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Preparation method of dicyclic sulfite and dicyclic sulfate

A technology of cyclic sulfite and cyclic sulfate, which is applied in the direction of organic chemistry, can solve the problems of high requirements for environmental protection and safety production, long reaction time, and unfriendly environment, so as to improve utilization rate and reduce reaction time. It takes a short time to avoid the effect of side effects

Active Publication Date: 2021-04-23
JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method uses a large amount of organic solvents, produces a large amount of waste liquid, is not friendly to the environment, and takes a long time for the reaction, and has relatively high requirements for environmental protection and safe production.

Method used

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  • Preparation method of dicyclic sulfite and dicyclic sulfate
  • Preparation method of dicyclic sulfite and dicyclic sulfate
  • Preparation method of dicyclic sulfite and dicyclic sulfate

Examples

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preparation example Construction

[0041] The invention provides a method for preparing bicyclic sulfite, which is prepared by mixing compound A with thionyl chloride for reaction;

[0042] Compound A has a structure shown in formula (1):

[0043]

[0044] Bicyclic sulfite has a structure shown in formula (2):

[0045]

[0046] Among them, R 1 ~R 8 Each occurrence is independently selected from H, a halogen atom, a cyano group, silane trifluoride, or a hydrocarbon group with 1 to 3 carbon atoms substituted by at least one X;

[0047] X are each independently selected from H, F, silyl, cyano or isocyanate.

[0048] In a concrete example, R 1 ~R 8 Each occurrence is independently selected from H, F, cyano, silane trifluoride, or an alkyl group with 1 to 3 carbon atoms substituted by at least one X.

[0049]In a specific example, compound A is pentaerythritol, 3,3-bis-(1-hydroxy-ethyl)-pentane-2,4-diol, 1,3-difluoro-2,2-dihydroxy Methylpropane-1,3-propanediol, 1,3-difluoro-2,2-bis-(fluoromethylol)prop...

Embodiment 1

[0069] The present embodiment provides a kind of preparation method of bicyclic sulfite and bicyclic sulfate, specifically as follows:

[0070] At room temperature, add thionyl chloride (0.8 mol) and pentaerythritol (0.2 mol) into a reaction flask protected by nitrogen circulation, stir and raise the reaction temperature to 60°C, stir for 6 hours, and cool to room temperature after the reaction is complete. Solid-liquid separation, liquid thionyl chloride recycling, solid bicyclic sulfite (3,9-dioxide-2,4,8,10-tetraoxa-3,9-dithiaspiro[ 5.5] Undecane), the yield is 85.5%, and the purity is 99.23%;

[0071] Subsequently, acetonitrile, bicyclic sulfite (0.171mol), and ruthenium trichloride hydrate (0.3%) were sequentially added to the reaction flask, and after cooling down to -5°C to stabilize, sodium hypochlorite (0.38mol) solution was added dropwise, and the addition was completed After the temperature was maintained at room temperature, after the reaction was completed for 1 ...

Embodiment 2

[0073] The present embodiment provides a kind of preparation method of bicyclic sulfite and bicyclic sulfate, specifically as follows:

[0074] At room temperature, add thionyl chloride (1.0 mol) and pentaerythritol (0.2 mol) into a reaction flask protected by nitrogen circulation, stir and raise the reaction temperature to 40°C, stir for 6 hours, cool to room temperature, and separate the solid and liquid. Liquid thionyl chloride is recycled and used, and the solid is bicyclic sulfite crude product (3,9-dioxide-2,4,8,10-tetraoxa-3,9-dithiaspiro[5.5]dec One alkane), the yield is 86.7%, and the purity is 99.41%.

[0075] Subsequently, dichloromethane, bicyclic sulfite (0.173mol), and ruthenium trichloride hydrate (0.25%) were sequentially added to the reaction flask, and after cooling down to -5°C to stabilize, sodium hypochlorite (0.47mol) solution was added dropwise. After the addition, the temperature was maintained at room temperature for 1 h, the organic phase was collect...

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Abstract

The invention provides a preparation method of dicyclic sulfite. The dicyclic sulfite is prepared by mixing a compound A and thionyl chloride and reacting; the compound A has a structure as shown in a formula (1) in the specification; the dicyclic sulfite has a structure as shown in a formula (2) in the specification; R1 to R8 are independently selected from H, a halogen atom, a cyano group, silane trifluoride or at least one X-substituted alkyl group with 1 to 3 carbon atoms when appearing at each time; and X is respectively and independently selected from H, F, silane group, cyano group or isocyanate group. The preparation method is mild in reaction, free of solvent participation, short in reaction time and easy in process control, and can be used for preparing high-yield and high-purity dicyclic sulfite.

Description

technical field [0001] The invention relates to the field of organic synthesis, in particular to a preparation method of bicyclic sulfite and bicyclic sulfate. Background technique [0002] In recent years, due to the advantages of high energy density, long cycle life and no pollution, lithium secondary batteries have very broad application prospects in electronics, batteries and energy. However, because lithium-ion batteries are prone to gas production under high temperature conditions, resulting in battery swelling or excessive internal pressure, resulting in a great potential safety hazard for the battery, and at the same time greatly reducing the service life of the battery. In order to solve the problem of high-temperature gas production in lithium batteries, some bicyclic sulfate additives are usually added to the electrolyte. This type of additive can form an SEI film on the surface of the positive and negative electrodes of the lithium battery to inhibit the high-tem...

Claims

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Application Information

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IPC IPC(8): C07D497/10
CPCC07D497/10Y02E60/10
Inventor 唐华英范伟贞赵经纬
Owner JIUJIANG TINCI ADVANCED MATERIALS CO LTD
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