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A kind of preparation method of butylene sulfite

A technology of butenyl sulfite and dialkyl sulfite, which is applied in the field of battery additives, can solve the problems of low yield, achieve high yield, reduce cost, and improve reaction yield

Active Publication Date: 2019-04-09
山东永浩新材料科技有限公司
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] This method uses the dangerous chemical thionyl chloride. Since this compound is prone to moisture and releases HCl gas, it has strict requirements for storage and use, and then puts forward higher requirements for production conditions and equipment; at the same time, this method produces a large amount of acid gas. , needs alkali absorption, due to the generation of strong acid gas, which requires the use of high-quality stainless steel or alloy materials for the reaction pipeline and tail gas absorption device; in addition, the reaction yield is 60%~70%, and the yield is low

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  • A kind of preparation method of butylene sulfite

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Embodiment 1

[0021] 1) Pre-dehydrate butanediol with calcium chloride for 24 hours; 2) Add dimethyl sulfite, butanediol, sodium methoxide and magnesium oxide, dimethyl sulfite and butanediol into the rectification reactor The molar ratio of sodium methoxide and magnesium oxide is 1:1.15, and the molar ratio of sodium methoxide and magnesium oxide is 2.3:1. 0.5% of the mass; the temperature was raised to 90°C, and the esterification reaction was performed for 1 hour, and then the temperature was raised to 110°C to continue the reaction for 1 hour, and the reaction was stopped; 3), rectification at -0.095MPa to obtain the butenyl sulfite fraction; 4) the The fraction was recrystallized at 0°C to obtain butenyl sulfite with a purity of 99.5% and a yield of 92.5%.

Embodiment 2

[0023] 1) Pre-dehydrate butanediol with calcium chloride for 24 hours; 2) Add diethyl sulfite, butanediol, sodium ethoxide and magnesium oxide, diethyl sulfite and butanediol to the rectification reactor The molar ratio of sodium ethoxide and magnesium oxide is 1:1.1, and the molar ratio of sodium ethoxide and magnesium oxide is 1.9:1. 0.05% of the mass; the temperature is raised to 100°C, the esterification reaction is performed for 1 hour, and then the temperature is raised to 115°C to continue the reaction for 1.5 hours, and the reaction is stopped; 3) Connect the vacuum system to the reaction system, and rectify at -0.090MPa to obtain butyl sulfite Enyl ester fraction; 4) The fraction was recrystallized at -2°C to obtain 105 g of butenyl sulfite, with a purity of 99.4% and a yield of 91.9%.

Embodiment 3

[0025] 1) Pre-dehydrate butanediol with calcium chloride for 24 hours; 2) Add dimethyl sulfite, butanediol, sodium ethoxide and magnesium oxide, dimethyl sulfite and butanediol into the rectification reactor The molar ratio of sodium ethoxide and magnesium oxide is 1:1.2, and the molar ratio of sodium ethoxide and magnesium oxide is 2.5:1. 1% of the mass; the temperature is raised to 90°C, the esterification reaction is 0.5 hours, and then the temperature is raised to 110°C to continue the reaction for 2.5 hours, and the reaction is stopped; 3) Connect the vacuum system to the reaction system, and rectify at 0.095MPa to obtain butene sulfite 120 g of the ester fraction; 4) Recrystallize the fraction at -4°C to obtain butenyl sulfite with a purity of 99.5% and a yield of 91.7%.

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Abstract

The invention relates to a preparation method for butylene glycol sulfite and belongs to the technical field of battery additives. The preparation method is characterized by comprising the following steps: performing transesterification on sulfurous dialkyl ester and dry butanediol in a rectifying reactor under an effect of a compound catalyst at 90 DEG C-180 DEG C, and then reacting for 2-10 hours, wherein the mole ratio of sulfurous dialkyl ester to dry butanediol is 1:(1.0-1.5) and the compound catalyst is the compound catalyst of alkyl sodium alkoxide and magnesium oxide; and after the ending of reaction, rectifying and recrystallizing, thereby obtaining the butylene glycol sulfite. The preparation method provided by the invention is low in risk of reaction raw materials, high in yield and free from acid side product.

Description

technical field [0001] The invention discloses a preparation method of butenyl sulfite, which belongs to the technical field of battery additives. Background technique [0002] Butenyl sulfite is mainly used in lithium-ion battery additives. The total potential energy and LUMO value of its molecules are lower than those of propylene carbonate (PC), and it has a strong ability to obtain electrons and is not easily oxidized. It is used as an additive mixed with propylene carbonate (PC) in lithium-ion batteries, which can effectively inhibit the co-intercalation of PC in graphite electrodes, better protect the electrodes, significantly improve the internal cycle performance of lithium batteries, and prolong the service life of batteries. [0003] In the prior art, butenyl sulfite is mainly made by butanediol and thionyl chloride through cyclodehydrochlorination (Journal of Organic Chemistry. 1990,55:1211~1217, J. Am. Chem. Soc. 1988,110 ;7538~7539) [0004] [0005] This ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07D327/10
CPCC07D327/10
Inventor 牛会柱
Owner 山东永浩新材料科技有限公司
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