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Method for preparing difluoro-lithium phosphate and lithium-ion battery non-aqueous electrolyte

A non-aqueous electrolyte and lithium difluorophosphate technology, which is applied in secondary batteries, chemical instruments and methods, circuits, etc., can solve the difficulties in the preparation of difluorophosphate, the difficulty in the synthesis of lithium difluorophosphate, and the lack of effective methods, etc. problems, achieve good electrochemical performance, reduce production costs, and simplify the preparation process

Active Publication Date: 2016-07-27
QUZHOU FLUORIDE & SILICON RES INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The synthesis of the above-mentioned lithium difluorophosphate is too difficult, so that an effective method suitable for industrial production has not been established; and there are many by-products, it is difficult to prepare high-purity difluorophosphate

Method used

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  • Method for preparing difluoro-lithium phosphate and lithium-ion battery non-aqueous electrolyte
  • Method for preparing difluoro-lithium phosphate and lithium-ion battery non-aqueous electrolyte
  • Method for preparing difluoro-lithium phosphate and lithium-ion battery non-aqueous electrolyte

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preparation example Construction

[0027] A preparation method of lithium difluorophosphate of the present invention comprises the following steps: under the protection of an inert gas, preferably, the inert gas is one of nitrogen or argon, and an organic solvent is used as the reaction medium, preferably, the organic solvent is Carbonate solvents or carboxylate solvents, the carbonate solvents or the carboxylate solvents include dimethyl carbonate, diethyl carbonate, butyl acetate, ethyl acetate, lithium hexafluorophosphate and ether compounds React in a reaction vessel with a PFA or PTFE protective layer on the inner layer. Preferably, the ether compound is a chain ether compound or a cyclic ether compound. The chain ether compound is such as ether, tert-butyl ether, etc., and the cyclic Ether compounds such as 18 crown-6, epoxy ether, the volume ratio of the moles of lithium hexafluorophosphate to the solvent is greater than 1.5mol / L, and the ratio of the moles of ether bonds (C-O-C) to the moles of lithium h...

Embodiment 1～5

[0032] Under the protection of a nitrogen atmosphere, firstly add ether compounds into the reactor, then add an organic solution containing a certain concentration of lithium hexafluorophosphate, and control the reaction temperature, time and stirring rate. The reaction conditions are shown in Table 1.

[0033] The above reaction liquid is processed, and the product is obtained by suction filtration, washing and drying. The reaction conditions and analysis results are shown in Table 1.

Embodiment 6～10

[0034] Embodiment 6~10 and comparative example

[0035] The formula of the lithium ion battery non-aqueous electrolyte of lithium difluorophosphate is shown in Table 2, and its preparation method is as follows:

[0036] In a glove box under the protection of argon, the electrolyte salt is added to the organic solvent, mixed evenly, and then the lithium difluorophosphate prepared in any one of Examples 1 to 5 is added to obtain a non-aqueous electrolytic solution for a lithium-ion battery. liquid.

[0037] The formulation of the non-aqueous electrolyte for lithium-ion batteries is shown in Table 2.

[0038] Preparation of positive electrode

[0039] The positive electrode is prepared through the following steps: 90% by weight of lithium iron phosphate, 5% by weight of polyvinylidene fluoride (PVdF), and 5% by weight of acetylene black are mixed; N-methylpyrrolidone is added to form a slurry; the slurry Coated on both surfaces of an aluminum current collector, followed by dry...

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Abstract

The invention discloses a method for preparing difluoro-lithium phosphate and a lithium-ion battery non-aqueous electrolyte.The method includes the steps that under protection of inert gas, an organic solvent serves as a reaction medium, lithium hexafluorophosphate and an ether compound are reacted in a reaction vessel with an inner layer containing a PFA protective layer or a PTFE protective layer, wherein the reacting temperature is 50 DEG C-150 DEG C, and the reacting time is 5 h-20 h; after reaction is finished, a product is filtered and dried to obtain the difluoro-lithium phosphate product.The invention further relates to the lithium-ion battery non-aqueous electrolyte of the difluoro-lithium phosphate prepared with the method.The lithium-ion battery non-aqueous electrolyte comprises 0.5%-2.0% of difluoro-lithium phosphate, 15%-20% of electrolyte salt and 80%-85% of organic solvent.The method for preparing the difluoro-lithium phosphate is easy to operate, mild in condition and convenient to purify, and the high-purity difluoro-lithium phosphate can be obtained.

Description

technical field [0001] The invention relates to a preparation method of lithium difluorophosphate and a non-aqueous electrolyte solution of a lithium ion battery. Background technique [0002] In recent years, the basic research and application development of lithium-ion batteries have become one of the hot spots in the field of new energy, and all developed countries in the world regard it as the breakthrough point of the next emerging industry for development and research. Positive electrode material, negative electrode material, electrolyte material and diaphragm material are the four key materials of lithium-ion batteries. Common electrolyte materials mainly include LiPF 6 、LiBF 4 , LiClO 4 , LiAsF 6 、LiCF 3 SO 3 , LiN(CF 3 SO 2 ) 2 etc., by dissolving these electrolytes in a carbonate organic solvent to form a non-aqueous electrolyte, in which LiPF 6 It is currently the most widely used electrolyte. [0003] Lithium ion batteries employing nonaqueous electroly...

Claims

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Application Information

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IPC IPC(8): C01B25/445H01M10/0525H01M10/0567
CPCC01B25/445H01M10/0525H01M10/0567Y02E60/10
Inventor 张品杰
Owner QUZHOU FLUORIDE & SILICON RES INST
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