Preparation method of cyclic sulfates

A technology of cyclic sulfate and cyclic sulfite, applied in the field of preparation of cyclic sulfate, can solve the problems of low conversion rate of a single batch, a large amount of waste, incomplete reaction, etc., and achieve a thorough reaction and an easy reaction. , the effect of less by-products

Inactive Publication Date: 2019-03-05
ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the following defects: the single batch conversion rate is low, there is a large amount of waste, and the reaction is not complete. In addition, the reaction temperature needs to be controlled at about 5 ° C during the reaction process, which requires the use of equipment such as refrigerators to freeze the reaction process. heat removal, resulting in cumbersome process and high energy consumption

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0017] The preparation method of cyclic sulfuric acid ester is described in detail below.

[0018] The preparation method of cyclic sulfuric acid ester, described cyclic sulfuric acid ester comprises: vinyl sulfate, butene sulfate, propylene sulfate. The structural formula of vinyl sulfate The structural formula of propylene sulfate The structural formula of butenyl sulfate is as follows:

[0019] The preparation method of cyclic sulfuric acid ester comprises the following steps.

[0020] 1. Add an organic solvent into the reaction kettle, then add cyclic sulfite and 30% hydrogen peroxide into the reaction kettle, and then add the catalyst. The reaction temperature is controlled at 30°C to 40°C. In order to improve the uniformity of heating The reaction temperature is achieved by heating the jacket layer. The reaction time is controlled within 1 to 5 hours, inclusive.

[0021] The organic solvent in the reactor is dichloromethane or ethylene dichloride; the mass ratio...

Embodiment 1

[0028] Example 1. Add 310 g of dichloromethane into a 1000 ml three-necked flask with a jacket, then add 30 g of vinyl sulfite, 63 g of hydrogen peroxide with a mass concentration of 30%, and then add 1 g of catalyst TS-1 (titanium-silicon molecular sieve), start stirring, and pass through the jacket. Add 32°C hot water to make the temperature in the three-necked flask reach 30°C, keep the temperature for 3 hours, and the reaction is over. The reaction solution was left to stand for liquid separation, the primary organic layer was about 332g, and the aqueous layer was 66g. The primary organic layer was washed with 83 g of water for 10 min, and left to stand for liquid separation to obtain a secondary organic layer of 326 g and an aqueous layer of 82 g. 197g of the organic solvent was distilled off from the secondary organic layer under reduced pressure, and the remaining liquid crystals were filtered and dried to obtain solids, i.e. 15g of the finished product vinyl sulfate, ...

Embodiment 2

[0029] Example 2. Add 413g of dichloromethane to a 1000ml three-necked flask with a jacket, then add 30g of vinyl sulfite and 63g of hydrogen peroxide with a mass concentration of 30%, then add 1g of catalyst TS-1 (titanium silicon molecular sieve), start stirring, and pass Add hot water at 42°C to make the temperature in the three-necked flask reach 40°C, keep the temperature for 1.5 hours, and the reaction ends. The reaction solution was left to stand for liquid separation, the primary organic layer was about 426g, and the aqueous layer was 67g. 170 g of water was added to the primary organic layer and washed for 10 min, and liquid separation was performed to obtain 421 g of the secondary organic layer and 173 g of the aqueous layer. 306g of organic solvent was distilled off from the secondary organic layer under reduced pressure, and the remaining liquid crystals were filtered and dried to obtain 15.8g of solid, i.e. finished vinyl sulfate, and 101g of mother liquor (which...

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Abstract

The invention discloses a preparation method of cyclic sulfates. The cyclic sulfates comprise ethylene sulfate, butylene sulfate, propylene sulfate. The preparation method comprises the following steps: (1) adding an organic solvent into a reaction kettle, then adding a cyclic sulfite and hydrogen peroxide with a mass concentration of 30% into a reaction kettle, adding a catalyst, and controllingthe reaction temperature to be 30-40 DEG C, wherein the cyclic sulfite comprise ethylene sulfite, butylene sulfite or propylene sulfite, and the catalyst is a TS-1 (titanium-silicon molecular sieve);(2) separating the reaction liquid after the reaction is finished, taking a primary organic layer, washing the primary organic layer by water, and then carrying out layering by standing to obtain a secondary organic layer; and (3) evaporating out the organic solvent from the secondary organic layer for crystallization, and carrying out drying to obtain a finished product. The preparation method has the advantages that the reaction process is mild, heat removal is not required, the reaction is easy to control, by-products are few, the reaction is thorough, and the conversion rate is high.

Description

technical field [0001] The invention relates to a preparation method of cyclic sulfuric acid ester. Background technique [0002] Cyclic sulfates, including vinyl sulfate, propylene sulfate, and butylene sulfate, can be used as battery electrolyte additives, pharmaceutical intermediates, etc., and are widely used. [0003] The structural formula of vinyl sulfate The structural formula of propylene sulfate The structural formula of butenyl sulfate is as follows: [0004] The method for preparing cyclic sulfuric acid ester at present mainly is: take cyclic sulfite and sodium hypochlorite as raw materials, react at a temperature of 5° C. under the effect of a ruthenium trichloride catalyst. This method has the following defects: the single batch conversion rate is low, there is a large amount of waste, and the reaction is not complete. In addition, the reaction temperature needs to be controlled at about 5°C during the reaction, which requires the use of equipment such a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D327/10
CPCC07D327/10
Inventor 卢云龙岳立王剑刘磊陈晓华杨波
Owner ZHANGJIAGANG GUOTAI HUARONG NEW CHEM MATERIALS CO LTD
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