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Method for preparing lithium difluorophosphate

A technology of lithium difluorophosphate and difluorophosphoric acid, applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as high production risk factor, high raw material utilization rate, complex production process, etc., and reduce production cost , convenient transportation, high purity effect

Active Publication Date: 2018-02-23
TIANJIN JINNIU POWER SOURCES MATERIAL +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the use of dangerous gases such as fluorine gas and phosphorus pentoxide in these methods, the production risk factor is relatively high; and in order to ensure production safety, it is necessary to precisely control the use of gas to prevent gas leakage, making the production process more complicated; In addition, because the gas participates in the reaction, it is difficult to ensure a high raw material utilization rate

Method used

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  • Method for preparing lithium difluorophosphate
  • Method for preparing lithium difluorophosphate
  • Method for preparing lithium difluorophosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1-4

[0070] The reaction principle is that lithium carbonate and difluorophosphoric acid react in a benign non-aqueous solvent of lithium difluorophosphate, and the reaction equation is: 2HPO 2 f 2 +Li 2 CO 3 =2LiPO 2 f 2 +H 2 O+CO 2 .

[0071] Specific steps include:

[0072] (1), reflux reaction

[0073] 1. Take lithium carbonate and difluorophosphoric acid in proportion, and set aside; ensure that lithium carbonate is excessive, so as to avoid containing unreacted difluorophosphoric acid in the solution obtained after the completion of the reaction, thereby causing the purity of the product to decrease and the yield to decrease;

[0074] 2. Add the above-mentioned weighed lithium carbonate into an appropriate amount of benign non-aqueous solvent of lithium difluorophosphate, stir to obtain a uniform mixture; obtaining a uniform mixture can stabilize the system, and lithium carbonate can be uniformly dispersed in the solvent; The amount of solvent used will ensure that t...

Embodiment 5-8

[0087] The reaction principle is that lithium hydroxide and difluorophosphoric acid react in a benign non-aqueous solvent of lithium difluorophosphate, and the reaction equation is: HPO 2 f 2 +LiOH=LiPO 2 f 2 +H 2 O;

[0088] Specific steps include:

[0089] (1), reflux reaction

[0090] 1. Weigh lithium hydroxide and difluorophosphoric acid in proportion, and set them aside; ensure that lithium hydroxide is excessive, so as to avoid containing unreacted difluorophosphoric acid in the solution obtained after the reaction is completed, thereby causing the purity of the product to decrease and the yield to decrease;

[0091] ②. Add the above-mentioned weighed lithium hydroxide into an appropriate amount of benign non-aqueous solvent of lithium difluorophosphate, and stir to obtain a uniform mixture; obtaining a uniform mixture can stabilize the system, and lithium hydroxide can be uniformly distributed in the solvent. Dispersion; the amount of solvent used should ensure th...

Embodiment 9-12

[0104] The reaction principle is that lithium carbonate and difluorophosphoric acid react in a poor non-aqueous solvent of lithium difluorophosphate, and the reaction equation is: 2HPO 2 f 2 +Li 2 CO 3 =2LiPO 2 f 2 +H 2 O+CO 2 .

[0105] Specific steps include:

[0106] (1) Crystallization reaction

[0107] ①. Weigh lithium carbonate and difluorophosphoric acid in proportion and set them aside; control the excess of difluorophosphoric acid to completely react the lithium carbonate in the system, so that all the insoluble solids in the final reaction system are lithium difluorophosphate, so as to ensure the stability of the product. purity;

[0108] ②. Add the above-mentioned weighed lithium carbonate into the poor non-aqueous solvent of lithium difluorophosphate, stir to obtain a uniform mixture; the amount of poor water solvent should meet the requirement of uniform dispersion of lithium carbonate in it; at the same time, due to the reaction After the end, a part of...

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Abstract

The invention discloses a method for preparing lithium difluorophosphate. The synthesis principle is that difluorophosphate is subjected to a contact reaction with lithium hydroxide in a non-aqueous solvent, or difluorophosphate contacts is subjected to the contact reaction with lithium carbonate in the non-aqueous solvent, and specifically a reaction equation is that HPO2F2+LiOH=LiPO2F2+H2O, or 2HPO2F2+Li2CO3=2LiPO2F2+H2O+CO2. According to the method, difluorophosphate and lithium carbonate or lithium hydroxide are adopted as main raw materials, lithium hexafluorophosphate which is common inthe prior art is not used, and thus the reaction cost is reduced; in addition, in the preparation process, no harmful gas such as a fluorine gas is used, and the reaction process is easy to control, high in security coefficient and low in equipment cost; the reaction process is a solid-liquid reaction, the raw materials are target products are both free of gas, the raw materials and the products are easy in purity control and convenient to transport, and the raw material utilization rate is high, so that the cost can be lowered.

Description

technical field [0001] The invention relates to a preparation method of difluorophosphate, in particular to a preparation method of lithium difluorophosphate. Background technique [0002] In recent years, lithium-ion power batteries and energy storage batteries have become one of the research hotspots in the field of new energy. At present, the anode materials of lithium-ion power batteries are mainly lithium iron phosphate and nickel-cobalt-manganese ternary materials, and the electrolyte is lithium hexafluorophosphate (LiPF 6 ) with a liquid electrolyte system of carbonate-based organic solvents. [0003] In the ternary cathode material system, an appropriate amount of lithium difluorophosphate (LiPO 2 f 2 ) can reduce the internal resistance of the battery, and form a protective film on the positive electrode of the battery, so that the cycle performance of the battery is significantly improved; at the same time, in the high-pressure lithium ferrous phosphate positive...

Claims

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Application Information

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IPC IPC(8): C01B25/445
CPCC01B25/445
Inventor 孙培亮赵庆云刘大凡安峰王坤袁莉
Owner TIANJIN JINNIU POWER SOURCES MATERIAL
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