CN1944392A - Process for preparing high purity dimethyl carbonate - Google Patents
Process for preparing high purity dimethyl carbonate Download PDFInfo
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- CN1944392A CN1944392A CN 200610140812 CN200610140812A CN1944392A CN 1944392 A CN1944392 A CN 1944392A CN 200610140812 CN200610140812 CN 200610140812 CN 200610140812 A CN200610140812 A CN 200610140812A CN 1944392 A CN1944392 A CN 1944392A
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- dimethyl carbonate
- methylcarbonate
- high purity
- preparing high
- purity
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Abstract
The present invention relates to process of fining dimethyl carbonate. The refining process includes the steps of cooling industrial level dimethyl carbonate product to its smelting point 4deg.c for dimethyl carbonate to crystallize, eliminating liquid after crystallization, and heating the crystallized solid to smelt and to obtain pure dimethyl carbonate product with purity higher than 99.99 %. The pure dimethyl carbonate product may be used directly in preparing solvent for lithium cell electrolyte.
Description
Technical field
The present invention relates to a kind of process for preparing high purity dimethyl carbonate.
Background technology
Methylcarbonate (English name Dimethyl carbonate), normal temperature is colourless transparent liquid, can mix with organic solvents such as alcohol, ketone, esters with arbitrary proportion, is slightly soluble in water, 4 ℃ of fusing points, 90.3 ℃ of boiling points, 18 ℃ of flash-points, density 1.069.It is very noticeable in recent years with stronger chemical property and hypotoxicity, be registered as in Europe in 1992 " non-toxic chemicals ", be known as " green chemical " in the world, be mainly used in synthetic intermediate and solvent, wherein high purity product is used to the lithium battery electrolytes solvent.
According to the methylcarbonate process for purification of present domestic and foreign literature report, mainly be by absorption and distillation or rectifying, or absorption, distillation or rectifying combination.In Chinese patent 01141439.1, to mention methylcarbonate with after the activated alumina drying, distillation can obtain purity greater than 99.99% methylcarbonate.
Summary of the invention
The purpose of this invention is to provide a kind of method by crystallisation by cooling purifying high-purity methylcarbonate.
Methylcarbonate is inflammable, explosive, volatile chemical, adopts the crystallisation by cooling process for purification can make the industrialization operation safe.Because the impurity in the methylcarbonate mainly is low carbon chain fatty alcohol, the inventive method can very effectively be removed.
The method of purifying high-purity methylcarbonate of the present invention is:
With the technical grade methylcarbonate, be cooled to 4 ℃ of methylcarbonate fusing points, it is solid that product begins crystallization, when the crystalline solid amount reaches a certain amount of, stop cooling, the liquid in the discharging solidliquid mixture, with the crystalline solid heat fused, obtain purity greater than 99.99% methylcarbonate.
Example 1:
In the enamel still of being furnished with stirring, thermometer, reflux exchanger, the methylcarbonate that adds 1000kg, purity 99.8%, moisture content 200ppm, open stirring, feed icy salt solution cooling 6 hours in chuck, temperature is 4 ℃, forms one deck xln on the still wall, after discharging clean liquid, feed hot water and be added to xln and melt fully in chuck, obtain the liquid product of 100kg fusing, purity is 99.993%, moisture content 30ppm.
Example 2:
The methylcarbonate of 3000kg, purity 99.8%, moisture content 200ppm is joined in the stainless steel tubular heat exchange of vertical placement, with icy salt solution cooling 6 hours, temperature is 4 ℃, form one deck xln on the tubulation surface, after discharging clean liquid, be added to xln with hot water and melt fully, obtain the liquid product of 2000kg fusing, purity is 99.991%, moisture content 30ppm.
Claims (1)
1, a kind of process for preparing high purity dimethyl carbonate, it is characterized in that: with the technical grade methylcarbonate, be cooled to 4 ℃ of methylcarbonate fusing points, it begins crystallization is solid, when the crystalline solid amount reaches a certain amount of, stop cooling, the liquid in the discharging solidliquid mixture, with the crystalline solid heat fused, obtain purity greater than 99.99% methylcarbonate.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610140812 CN1944392A (en) | 2006-10-11 | 2006-10-11 | Process for preparing high purity dimethyl carbonate |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 200610140812 CN1944392A (en) | 2006-10-11 | 2006-10-11 | Process for preparing high purity dimethyl carbonate |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN1944392A true CN1944392A (en) | 2007-04-11 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 200610140812 Pending CN1944392A (en) | 2006-10-11 | 2006-10-11 | Process for preparing high purity dimethyl carbonate |
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| CN (1) | CN1944392A (en) |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ITMI20091927A1 (en) * | 2009-11-04 | 2011-05-05 | Polimeri Europa Spa | PROCEDURE FOR THE PRODUCTION OF DIMETHYL CARBONATE WITH HIGH PURITY |
| CN105384639A (en) * | 2015-11-11 | 2016-03-09 | 东营市海科新源化工有限责任公司 | Refining purifying device and method used for continuously producing battery grade dimethyl carbonate |
| CN105399629A (en) * | 2015-11-27 | 2016-03-16 | 铜陵金泰化工股份有限公司 | Refining method and device for high-purity DMC (dimethyl carbonate) |
| CN107501096A (en) * | 2017-09-26 | 2017-12-22 | 天津科技大学 | Rectifying couples the method for preparing electron level dimethyl carbonate with crystallization |
| CN111704545A (en) * | 2020-08-24 | 2020-09-25 | 天津乐科节能科技有限公司 | Method for separating dimethyl carbonate methanol azeotrope by melt crystallization and application thereof |
-
2006
- 2006-10-11 CN CN 200610140812 patent/CN1944392A/en active Pending
Cited By (12)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| ITMI20091927A1 (en) * | 2009-11-04 | 2011-05-05 | Polimeri Europa Spa | PROCEDURE FOR THE PRODUCTION OF DIMETHYL CARBONATE WITH HIGH PURITY |
| WO2011055204A1 (en) | 2009-11-04 | 2011-05-12 | Polimeri Europa S.P.A. | Process for the production of high-purity dimethyl carbonate |
| CN102656136A (en) * | 2009-11-04 | 2012-09-05 | 维尔萨利斯股份公司 | Process for the production of high-purity dimethyl carbonate |
| CN102656136B (en) * | 2009-11-04 | 2014-08-13 | 维尔萨利斯股份公司 | Process for the production of high-purity dimethyl carbonate |
| RU2532266C2 (en) * | 2009-11-04 | 2014-11-10 | ВЕРСАЛИС С.п.А. | Method of obtaining highly pure dimethylcarbonate |
| TWI471304B (en) * | 2009-11-04 | 2015-02-01 | Polimeri Europa Spa | Process for the production of high-purity dimethyl carbonate |
| US9006476B2 (en) | 2009-11-04 | 2015-04-14 | Versalis S.P.A. | Process for the production of high-purity dimethyl carbonate |
| CN105384639A (en) * | 2015-11-11 | 2016-03-09 | 东营市海科新源化工有限责任公司 | Refining purifying device and method used for continuously producing battery grade dimethyl carbonate |
| CN105384639B (en) * | 2015-11-11 | 2017-07-14 | 东营市海科新源化工有限责任公司 | Refined purifying plant for continuously producing LITHIUM BATTERY dimethyl carbonate |
| CN105399629A (en) * | 2015-11-27 | 2016-03-16 | 铜陵金泰化工股份有限公司 | Refining method and device for high-purity DMC (dimethyl carbonate) |
| CN107501096A (en) * | 2017-09-26 | 2017-12-22 | 天津科技大学 | Rectifying couples the method for preparing electron level dimethyl carbonate with crystallization |
| CN111704545A (en) * | 2020-08-24 | 2020-09-25 | 天津乐科节能科技有限公司 | Method for separating dimethyl carbonate methanol azeotrope by melt crystallization and application thereof |
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Legal Events
| Date | Code | Title | Description |
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| C06 | Publication | ||
| PB01 | Publication | ||
| C10 | Entry into substantive examination | ||
| SE01 | Entry into force of request for substantive examination | ||
| C02 | Deemed withdrawal of patent application after publication (patent law 2001) | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Open date: 20070411 |