Method for preparing perfluor alkyl ethide phosphite ester

A technology of perfluoroalkyl ethyl phosphite and perfluoroalkyl ethanol is applied in the field of preparation of perfluoroalkyl ethyl phosphite, which can solve the problem of electrochemical instability of flame retardant additives and negative performance of lithium ion batteries. Influence and other issues, to achieve the effects of good electrochemical stability and thermodynamic stability, obvious flame retardant effect, and good comprehensive performance

Inactive Publication Date: 2013-04-24
JIANGSU GUOTAI SUPER POWER NEW MATERIALS
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0010] However, according to the current research results, the flame retardant additives used have electrochemical instability or other unfavorable physical and chemical properties - such as high melting point, high viscosity, etc., which will have a certain negative impact on the performance of lithium-ion batteries

Method used

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Examples

Experimental program
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Embodiment

[0037] Step 1 Synthesis

[0038] In a 2000mL four-neck flask, configure a cold bath with a freezing temperature of less than -10°C, a thermometer with a range of -50°C to +150°C, with stirring, and a condensing reflux tube with a freezing temperature of less than -10°C (exhaust gas discharge ), equipped with HCl tail gas absorption device. 1681g of CF with a content greater than 99% 3 CH 2 Put OH into a four-neck flask, stir, turn on the freezer, cool down to -10°C, slowly add 770g of PCl with a content greater than 99% dropwise through a constant pressure titration funnel 3 , The dropping process continued for 5h, and the generated HCl gas was absorbed and removed by the absorption device. When no HCl gas is generated, turn on a small amount of N 2 , bubbling to drive away free HCl, use acid-base extensive pH test to release gas, when it is weakly acidic, stop bubbling N 2 ;

[0039] Step 2 neutralizes and removes impurities (CF 3 CH 2 O) 2 POH and Filtration

[004...

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PUM

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Abstract

The invention discloses a method for preparing perfluor alkyl ethide phosphite ester with better inflaming retarding effect, lower viscosity, and better electrochemical stability, which comprises the following steps: (1) phosphorus trichloride and perfluor alkyl ethanol are fully reacted according to the mol ratio of 1:2-1:9 within minus 30 DEG C to 100 DEG C; generated primary product is an acid mixture of perfluor alkyl ethide phosphite ester; (2) the acid mixture is fully neutralized by using alkaline matter with minus 30 DEG C to 100 DEG C of neutral temperature to ensure that the PH value of a neutralized solution is more than 7, and then the solution is filtered to remove impurities; filtrate is collected; (3) the filtrate is distilled in subpressure under minus 0.05Mpa to minus 0.1Mpa; distillation with more than 99% of contents of perfluor alkyl ethide phosphite ester is collected; (4) distillation with more than 99% of contents is dehydrated with a molecular sieve under minus50 DEG C to minus 100 DEG C, thus obtaining perfluor alkyl ethide phosphite ester with the contents of 99%, which can be used as flame retardant of lithium ion battery electrolyte.

Description

technical field [0001] The invention relates to a preparation method of a perfluoroalkyl ethyl phosphite that can be used as a flame retardant for a lithium-ion battery electrolyte. Background technique [0002] The huge application prospects of large-capacity lithium-ion power batteries have attracted the attention of many scientists. However, one of the obstacles to the development of large-capacity lithium-ion power batteries is safety issues, especially under abuse (such as thermal shock, overcharge, overdischarge, short circuit, etc.), there are often safety hazards such as fire and explosion. In order to develop high-capacity lithium-ion batteries, safety issues must be solved, and the purpose of adding flame retardant additives is to improve the safety performance of batteries. When the flame retardant additive is heated, it releases free radicals with flame retardant properties, which can capture hydrogen radicals or hydroxyl radicals in the gas phase, thereby preve...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C07F9/142
Inventor 陶荣辉徐晓强陈剑钱晓兵赵世勇
Owner JIANGSU GUOTAI SUPER POWER NEW MATERIALS
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