A preparation method of fluoro phosphate materials

A technology of fluorophosphate and ethyl phosphate, which is applied in the field of preparation of fluorophosphate materials, to achieve the effects of precise control of reaction conditions, low cost and easy realization

Active Publication Date: 2012-09-12
HEBEI UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The technical problem to be solved by the present invention is to solve the problems of complex material preparation process, easy to appear derivatives, many side reactions, and difficult to remove by-products in the current technology. A kind of preparation method of electrolyte flame retardant additive fluorophosphate ester material in lithium ion battery, this method adopts ethyl phosphate ((CH3CH2O)PO 4 is used as raw material, fluorinated by hydrogen fluoride, the temperature is 80-92 ° C, 2 atmospheric pressure conditions, using high-purity iron as a catalyst, the obtained product has high yield, high purity, easy purification, and excellent performance Good advantages

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] The invention uses a constant temperature water bath to carry out the reaction, and adopts a sealed polytetrafluoroethylene-lined corrosion-resistant austenitic stainless steel container. The volume of the container content space is 2L. First add 140g of ethyl phosphate and 1.4g of high-purity iron powder (in high-purity iron powder, the iron purity is greater than 99%) in the container, when heated to 80 ° C, feed nitrogen to replace the air, and then slowly (dropping speed is 1-2 drops) / sec) dropwise the hydrofluoric acid liquid 300ml of 10M concentration, this moment according to molar ratio HF: (CH 3 CH 2 O)PO 4 It is 3:1. After the addition, continue to feed nitrogen until the internal pressure reaches 2 atmospheres. After constant temperature and pressure for 6 hours, release the pressure to atmospheric pressure to end the reaction. Then use 0.01Mpa vacuum, distill under reduced pressure at 60°C to remove water, put 1.4g of dried 4A molecular sieve into it, l...

Embodiment 2

[0025] The invention uses a constant temperature water bath for the reaction, adopts a sealed polytetrafluoroethylene-lined corrosion-resistant austenitic stainless steel container, and the internal space volume of the container is 20L. First add 1.4Kg ethyl phosphate and 24g high-purity iron powder in the container, when heated to 92°C, feed nitrogen to replace the air, then slowly add 1.75L of hydrofluoric acid liquid with a concentration of 20M, according to the molar ratio HF:( CH 3 CH 2 O)PO 4 The ratio is 3.5:1. After the addition, continue to feed nitrogen until the internal pressure reaches 3 atmospheres. After constant temperature for 2 hours, release the pressure to atmospheric pressure to end the reaction. Then use 0.01Mpa vacuum, 70 ℃ vacuum distillation to remove water, continue to put in 70g of dried 4A molecular sieve, let it stand for 1h, use 4A molecular sieve to further remove water, filter the liquid with a 1um precision filter, that is what you need The ...

Embodiment 3

[0028] The invention uses a constant temperature water bath for the reaction, adopts a sealed polytetrafluoroethylene-lined corrosion-resistant austenitic stainless steel container, and the internal space volume of the container is 1000L. First add 140Kg ethyl phosphate and 2100g high-purity iron powder in the container, when heated to 90°C, feed nitrogen to replace the air, then slowly add 200L of hydrofluoric acid liquid with a concentration of 15M, molar ratio HF:(CH 3 CH 2 O)PO 4 After the addition, continue to feed nitrogen until the internal pressure reaches 2.5 atmospheres, keep the temperature for 3 hours, release the pressure to atmospheric pressure, and end the reaction. Then use 0.01Mpa vacuum, distill under reduced pressure at 65°C to remove water, continue to put in 4.2Kg dried 4A molecular sieve, let it stand for 1h, use 4A molecular sieve to further remove water, and filter the liquid with a 0.5um precision filter, that is The desired product trifluorophosphat...

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Abstract

The present invention provides a preparation method of fluoro phosphate materials, comprising the following steps: adding into a sealed polytetrafluoroethylene-lined anti-corrosion austenitic stainless steel container ethyl-phosphate and iron powder with the mass of the iron powder being 1-2% of that of the ethyl-phosphate, a step of pumping nitrogen into the container to displace air when the temperature of the container reaches 80-92 DEG C via heating in a water bath, a step of slowly adding hydrofluoric acid liquor in a dropwise manner with a molar ratio of HF and (CH3CH2O)PO4 being 2.5-3.5:1], a step of pumping nitrogen into the container again after the adding step until the inner pressure of the container reaches 2-3 atmospheres, a step of ending the reaction by relieving the inner pressure to atmospheric pressure after the container maintains 2-6 hours of constant temperature, a step of distilling the obtained product under reduced pressure, and a final step of dewatering and filtrating the obtained product and therefore the required product is gained. The gained product in the present invention is free from acidic material such as hydrochloric acid produced by the prior art and capable of overcoming the following acidolysis phenomenon while water is the only material left in the product and can be removed. The preparation method has advantages of simple technological process, low cost and suitability for mass production.

Description

technical field [0001] The technical solution of the present invention relates to a phosphoric acid ester compound, specifically a preparation method of a fluorophosphate ester material. Background technique [0002] Lithium-ion batteries have been widely used as a reliable energy source for portable electronic products such as mobile phones, notebook computers and small power-driven devices due to their advantages of high specific energy, high voltage, no memory effect, environmental protection and long life. However, in recent years, many battery safety accidents have occurred in various countries, mainly due to safety problems caused by thermal runaway caused by batteries under abuse (thermal shock, overcharge, short circuit, etc.), especially in electric vehicles, etc. Safety issues are especially important in bulk power supply applications. Adding flame retardant additives to the electrolyte can effectively improve the safety of batteries, which is a simple and practi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F9/14H01M10/0567
CPCY02E60/10
Inventor 梁广川欧秀芹王丽
Owner HEBEI UNIV OF TECH
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