol), after dripping off insulation 12 h, obtain the mixture containing vinylene carbonate (VC).The mixture obtained in step (2) is removed solids through filter press by step (3), and filtrate precipitation, rectification under vacuum, recrystallization, again rectification under vacuum obtain target product vinylene carbonate (VC).Precipitation temperature is 35 ~ 45 DEG C, vacuum tightness-0.03 ~-0.06 MPa.Rectification under vacuum is collected as the cut of 40 ~ 58 DEG C/4 ~ 7 mmHg.The solvent of recrystallization is toluene, VC: toluene=1:0.5-0.6 (w/v), solvent temperature 45 ~ 50 DEG C, Tc < 0 DEG C.Finally obtain NSC 11801 (VC) 216 kg, purity 99.5 % is by total recovery 44.2 % of EC to VC.The stablizer 2,6 di tert butyl 4 methyl phenol (BHT) of output 0.5 % is added with in finished product.
Present invention process is simple, mild condition, temperature of reaction are lower, production security improves, adopt DMC to be easy to be separated as solvent product, has very high practicality and good economic benefit and social benefit.
Claims (10)
1. a preparation method for vinylene carbonate, is characterized in that comprising the steps:
(1) monochloroethylene carbonate (ClEC) is synthesized: with NSC 11801 (EC) for raw material, azo is initiator, and SULPHURYL CHLORIDE is chlorizating agent; NSC 11801 (EC) is added in reactor, azo is added by oil-soluble initiator azo: EC=2-3:100 (weight ratio), be that 1.1-1.2:1 drips SULPHURYL CHLORIDE by the mol ratio of SULPHURYL CHLORIDE and EC, dropping temperature 55 ~ 80 DEG C, time for adding 5 ~ 6 h, be incubated 1 h again, vacuum purifies tail gas and obtains ClEC crude product;
(2) be added in reactor by solvent methylcarbonate (DMC) and ClEC crude product weight ratio 2.5-3.5:1, trialkylamine is dripped by the weight ratio 1-1.1:1 of trialkylamine and ClEC crude product, time for adding 6 ~ 7 h, dropping temperature 50 ~ 59 DEG C, insulation 10 ~ 12 h; Under methylcarbonate (DMC) exists, the ClEC crude product that step (1) obtains and trialkylamine generation bimolecular elimination reaction, dehydrochlorination, obtains the mixture containing vinylene carbonate (VC);
(3) mixture obtained in step (2) is obtained target product vinylene carbonate (VC) through precipitation, rectification under vacuum, recrystallization, again rectification under vacuum.
2. the preparation method of vinylene carbonate according to claim 1, it is characterized in that: described step (1) oil-soluble initiator azo is Diisopropyl azodicarboxylate (AIBN) or 2,2'-Azobis(2,4-dimethylvaleronitrile) (AMBN) or 2,2'-Azobis(2,4-dimethylvaleronitrile) (ABVN), disposablely to join in reactor.
3. the preparation method of vinylene carbonate according to claim 2, is characterized in that: the add-on of described 2,2'-Azobis(2,4-dimethylvaleronitrile) (ABVN) is ABVN:EC=2.5:100 (weight ratio).
4. the preparation method of vinylene carbonate according to claim 1, is characterized in that: the mol ratio of described SULPHURYL CHLORIDE and EC is 1.15:1.
5. the preparation method of vinylene carbonate according to claim 1, is characterized in that: the weight ratio of described solvent methylcarbonate (DMC) and ClEC crude product is 3:1.
6. the preparation method of vinylene carbonate according to claim 1, is characterized in that: described trialkylamine is triethylamine, and the weight ratio of ClEC crude product and triethylamine is 1:1.
7. the preparation method of vinylene carbonate according to claim 1, is characterized in that: be also added with stopper MEHQ when solvent methylcarbonate (DMC) and the mixing of ClEC crude product in described step (2).
8. the preparation method of vinylene carbonate according to claim 1, is characterized in that: in described step (3), precipitation temperature is 35 ~ 45 DEG C, vacuum tightness-0.03 ~-0.06 MPa.
9. the preparation method of vinylene carbonate according to claim 1, is characterized in that: in described step (3), rectification under vacuum is collected as the cut of 40 ~ 58 DEG C/4 ~ 7 mmHg.
10. the preparation method of vinylene carbonate according to claim 1, it is characterized in that: in described step (3), the solvent of recrystallization is toluene, VC: toluene=1:0.5-0.6 (w/v), solvent temperature 45 ~ 50 DEG C, Tc < 0 DEG C.
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Cited By (19)
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|---|---|---|---|---|
| CN104744423A (en) * | 2015-03-17 | 2015-07-01 | 沈阳化工大学 | Method for continuously producing vinylene carbonate |
| CN104844556A (en) * | 2015-04-30 | 2015-08-19 | 荣成青木高新材料股份有限公司 | Method for continuously preparing vinylene carbonate by tubular reactor |
| CN105384719A (en) * | 2015-12-14 | 2016-03-09 | 苏州华一新能源科技有限公司 | Vinylene carbonate purification method |
| CN105503812A (en) * | 2015-12-28 | 2016-04-20 | 苏州华一新能源科技有限公司 | Continuous production method for high-purity vinylene carbonate |
| CN105541782A (en) * | 2015-12-18 | 2016-05-04 | 苏州华一新能源科技有限公司 | Vinylene carbonate purifying method |
| CN106588862A (en) * | 2016-12-05 | 2017-04-26 | 东营市海科新源化工有限责任公司 | Ethylene carbonate purification process and purification system |
| CN106632225A (en) * | 2016-12-27 | 2017-05-10 | 苏州华新能源科技有限公司 | Method for preparing high-purity vinylene carbonate |
| CN106749155A (en) * | 2017-01-06 | 2017-05-31 | 淮安瀚康新材料有限公司 | A kind of method that microchannel plate should prepare vinylene carbonate |
| CN109107503A (en) * | 2018-09-19 | 2019-01-01 | 长园华盛(泰兴)锂电材料有限公司 | Tandem reaction equipment of vinylene carbonate and preparation method thereof |
| CN112266373A (en) * | 2020-11-24 | 2021-01-26 | 泰兴华盛精细化工有限公司 | Method for purifying vinylene carbonate |
| CN113620924A (en) * | 2021-08-30 | 2021-11-09 | 泰兴华盛精细化工有限公司 | Rapid continuous flow synthesis process of fluoroethylene carbonate |
| CN113816937A (en) * | 2021-11-23 | 2021-12-21 | 山东海科创新研究院有限公司 | Method for preparing vinylene carbonate |
| CN113999199A (en) * | 2021-12-04 | 2022-02-01 | 青岛科技大学 | Vinylene carbonate synthesis method |
| CN114230549A (en) * | 2021-11-24 | 2022-03-25 | 青岛科技大学 | Synthetic method of fluoroethylene carbonate |
| CN114539203A (en) * | 2022-03-10 | 2022-05-27 | 李科 | Low-cost vinylene carbonate synthesis method |
| CN114874179A (en) * | 2022-06-14 | 2022-08-09 | 华东理工大学 | Method for continuously synthesizing vinylene carbonate or/and fluoroethylene carbonate through micro-channel |
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Cited By (20)
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| CN104744423A (en) * | 2015-03-17 | 2015-07-01 | 沈阳化工大学 | Method for continuously producing vinylene carbonate |
| CN104844556A (en) * | 2015-04-30 | 2015-08-19 | 荣成青木高新材料股份有限公司 | Method for continuously preparing vinylene carbonate by tubular reactor |
| CN105384719A (en) * | 2015-12-14 | 2016-03-09 | 苏州华一新能源科技有限公司 | Vinylene carbonate purification method |
| CN105541782A (en) * | 2015-12-18 | 2016-05-04 | 苏州华一新能源科技有限公司 | Vinylene carbonate purifying method |
| CN105503812A (en) * | 2015-12-28 | 2016-04-20 | 苏州华一新能源科技有限公司 | Continuous production method for high-purity vinylene carbonate |
| CN106588862A (en) * | 2016-12-05 | 2017-04-26 | 东营市海科新源化工有限责任公司 | Ethylene carbonate purification process and purification system |
| CN106632225A (en) * | 2016-12-27 | 2017-05-10 | 苏州华新能源科技有限公司 | Method for preparing high-purity vinylene carbonate |
| CN106632225B (en) * | 2016-12-27 | 2018-06-26 | 苏州华一新能源科技有限公司 | A kind of preparation method of high-purity vinylene carbonate |
| CN106749155A (en) * | 2017-01-06 | 2017-05-31 | 淮安瀚康新材料有限公司 | A kind of method that microchannel plate should prepare vinylene carbonate |
| CN109107503A (en) * | 2018-09-19 | 2019-01-01 | 长园华盛(泰兴)锂电材料有限公司 | Tandem reaction equipment of vinylene carbonate and preparation method thereof |
| CN112266373A (en) * | 2020-11-24 | 2021-01-26 | 泰兴华盛精细化工有限公司 | Method for purifying vinylene carbonate |
| CN113620924A (en) * | 2021-08-30 | 2021-11-09 | 泰兴华盛精细化工有限公司 | Rapid continuous flow synthesis process of fluoroethylene carbonate |
| CN113816937A (en) * | 2021-11-23 | 2021-12-21 | 山东海科创新研究院有限公司 | Method for preparing vinylene carbonate |
| CN114230549A (en) * | 2021-11-24 | 2022-03-25 | 青岛科技大学 | Synthetic method of fluoroethylene carbonate |
| CN113999199A (en) * | 2021-12-04 | 2022-02-01 | 青岛科技大学 | Vinylene carbonate synthesis method |
| CN114539203A (en) * | 2022-03-10 | 2022-05-27 | 李科 | Low-cost vinylene carbonate synthesis method |
| CN114957193A (en) * | 2022-05-11 | 2022-08-30 | 内蒙古源宏精细化工有限公司 | Method for green synthesis of vinylene carbonate |
| CN114874179A (en) * | 2022-06-14 | 2022-08-09 | 华东理工大学 | Method for continuously synthesizing vinylene carbonate or/and fluoroethylene carbonate through micro-channel |
| CN115073414A (en) * | 2022-06-22 | 2022-09-20 | 浙江天硕氟硅新材料科技有限公司 | Synthesis method of high-purity vinylene carbonate |
| CN115232100A (en) * | 2022-09-21 | 2022-10-25 | 湖南省正源储能材料与器件研究所 | Method for recovering solvent in vinylene carbonate rectification process |
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