Preparation method of cyclic sulfate

A technology of cyclic sulfate and dihydrocarbyl sulfate is applied in the field of preparation of cyclic sulfate, and can solve the problems of difficult control of reaction heat release, equipment corrosion, large salt content and the like

Active Publication Date: 2020-11-27
VALIANT CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The present invention aims at problems such as large amount of acid gas, serious corrosion of equipment, large amount of waste water, large salt content, difficult control of reaction heat release and the like in the existing process for synthesizing cyclic sulfuric acid ester, and provides a preparation method of cyclic sulfuric acid ester. Method Using dihydrocarbyl sulfate as raw material, reacting with dibasic ester or cyclic carbonate to prepare cyclic sulfate in one step

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] The preparation of compound A1 vinyl sulfate, concrete steps are as follows:

[0029] A 1000mL three-necked flask was equipped with a vacuum distillation device, and 146.1g (1.0mol) of ethylene glycol diacetate, 151.6g (1.2mol) of dimethyl sulfate and 75g of activated clay were added to a 1000mL three-necked flask, and magnetically stirred. N 2 (50mL / min) replacement, control the vacuum of the reaction system to 1800-2000Pa, raise the temperature to 120°C, the system boils slightly, the vacuum distillation receiving bottle gradually distills out fractions, and the obtained fractions are methyl acetate, which can be sold or recycled ;

[0030] Control the internal temperature at 120-125°C and keep it warm until no fraction distills out, stop the reaction, lower the temperature to 20-30°C, add 500g of dichloroethane, stir for 30min, filter with suction, filter out activated clay, and desolventize the obtained filtrate to Slight solid precipitation in the system;

[003...

Embodiment 2

[0034] The preparation of compound A2 propylene sulfate, concrete steps are as follows:

[0035] 1000mL three-necked flask, equipped with a vacuum distillation device, weighed 102.09g (1.0mol) propylene carbonate, 151.6g (1.2mol) dimethyl sulfate and 63g activated clay into the 1000mL three-necked flask, magnetically stirred, N 2 (50mL / min) displacement, control the vacuum of the reaction system to 1500-1700Pa, raise the temperature to an internal temperature of 125°C, the system boils slightly, and a fraction is gradually distilled out from the receiving bottle of vacuum distillation, and the obtained fraction is dimethyl carbonate, which can be sold or recycled use;

[0036] Control the internal temperature at 125-130°C and keep it warm until no fraction distills out, stop the reaction, lower the temperature to 20-30°C, add 600g of dichloromethane, stir for 30min, filter with suction, filter out activated clay, and desolventize the obtained filtrate to the system Slight sol...

Embodiment 3

[0040] The preparation of compound A3 fluoroethylene sulfate, concrete steps are as follows:

[0041] A 1000mL three-necked flask, equipped with a vacuum distillation device, weighed 106.0g (1.0mol) of fluoroethylene carbonate, 138.7g (1.1mol) of dimethyl sulfate and 48g of activated clay into a 1000mL three-necked flask, magnetically stirred, N 2 (50mL / min) replacement, control the vacuum of the reaction system to 1500-1700Pa, raise the temperature to 105°C, the system boils slightly, the vacuum distillation receiving bottle gradually distills out fractions, and the obtained fractions are dimethyl carbonate, which can be sold or recycled use;

[0042] Control the internal temperature at 105-110°C and keep it warm until no fraction distills out, then stop the reaction. Cool down to 20-30°C, add 500g of dichloromethane, stir for 30 minutes, filter with suction, filter out activated clay, and desolventize the obtained filtrate under reduced pressure until the system has a sligh...

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Abstract

The invention discloses a preparation method of cyclic sulfate. According to the preparation method, dialkyl sulfate serving as a raw material reacts with dibasic ester or cyclic carbonate to preparethe cyclic sulfate in one step. According to the method for preparing the cyclic sulfate in one step by adopting the dialkyl sulfate as the raw material is provided, noble metal catalysis is not needed in the preparation process, corrosive gas is not generated, no wastewater is generated in the post-treatment process, and the method is safer and more environmentally friendly.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of cyclic sulfuric acid ester. Background technique [0002] Cyclic sulfate esters have been known for a long time and have received great attention in organic synthesis. In recent years, a large number of literatures have introduced substances with such similar structures as intermediates of medicine and surfactants, which have broad application prospects. In recent years, cyclic sulfate ester materials have been gradually used as electrolyte additives for lithium-ion batteries, which can effectively suppress side reactions on the electrode surface. [0003] At present (such as Chinese patents CN109485633, CN109369609, CN108707095, CN102241662) the main synthetic routes of these compounds are as follows: [0004] [0005] This route requires a two-step reaction. First, diol compounds and thionyl chloride are used to react to obtain sulfite, and further,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D327/10
CPCC07D327/10
Inventor 林存生付少邦高斌刘兆林石宇
Owner VALIANT CO LTD
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