Method for preparing high-purity lithium difluorophosphate by utilization of organo tin fluoride

A technology of lithium difluorophosphate and lithium dichlorophosphate, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve the problems of multiple production links, low product purity, difficult extraction and separation, and achieve equipment and environmental protection Low requirements, simple process, high purity effect

Active Publication Date: 2013-08-21
中山市华玮新能源科技有限公司 +2
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] The purpose of the present invention is to overcome the many production links in the preparation of lithium difluorophosphate in the prior art. Whether it is controlled hydrolysis reaction or gas-solid reaction under high temperature conditions, the products are mostly mixtures, extraction and separation are difficult, and the product purity is not high. To provide a method for preparing high-purity lithium difluorophosphate using organic tin fluoride, which is technically easy to control and has simple process conditions, and can be used to improve the performance of non-aqueous electrolyte batteries by using cheap and easy-to-obtain raw materials for low-cost industrial production The additive lithium difluorophosphate

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0041] In a closed reaction kettle, under the protection of nitrogen with a water content of less than 10ppm and a pressure of 0.5Mpa, 30.7g (0.2mol) POCl 3 and 11.6g (0.1mol) Li 3 PO 4 Suspended in 800mL of dry ethylene glycol dimethyl ether, the temperature of the reactor was slowly raised to 120°C for 5 hours under stirring, then the temperature of the reactor was lowered to room temperature, and 109.7g (0.6mol) Me 3 SnF was added to the reaction kettle, and the temperature of the reaction kettle was slowly raised to 100°C under stirring for 7 hours. After cooling to room temperature, a clear and transparent solution was obtained, and the solvent and the generated Me 3 SnCl, the remaining solids were redissolved with freshly dried tetrahydrofuran, and then recrystallized at -20 to 0°C to generate crystalline products in the solution. The mother liquor was removed by filtration, and the crystalline solids were collected. 30.4g LiPO was obtained after vacuum drying 2 f 2 ...

Embodiment 2

[0043] In a closed reaction kettle, under the protection of nitrogen with a water content of less than 10ppm and a pressure of 0.8Mpa, 30.7g (0.2mol) POCl 3 and 11.6g (0.1mol) Li 3 PO 4 Suspended in 800mL dry acetonitrile, under stirring, the temperature of the reactor was slowly raised to 100°C for 5 hours, and then the temperature of the reactor was lowered to room temperature, and 56.1g (0.3mol) Me 2 SnF 2 Add it in the reaction kettle, and then slowly raise the temperature of the reaction kettle to 120° C. for 7 hours under stirring. After cooling to room temperature, a clear and transparent solution is obtained, and the solvent and the generated Me 2 SnCl 2 , the remaining solid was redissolved with freshly dried acetonitrile, and then recrystallized at -20 to 0°C to form a crystalline product in the solution, the mother liquor was removed by filtration, the crystalline solid was collected, and vacuum 28.1gLiPO was obtained after drying 2 f 2 Crystalline solid with ...

Embodiment 3

[0045] In a closed reaction kettle, under the protection of nitrogen with a water content of less than 10ppm and a pressure of 1.0Mpa, 30.7g (0.2mol) of POCl 3 , 11.6g (0.1mol) Li 3 PO 4 and 109.7g (0.6mol) Me 3 SnF was added to the reactor and suspended in 800mL of dry ethyl methyl carbonate, and the temperature of the reactor was slowly raised to 120° C. for 10 hours under stirring, and then the temperature of the reactor was lowered to room temperature to obtain a clear and transparent solution. The solvent and the resulting Me 3SnCl, the remaining solids were redissolved with freshly dried acetonitrile, and then recrystallized at -20 to 0°C to generate crystalline products in the solution. The mother liquor was removed by filtration, and the crystalline solids were collected and heated at 60°C. 30.2g LiPO was obtained after vacuum drying 2 f 2 Crystalline solid with a purity of 99.5%.

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PUM

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Abstract

The invention discloses a method for preparing high-purity lithium difluorophosphate by the utilization of organo tin fluoride. By the utilization of the characteristic that organo tin fluoride is easily subjected to a halogen exchange reaction with a phosphorus compound containing chlorine, bromine and iodine, lithium dichlorophosphate is firstly prepared by a simple method, and then organo tin fluoride and lithium dichlorophosphate undergo a contact reaction so as to generate lithium difluorophosphate. The raw materials provided by the invention are easily available and the reactions are easy to operate. Conditions of the whole reaction process are mild; no by-products appear; the process is simple; requirements on equipment and environmental protection are low; and the possibility of impurity introduction is avoided. Thus, the lithium difluorophosphate generated by the preparation method has high purity and good quality.

Description

【Technical field】 [0001] The invention relates to a method for preparing lithium difluorophosphate, in particular to a method for preparing high-purity lithium difluorophosphate by using organic tin fluoride. 【Background technique】 [0002] In recent years, the basic research and application development of lithium-ion batteries have become one of the hotspots in the field of new energy, and developed countries around the world have developed and researched them as a breakthrough point for the next emerging industry. Positive electrode material, negative electrode material, electrolyte material and separator material are the four key materials of lithium ion battery. The common electrolyte materials are LiPF 6 , LiBF 4 , LiClO 4 , LiAsF 6 , LiCF 3 SO 3 , LiN (CF 3 SO 2 ) 2 etc., by dissolving these electrolytes in carbonate organic solvents to formulate non-aqueous electrolytes, in which LiPF 6 It is the most widely used electrolyte. [0003] Lithium-ion batteries u...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): H01M10/0563C01B25/455
CPCY02E60/10
Inventor 余佩华余佩娟
Owner 中山市华玮新能源科技有限公司
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