CN101717390A - Purifying process of difluoroethylene carbonate - Google Patents
Purifying process of difluoroethylene carbonate Download PDFInfo
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- CN101717390A CN101717390A CN200910213451A CN200910213451A CN101717390A CN 101717390 A CN101717390 A CN 101717390A CN 200910213451 A CN200910213451 A CN 200910213451A CN 200910213451 A CN200910213451 A CN 200910213451A CN 101717390 A CN101717390 A CN 101717390A
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- difluoroethylene carbonate
- carbonate
- difluoroethylene
- organic solvent
- pyrrolidone
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Abstract
The invention discloses a purifying process of difluoroethylene carbonate, which has the advantages of simple processes, easy operation, low unit consumption and high yield. The purifying process is characterized by comprising the following steps: adding an organic solvent and pyrrolidone into a crude product containing 10%-60% by weight of difluoroethylene carbonate, wherein the adding amount of the organic solvent is 5%-30% by weight of the crude product containing the difluoroethylene carbonate, and the adding amount of the pyrrolidone is 2%-10% by weight of the crude product containing the difluoroethylene carbonate; then, carrying out reduced pressure distillation, first distilling and collecting solvent fractions at 20-70 DEG C/1-60KPa; and then, distilling and collecting main fractions containing the difluoroethylene carbonate at 70-120 DEG C/70-100KPa. The invention can be used for purifying the difluoroethylene carbonate.
Description
Technical field
The present invention relates to a kind of purifying technique of difluoroethylene carbonate.
Background technology
Difluoroethylene carbonate is mainly used in the lithium-ion electrolyte of high power lithium battery, can effectively improve the lower temperature resistance of lithium cell, and the flame retardant resistance of raising lithium cell etc.But contain more by product in the product of traditional difluoroethylene carbonate production technique gained: as fluorinated ethylene carbonate, vinylene carbonate and a large amount of hydrofluoric acid, polymerization and decomposition easily take place in product under strong acidic condition, and the purification of product is caused very big difficulty.In the prior art, purify, but there are problems such as unstable product quality, unit consumption height, yield are low in this technology, production cost are increased greatly and environment produced and pollute by adopting the rectifying absorbing process.
Summary of the invention
Technical problem to be solved by this invention is: the purifying technique that the simple to operation and difluoroethylene carbonate that unit consumption is low, yield is high of a kind of technology will be provided.
For solving the problems of the technologies described above, the technical solution used in the present invention is: the purifying technique of described difluoroethylene carbonate, be characterized in: in containing the crude product that weight part is 10%～60% difluoroethylene carbonate, add organic solvent and pyrrolidone, wherein the add-on of organic solvent is 5%～30% weight part of difluoroethylene carbonate crude product, and the add-on of pyrrolidone is 2%～10% weight part of difluoroethylene carbonate crude product; Then carry out underpressure distillation, the cut that 20～70 ℃/1～60KPa is rich in organic solvent is collected in distillation earlier, and then the main distillate fraction that 70～120 ℃/70～100Kpa is rich in difluoroethylene carbonate is collected in distillation.
Among the present invention, the main distillate fraction that is rich in difluoroethylene carbonate that obtains can be proceeded rectification under vacuum, obtain the electronic-grade difluoroethylene carbonate.The temperature range of rectification under vacuum is 40～110 ℃, and vacuum ranges is 80～100KPa.
Among the present invention, the bed material reusable edible that is rich in pyrrolidone that is left after the underpressure distillation.
Organic solvent recited above is that specific inductivity is 2.0～4.0 solvent.Described organic solvent is selected from least a in the following material: methylcarbonate, diethyl carbonate, dipropyl carbonate, carbonic acid methylethyl ester, methylpropyl carbonate, ethylpropyl carbonate, acetone, acetonitrile, toluene, hexanaphthene, normal hexane.
Above-mentioned pyrrolidone has following structural formula:
In the formula, R is CH
3, CH
2CH
3Or CH=CH
2
The invention has the beneficial effects as follows: described method of purification is simply effective, and is easy to operate, constant product quality, and unit consumption is low, yield is high.
Embodiment
Following the present invention will be described in further detail in conjunction with specific embodiments, make advantage of the present invention more obvious.Should be appreciated that content wherein is just with explaining, and absolutely not protection scope of the present invention is construed as limiting.
Embodiment 1
Get content and be 10% difluoroethylene carbonate 5000g, to wherein adding 1500g methylcarbonate and 250gN-methyl-2-pyrrolidone, underpressure distillation, collect cut 3352g under 20～70 ℃/1～20KPa, with gas chromatograph (GC-2014, available from Shimadzu company) this cut is analyzed, containing difluoroethylene carbonate is 0.2%.Continue to collect cut 836g under 70～120 ℃/70～100KPa, analyzing difluoroethylene carbonate content with gas chromatograph (GC-2014 is available from Shimadzu company) is 53.8%, and residue raffinate 1812g contains difluoroethylene carbonate 1.65%.
With the rectifying of above-mentioned 836g fraction second depressurized, collect cut 430g under 80～100 ℃/90～100KPa, stratographic analysis difluoroethylene carbonate content is 98%, yield 93.6%.
The bed material reusable edible that is rich in pyrrolidone that is left after the underpressure distillation.
Embodiment 2
Get content and be 48% difluoroethylene carbonate 2000g, to wherein adding 100g carbonic acid methylethyl ester and 40gN-ethyl pyrrolidone, underpressure distillation, collect cut 560g under 20～60 ℃/20～60KPa, with gas chromatograph (GC-2014, available from Shimadzu company) this cut is analyzed, containing difluoroethylene carbonate is 3.6%.Continue to collect cut 1030g under 80～110 ℃/70～100KPa, analyzing difluoroethylene carbonate content with gas chromatograph (GC-2014 is available from Shimadzu company) is 86.9%, and residue raffinate 430g contains difluoroethylene carbonate 4.6%.
With the rectifying of above-mentioned 1030g fraction second depressurized, collect cut 856g under 80～100 ℃/90～100KPa, stratographic analysis difluoroethylene carbonate content is 98.5%, yield 92.1%.
Embodiment 3
Get content and be 60% difluoroethylene carbonate 1500g, to wherein adding 300g hexanaphthene and 150gN-vinyl pyrrolidone, underpressure distillation, collect cut 638g under 30～60 ℃/20～60KPa, with gas chromatograph (GC-2014, available from Shimadzu company) this cut is analyzed, containing difluoroethylene carbonate is 4.2%.Continue to collect cut 850g under 80～110 ℃/80～100KPa, analyzing difluoroethylene carbonate content with gas chromatograph (GC-2014 is available from Shimadzu company) is 89%, and residue raffinate 450g contains difluoroethylene carbonate 5.8%.
With the rectifying of above-mentioned 850g fraction second depressurized, collect cut 724g under 80～100 ℃/90～100KPa, stratographic analysis difluoroethylene carbonate content is 98.3%, yield 94%.
Claims (7)
1. the purifying technique of difluoroethylene carbonate, it is characterized in that: in containing the crude product that weight part is 10%～60% difluoroethylene carbonate, add organic solvent and pyrrolidone, wherein the add-on of organic solvent is 5%～30% weight part of difluoroethylene carbonate crude product, and the add-on of pyrrolidone is 2%～10% weight part of difluoroethylene carbonate crude product; Then carry out underpressure distillation, the cut that 20～70 ℃/1～60KPa is rich in organic solvent is collected in distillation earlier, and then the main distillate fraction that 70～120 ℃/70～100Kpa is rich in difluoroethylene carbonate is collected in distillation.
2. the purifying technique of difluoroethylene carbonate according to claim 1, it is characterized in that: the main distillate fraction that is rich in difluoroethylene carbonate that will obtain is proceeded rectification under vacuum, obtains the electronic-grade difluoroethylene carbonate.
3. the purifying technique of difluoroethylene carbonate according to claim 1 is characterized in that: the bed material reusable edible that is rich in pyrrolidone that is left after the underpressure distillation.
4. the purifying technique of difluoroethylene carbonate according to claim 1 and 2, it is characterized in that: described organic solvent is that specific inductivity is 2.0～4.0 solvent.
5. the purifying technique of difluoroethylene carbonate according to claim 4 is characterized in that: described organic solvent is selected from least a in the following material: methylcarbonate, diethyl carbonate, dipropyl carbonate, carbonic acid methylethyl ester, methylpropyl carbonate, ethylpropyl carbonate, acetone, acetonitrile, toluene, hexanaphthene, normal hexane.
6. the purifying technique of difluoroethylene carbonate according to claim 1 and 2, it is characterized in that: described pyrrolidone has following structural formula:
In the formula, R is CH
3, CH
2CH
3Or CH=CH
2
7. the purifying technique of difluoroethylene carbonate according to claim 2, it is characterized in that: the temperature range of rectification under vacuum is 40～110 ℃, and vacuum ranges is 80～100KPa.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910213451A CN101717390A (en) | 2009-10-29 | 2009-10-29 | Purifying process of difluoroethylene carbonate |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN200910213451A CN101717390A (en) | 2009-10-29 | 2009-10-29 | Purifying process of difluoroethylene carbonate |
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| CN101717390A true CN101717390A (en) | 2010-06-02 |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102887883A (en) * | 2012-09-26 | 2013-01-23 | 中国海洋石油总公司 | Continuous purifying method of crude product of fluoroethylene carbonate |
| CN106905290A (en) * | 2017-03-08 | 2017-06-30 | 江苏理文化工有限公司 | A kind of preparation method of difluoroethylene carbonate |
| CN106905289A (en) * | 2017-04-14 | 2017-06-30 | 南通新宙邦电子材料有限公司 | A kind of method of purification of vinylene carbonate |
| CN108160039A (en) * | 2017-11-23 | 2018-06-15 | 孝感市锐思新材科技有限公司 | A kind of preparation method of fluorinated ethylene carbonate purification material |
-
2009
- 2009-10-29 CN CN200910213451A patent/CN101717390A/en active Pending
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102887883A (en) * | 2012-09-26 | 2013-01-23 | 中国海洋石油总公司 | Continuous purifying method of crude product of fluoroethylene carbonate |
| CN106905290A (en) * | 2017-03-08 | 2017-06-30 | 江苏理文化工有限公司 | A kind of preparation method of difluoroethylene carbonate |
| CN106905290B (en) * | 2017-03-08 | 2019-06-07 | 江苏理文化工有限公司 | A kind of preparation method of difluoroethylene carbonate |
| CN106905289A (en) * | 2017-04-14 | 2017-06-30 | 南通新宙邦电子材料有限公司 | A kind of method of purification of vinylene carbonate |
| CN106905289B (en) * | 2017-04-14 | 2019-03-22 | 南通新宙邦电子材料有限公司 | A kind of method of purification of vinylene carbonate |
| CN108160039A (en) * | 2017-11-23 | 2018-06-15 | 孝感市锐思新材科技有限公司 | A kind of preparation method of fluorinated ethylene carbonate purification material |
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Address after: No. 28, Qinghai Road, Jiangsu International Chemical Industry Park, Yangtze River Applicant after: Jiangsu Huasheng Chemicals Co., Ltd. Address before: Gold town after Cheng Gaoqiao village 215631 Jiangsu city of Zhangjiagang Province Applicant before: Zhangjiagang Huasheng Chemistry Co., Ltd. |
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Application publication date: 20100602 |