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A kind of preparation method of fluorophosphate material

A technology of fluorotriethyl phosphate and substituted triethyl phosphate, which is applied in the field of preparation of fluorotriethyl phosphate materials, can solve the problems of complex preparation process, difficult removal of by-products, and easy occurrence of derivatives, etc. Achieve the effects of simple process, low cost, and precise control of reaction conditions

Active Publication Date: 2016-02-17
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 provide a kind of flame retardant additive fluorotriethyl fluoride in the electrolyte of lithium-ion batteries in view of the complex preparation process of materials in the current technology, which is prone to derivatives, many side reactions, and difficult to remove by-products. The preparation method of base phosphate material, this method adopts triethyl phosphate (CH 3 CH 2 O) 3 PO is used as a raw material, fluorinated by hydrogen fluoride, the temperature is 80-92 ° C, and 2 atmospheric pressure conditions, using high-purity iron as a catalyst, the obtained product has the advantages of high yield, high purity, easy purification, and good performance.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] 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 triethyl phosphate and 1.4g 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 drop / second) dropwise 300ml of hydrofluoric acid liquid of 10M concentration, at this time according to the molar ratio HF:(CH 3 CH 2 O) 3 PO 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 in 1.4g of dried 4A molecular sieve, let it st...

Embodiment 2

[0022] 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 triethyl phosphate and 24g high-purity iron powder into the container, when heated to 92°C, blow in nitrogen to replace the air, slowly add 1.75L of 20M hydrofluoric acid liquid dropwise, according to the molar ratio of HF:(CH 3 CH 2 O) 3 The PO 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 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 product of fluorop...

Embodiment 3

[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 1000L. First, add 140Kg triethyl phosphate and 2100g high-purity iron powder into the container, when heated to 90°C, blow in nitrogen to replace the air, then slowly add 200L of 15M hydrofluoric acid liquid dropwise, molar ratio HF:(CH 3 CH 2 O) 3 The ratio of PO is 3:1. After adding, continue to feed nitrogen until the internal pressure reaches 2.5 atmospheres. After constant temperature for 3 hours, release the pressure to atmospheric pressure to end the reaction. Then use 0.01Mpa vacuum, 65 ℃ vacuum distillation 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, filter the liquid with a 0.5um precision filter, that is The desired product fluorophosphate.

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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 phosphate compound, specifically a preparation method of a fluorotriethyl phosphate 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 practical techni...

Claims

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Application Information

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Patent Type & Authority Patents(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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