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Preparation method of vinyl sulfate

A technology of vinyl sulfate and vinyl sulfite, which is applied in the field of lithium-ion battery electrolyte additives, can solve the problems of high corrosion of sulfur trioxide, high risk of ethylene oxide, and increased product cost, and achieve low price and low production cost. Low, the effect of reducing production costs

Inactive Publication Date: 2019-02-22
ZHUHAI SMOOTHWAY ELECTRONICS MATERIALS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Report the synthetic method of a large amount of vinyl sulfates in literature and patent at present, as: CN102241662A discloses adopting ruthenium trichloride as catalyzer, and sodium hypochlorite prepares vinyl sulfate as oxidant oxidation vinyl sulfite, but ruthenium trichloride is as catalyzer, and catalyst Expensive, accounting for more than 50% of the product cost, resulting in a substantial increase in product cost
CN106831701A discloses the catalytic addition of sulfur trioxide and ethylene oxide to prepare vinyl sulfate. Although this method has a high atom utilization rate, ethylene oxide belongs to high-risk chemicals, and sulfur trioxide is highly corrosive

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] (1) Cyclization reaction: Add 100g of ethylene glycol and 50g of dichloromethane to the reaction kettle A, adjust the temperature of the reaction kettle to 12°C, add 230g of thionyl chloride dropwise, and the dropping time is 30min. , continue to react for 2h. After the reaction is completed, carry out vacuum distillation to remove HCl and unreacted SOCl 2 , and then add saturated aqueous sodium bicarbonate to wash until the pH value of the solution is ≥7, and then separate the liquid to obtain 200 g of a dichloromethane solution of vinyl sulfite, containing 160 g of the product, and the yield is 92%. The vinyl sulfite dichloromethane solution was transferred to Reactor B for later use.

[0024] (2) Oxidation reaction: add 150 g of dichloromethane in reactor B, add 7.3 g of 10% potassium dihydrogen phosphate solution, and use 15% sodium bicarbonate solution to adjust pH=9, reduce the temperature of the reactor to 8°C, 734.4 g of 30% sodium hypochlorite aqueous solutio...

Embodiment 2

[0027] (1) Cyclization reaction: Add 100g of ethylene glycol and 100g of dichloromethane to the reactor A, adjust the temperature of the reactor to 12°C, add 250g of thionyl chloride dropwise for 30min, after the dropwise addition , continue to react for 2h. After the reaction is completed, carry out vacuum distillation to remove HCl and incompletely reacted SOCl 2 , and then add saturated aqueous sodium bicarbonate to wash until the pH value of the solution is ≥7, and then separate the liquid to obtain 210 g of a dichloromethane solution of vinyl sulfite, containing 152 g of the product, and the yield is 87.3%. The vinyl sulfite dichloromethane solution was transferred to Reactor B for later use.

[0028] (2) Oxidation reaction: add 100 g of dichloromethane into reactor B, add 0.69 g of 10% potassium dihydrogen phosphate solution, and adjust pH=9 with 15% sodium bicarbonate solution, and reduce the temperature of the reactor to 8° C. 697.7 g of 30% sodium hypochlorite aqueo...

Embodiment 3

[0031] (1) Cyclization reaction: Add 100g of ethylene glycol and 50g of dichloromethane to the reaction kettle A, adjust the temperature of the reaction kettle to 12°C, add 230g of thionyl chloride dropwise, and the dropping time is 30min. , continue to react for 2h. After the reaction is completed, carry out vacuum distillation to remove HCl and incompletely reacted SOCl 2 , and then add saturated aqueous sodium bicarbonate for washing until the pH value of the solution is ≥7, and then separate the liquids to obtain 203 g of a dichloromethane solution of vinyl sulfite, containing 161 g of the product, and the yield is 92.4%. The vinyl sulfite dichloromethane solution was transferred to Reactor B for later use.

[0032] (2) Oxidation reaction: add 150g of dichloromethane to reactor B, add 11.61g of 10% sodium tungstate aqueous solution, and use 15% sodium bicarbonate solution to adjust the pH=9, reduce the temperature of the reactor to 8°C, drop Add 739.2 g of 30% sodium hyp...

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Abstract

The invention relates to a preparation method of vinyl sulfate. The preparation method comprises the following steps: adding ethylene glycol into a reaction kettle A filled with a halohydrocarbon solvent, uniformly stirring, dropwise adding thionyl chloride to carry out a substitution reaction, removing hydrogen chloride by reduced-pressure distillation, then, washing a reaction solution to be neutral by using a saturated sodium bicarbonate solution, standing still, and skimming to obtain a glycol sulfite halohydrocarbon solution; adding the glycol sulfite halohydrocarbon solution into a reaction kettle B, adding monopotassium phosphate or sodium tungstate as a catalyst, regulating the pH by using a sodium bicarbonate aqueous solution, and adding a sodium hypochlorite aqueous solution to carry out an oxidation reaction; at the end of the reaction, skimming to obtain a vinyl sulfate halogenated alkane solution, carrying out concentration, then, adding n-hexane to carry out recrystallization, and carrying out filtration to obtain high-purity vinyl sulfate. By using the preparation method, raw materials are available, the price of the catalyst is low, the product is easy to purify, and the obtained product is low in acidity, low in water content, high in purity and suitable for large-scale production.

Description

[technical field] [0001] The invention discloses a preparation method of vinyl sulfate, belonging to the technical field of electrolyte additives for lithium-ion batteries. [Background technique] [0002] With the depletion of oil resources and the aggravation of environmental pollution, new energy electric vehicles driven by lithium-ion power batteries have become the direction of future automobile development, and are also the commanding heights of competition among countries. Among them, ternary NCM and NCA batteries have the characteristics of high energy density and low cost, and have become a hot spot in the research of power lithium-ion batteries, but there are still some defects in their cycle life, high and low temperature cycle and storage performance. Vinyl sulfate, as a lithium-ion battery electrolyte additive, can effectively inhibit the initial capacity drop of lithium-ion batteries, increase the initial discharge capacity, improve the charge and discharge perf...

Claims

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Application Information

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IPC IPC(8): C07D327/10
CPCC07D327/10
Inventor 毛冲宋金龙刘李阳时迎华沙向峰王霹雳戴晓兵
Owner ZHUHAI SMOOTHWAY ELECTRONICS MATERIALS
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