Preparation method of vinyl alkylphosphonate, vinyl alkylphosphonate and application of vinyl alkylphosphonate

A technology of ethylene hydrocarbyl phosphate and ethylene propylene phosphate, which is applied in the field of electrolyte additives, can solve the problems of poor stability of chlorinated cyclic phosphate intermediates, reduced reaction efficiency, difficulty in purification and storage, etc.

Active Publication Date: 2020-10-23
ZHANGJIAGANG HUASHENG CHEM CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that a two-step reaction is required to obtain the final product, and the chlorinated cyclic phosphate intermediate has poor stability and is not easy to purify and store, which will eventually affect the subsequent reaction yield and reduce the overall reaction efficiency

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] This embodiment provides a preparation method of ethylene trifluoroethyl phosphate, which is carried out according to the following steps:

[0037] A. mixed reaction: 100 grams of phosphorus oxychloride and 116.5 grams of hexamethyldisiloxane were mixed and reacted for 1 hour;

[0038] B. The catalyst is added: 2 grams of catalyst gamma-alumina nanofibers are added to the reaction solution in the A step;

[0039] C. Dropping reaction: The mixed solution of 40.5 grams of ethylene glycol and 71.8 grams of trifluoroethanol is added dropwise to the reaction solution of step B, the temperature of the dropping process is controlled at 80 ° C to 90 ° C, and the reaction is kept for 5 hours after the dropping;

[0040] D. Distillation under reduced pressure: Collect 100°C-120°C / (10-15) mmHg fractions to obtain 107.6 grams of ethylene trifluoroethyl phosphate, with a yield of 81% and a content of 98.5%.

Embodiment 2

[0042] This embodiment provides a preparation method of ethylene trifluoroethyl phosphate, which is carried out according to the following steps:

[0043] A. mixed reaction: 150 grams of phosphorus oxychloride and 190.5 grams of hexamethyldisiloxane were mixed and reacted for 1 hour;

[0044] B. The catalyst is added: 6 grams of catalyst gamma-alumina nanofibers are added to the reaction solution in the A step;

[0045] C. Dropping reaction: the mixed solution of 66.8 grams of ethylene glycol and 117.4 grams of trifluoroethanol is added dropwise to the reaction solution of step B, the temperature of the dropping process is controlled at 80 ° C to 90 ° C, and the reaction is kept for 5 hours after the dropping;

[0046] D. Distillation under reduced pressure: Collect 100°C-120°C / (10-15) mmHg fractions to obtain 165.3 grams of ethylene trifluoroethyl phosphate, with a yield of 83% and a content of 98.6%.

Embodiment 3

[0048] This embodiment provides a preparation method of ethylene propylene phosphate, which is carried out according to the following steps:

[0049] A. mixed reaction: 100 grams of phosphorus oxychloride and 116.5 grams of hexamethyldisiloxane were mixed and reacted for 1 hour;

[0050] B. The catalyst is added: 2 grams of catalyst gamma-alumina nanofibers are added to the reaction solution in the A step;

[0051] C. Dropping reaction: the mixed solution of 40.5 grams of ethylene glycol and 41.7 grams of propylene alcohol is added dropwise to the reaction solution of step B, the temperature of the dropping process is controlled at 80 ° C to 90 ° C, and the reaction is kept for 5 hours after the dropping;

[0052] D. Distillation under reduced pressure: Collect 100°C-120°C / (10-15) mmHg fractions to obtain 85.7 grams of ethylene propylene phosphate, with a yield of 80% and a content of 98.4%.

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Abstract

The invention discloses a preparation method of vinyl alkylphosphonate, the vinyl alkylphosphonate and application of the vinyl alkylphosphonate. The preparation method of the vinyl alkylphosphonatecomprises the following steps: A, performing a mixing reaction: mixing phosphorus oxychloride and hexamethyldisiloxane to react for 1 hour; B, adding a catalyst: adding a catalyst into a reacted solution in step A, wherein the catalyst is gamma-aluminum oxide nanofibers; C, carrying out a dropwise adding reaction: dropwise adding a mixed solution of ethylene glycol and trifluoroethanol or a mixed solution of ethylene glycol and allyl alcohol into the reacted solution obtained in step B, controlling the temperature to be 80-90 DEG C in the dropwise adding process, and carrying out heat preservation reaction for 5 hours after dropwise adding is finished; and D, carrying out reduced pressure distillation: collecting 100-120 DEG C/(10-15) mmHg fractions to obtain the vinyl trifluoroethyl phosphate or vinyl allyl phosphate. The method has the beneficial effects of simple process, easiness in operation, low energy consumption, simple feeding mode, few byproducts, high product yield and high product purity.

Description

technical field [0001] The invention belongs to the technical field of electrolyte additives, and in particular relates to a preparation method of vinyl phosphate, vinyl phosphate and application thereof. Background technique [0002] Rechargeable lithium-ion batteries are currently the most important power components of electric vehicles. In order to meet the needs of high battery life, long life, and fast charging, rechargeable lithium-ion batteries are currently developing in the direction of high active positive and negative electrodes, high voltage, and high temperature work. , put forward higher requirements for the safety of rechargeable lithium-ion batteries. Preventing battery thermal runaway is a central goal of improving the safety of rechargeable Li-ion batteries. Therefore, the development of high-safety electrolyte additives has become a hot and difficult point of current research. Hydrocarbon vinyl phosphate (also known as hydrocarbyl vinyl phosphate) additiv...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/6574H01M10/0567H01M10/0525
CPCC07F9/65742H01M10/0567H01M10/0525H01M2300/0025Y02E60/10
Inventor 吴国栋陆海媛曹娜周立新
Owner ZHANGJIAGANG HUASHENG CHEM CO LTD
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