CN100567259C - A kind of method for preparing glycol sulfite - Google Patents
A kind of method for preparing glycol sulfite Download PDFInfo
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- CN100567259C CN100567259C CNB2005100069084A CN200510006908A CN100567259C CN 100567259 C CN100567259 C CN 100567259C CN B2005100069084 A CNB2005100069084 A CN B2005100069084A CN 200510006908 A CN200510006908 A CN 200510006908A CN 100567259 C CN100567259 C CN 100567259C
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- glycol sulfite
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Abstract
A kind of method for preparing glycol sulfite relates to the field of chemical synthesis.Present method is a raw material with dimethyl sulfite and ethylene glycol, is catalyzer with the tosic acid, and wherein the ratio to dimethyl sulfite and ethylene glycol does not have special stipulation, and they can reaction with same mole, also reaction with same mole not; And catalyst consumption is 0.01%～5% of a reactant weight.In reaction process, progressively be warming up to 160～180 ℃ from 60～70 ℃, constantly remove the methyl alcohol that generates in the reaction process simultaneously, reaction is tending towards fully, the method for purifying by fractionation obtains glycol sulfite at last.This method has safe, yield height, the purity advantages of higher of equipment not had the burn into product simple to operate.
Description
Technical field
The present invention relates to the field of chemical synthesis, particularly relate to a kind of preparation method of glycol sulfite.
Background technology
Glycol sulfite is a kind of organic synthesis raw material, and can be used as electrolytical solvent of lithium secondary battery or additive.At present, the method for production glycol sulfite mainly contains following several:
(1) method with oxyethane and sulfurous gas reaction prepares glycol sulfite, and this method security is relatively poor, and is very high to equipment and operational requirement;
(2) method of spent glycol and sulfur oxychloride reaction prepares glycol sulfite, though this method cost is low, sulfur oxychloride toxicity is big, and reaction generates a large amount of sour gas, the aftertreatment difficulty of purifying, and the content of impurity such as chloroethanol is very high usually;
(3) method with the depolymerization of polyoxyethylene glycol sulfite prepares glycol sulfite, and this method is not too practical;
(4) method of spent glycol and dimethyl sulfite reaction prepares glycol sulfite, if this method does not have the existence of catalyzer, though also can carry out, the reaction times needs very long, and reaction to carry out ground very not thorough.
The glycol sulfite that above method is produced contains a large amount of impurity.And this glycol sulfite is not suitable for as electrolytical solvent of lithium secondary battery or additive, and they can influence electrolytical stability in storage.
Summary of the invention
Purpose of the present invention just is to disclose a kind of under the situation that catalyzer exists, and ethylene glycol and dimethyl sulfite carry out the method that transesterification reaction is produced glycol sulfite, thereby improves the purity of glycol sulfite, has also improved the performance of battery.
Concrete technical scheme of the present invention is: when ethylene glycol and dimethyl sulfite carry out transesterification reaction, be catalyzer with the tosic acid, its consumption is 0.01%～5% of a reactant weight, and preferred value is 0.1%～1%; And the ratio of ethylene glycol and dimethyl sulfite is not had special stipulation, they can reaction with same mole, also reaction with same mole not.
In reaction process, adopt the temperature that improves reaction step by step, when 60～70 ℃ of beginning to react rise to reaction and finish 160～180 ℃ are constantly removed the methyl alcohol that reaction generates simultaneously, make reaction be tending towards complete.
The glycol sulfite crude product that adopts the inventive method to produce is because the content of impurity is less, at last as long as can obtain the product of required purity with the fractionation method of purification.
Compared with prior art, the present invention has the following advantages: (1) materials safety, reacting balance, that equipment is not had burn into is easy and simple to handle; (2) catalyzer is a solid matter, and stable in properties, does not decompose, and can recycle; (3) particularly there are not the chloride impurity that lithium cell is had a significant impact in reaction yield height, product purity height.
Embodiment
Embodiment 1:
In 2000 milliliters of there-necked flasks that agitator, fractional column, thermometer are housed, add 1100g (10mol) dimethyl sulfite and 620g (10mol) ethylene glycol, and the 8.6g tosic acid, be heated to 70 ℃ and begin reaction, by fractionated method, constantly remove the methyl alcohol that reaction generates, in reaction process, improve the temperature of reaction step by step, when the temperature of reaction system reaches more than 170 ℃, and when no longer including methyl alcohol and steaming, show that reaction carried out fully.The product that last fractionation is purified and obtained extracts 172-173 ℃ cut, is the product glycol sulfite.Output 970g, purity 99% (HPLC).
Embodiment 2:
In 2000 milliliters of there-necked flasks that agitator, fractionation plant, thermometer are housed, add 1100 (10mol) dimethyl sulfites and 682g (11mol) ethylene glycol, and the 7.5g tosic acid, reaction system is heated to 70 ℃ and begins reaction, by fractionated method, constantly remove the methyl alcohol that reaction generates, in reaction process, improve the temperature of reaction step by step, when the temperature of reaction system reaches more than 170 ℃, and when no longer including methyl alcohol and steaming, show that reaction carried out fully.The product that last fractionation is purified and obtained extracts 172-173 ℃ cut, is the product glycol sulfite.Output 965g, purity 99% (HPLC).
Claims (2)
1. method for preparing glycol sulfite, it is characterized in that: this method is a raw material with dimethyl sulfite and ethylene glycol, is catalyzer with the tosic acid, catalyst consumption is 0.01%～5% of a reactant weight; In reaction process, progressively be warming up to 160～180 ℃ from 60～70 ℃, constantly remove the methyl alcohol that generates in the reaction process simultaneously; And the further fractionation purification of warp obtains glycol sulfite.
2. the method for preparing glycol sulfite as claimed in claim 1 is characterized in that: described catalyst consumption is 0.1%～1% of a reactant weight.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100069084A CN100567259C (en) | 2005-01-12 | 2005-01-12 | A kind of method for preparing glycol sulfite |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100069084A CN100567259C (en) | 2005-01-12 | 2005-01-12 | A kind of method for preparing glycol sulfite |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1803767A CN1803767A (en) | 2006-07-19 |
| CN100567259C true CN100567259C (en) | 2009-12-09 |
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
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| CNB2005100069084A Active CN100567259C (en) | 2005-01-12 | 2005-01-12 | A kind of method for preparing glycol sulfite |
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| CN (1) | CN100567259C (en) |
Families Citing this family (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN103030626A (en) * | 2011-10-10 | 2013-04-10 | 中国科学院福建物质结构研究所 | Method for synthesizing ethylene-base glycol sulfite |
| CN107987052A (en) * | 2017-12-22 | 2018-05-04 | 辽宁科隆精细化工股份有限公司 | A kind of synthetic method of ethylene sulfite derivative |
| CN108675984A (en) * | 2018-06-22 | 2018-10-19 | 江苏阿尔法药业有限公司 | The preparation method of Suo Feibuwei intermediates |
| CN112574168B (en) * | 2020-12-21 | 2022-08-09 | 上海如鲲新材料股份有限公司 | Preparation method of ethylene-based ethylene sulfite |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6423861B1 (en) * | 1999-02-03 | 2002-07-23 | Basf Aktiengesellschaft | Method of producing dimethyl sulfite |
| JP2003160580A (en) * | 2001-08-29 | 2003-06-03 | Mitsubishi Chemicals Corp | Ethylene sulfite and production method thereof |
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2005
- 2005-01-12 CN CNB2005100069084A patent/CN100567259C/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US6423861B1 (en) * | 1999-02-03 | 2002-07-23 | Basf Aktiengesellschaft | Method of producing dimethyl sulfite |
| JP2003160580A (en) * | 2001-08-29 | 2003-06-03 | Mitsubishi Chemicals Corp | Ethylene sulfite and production method thereof |
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| Publication number | Publication date |
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| CN1803767A (en) | 2006-07-19 |
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Owner name: FUJIAN CHUANGXIN SCIENCE AND TECHNOLOGY DEVELOPS C Free format text: FORMER OWNER: FUJIAN INST. OF MATTER STRUCTURE, CHINESE ACADEMY OF SCIENCES Effective date: 20100308 |
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