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Method for continuous preparation of lithium borate dioxalate

A technology of lithium bisoxalate borate and oxalate, which is applied in the field of continuous preparation of lithium bisoxalate borate, can solve the problems of large SEI film impedance, battery capacity attenuation, and limited working conditions, and achieve good electrochemical stability and thermal stability. Improved electrical conductivity and high thermal stability

Active Publication Date: 2019-04-12
HUBEI HONGYUAN PHARMA
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Problems solved by technology

[0002] With the development of microelectronics technology and the increase of miniaturized electronic equipment, lithium batteries can be fully developed and used due to their superior performance. As an important part of batteries, electrolytes have a very important impact on battery performance. At present, the most widely used lithium ion The battery electrolyte is lithium hexafluorophosphate, which has good electrical conductivity and electrochemical stability. However, lithium hexafluorophosphate still has obvious shortcomings such as sensitivity to water, excessive resistance of the SEI film formed at low temperature, and decomposition at 80°C, which lead to its working conditions being severely affected. It is easy to decompose and produce HF at high temperature and when it encounters water. The existence of HF will dissolve the positive metal material and change the structure, which will cause the battery capacity to decay.

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  • Method for continuous preparation of lithium borate dioxalate

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Embodiment 1

[0024] The present invention provides the following technical solutions: a method for continuously preparing lithium bisoxalate borate, comprising the following steps:

[0025] Step (1): Weigh lithium hydroxide, boric acid and oxalic acid according to Li:B:C2O4 with a molar ratio of 1:1:2.05, and grind them with a ball mill for 45 minutes respectively.

[0026] Step (2): Slowly add the three materials in proportion to the stirring tank at room temperature, and slowly add a small amount of pure water, the amount of water accounts for about 3% of the weight of the solid material, and adjust the material to mix evenly.

[0027] Step (3): Turn on the feeder, add the mixed material obtained in step (2) into the feeding bin of the three-stage temperature zone rotary reaction furnace, and send the material into the reaction furnace at a rate of 0.5kg per hour for reaction. Turn on the nitrogen gas, and keep the pressure inside the furnace tube slightly positive.

[0028] Step (4): T...

Embodiment 2

[0033] The present invention provides the following technical solutions:.

[0034] Step (1): Lithium hydroxide, boric acid and oxalic acid were weighed at a molar ratio of 1:1:2.10 according to Li:B:C2O4, and were milled for 30 minutes by a ball mill.

[0035] Step (2): Slowly add the three materials in proportion to the stirring tank at room temperature, and slowly add a small amount of pure water, the amount of water accounts for about 4% of the weight of the solid material, and mix the materials evenly.

[0036] Step (3): Turn on the feeder, add the mixed material obtained in step (2) into the feeding bin of the three-stage temperature zone rotary reaction furnace, and send the material into the reaction furnace at a rate of 0.7kg per hour for reaction. Turn on the nitrogen gas, and keep the pressure inside the furnace tube slightly positive.

[0037] Step (4): The material passes through the first reaction temperature zone, the temperature is 90°C, the residence time of t...

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Abstract

The invention belongs to the technical field of preparation of lithium borate dioxalate, in particular to a method for continuous preparation of lithium borate dioxalate. The method comprises the following steps that a lithium source compound, a boron source compound and an oxalate containing compound are weighed with the molar ratio of Li:B:C2O4(2-) of 1:1:2.0-1:1:2.2, and ball milling is performed for 30-60 min. A lithium borate complex is a novel lithium ion battery electrolyte, wherein LiBOB is the most representative; lithium borate dioxalate is a coordination chelate, formed electrolytehas much negative ion, the lattice energy is very small, and more ions can be obtained from the solvent to improve the electric conductivity of the electrolyte; the LiBOB has good electrochemical stability and thermal stability, and can react with specific solvents to form a stable SEI film. Compared with a traditional batch synthesis method for lithium borate dioxalate, the method for continuouspreparation of lithium borate dioxalate is more conducive to the realization of industrialization, and the method is economical, environmentally friendly and low in energy consumption.

Description

technical field [0001] The invention belongs to the technical field of preparing lithium bisoxalate borate, and in particular relates to a method for continuously preparing lithium bisoxalate borate. Background technique [0002] With the development of microelectronics technology and the increase of miniaturized electronic equipment, lithium batteries can be fully developed and used due to their superior performance. As an important part of batteries, electrolytes have a very important impact on battery performance. At present, the most widely used lithium ion The battery electrolyte is lithium hexafluorophosphate, which has good electrical conductivity and electrochemical stability. However, lithium hexafluorophosphate still has obvious shortcomings such as sensitivity to water, excessive resistance of the SEI film formed at low temperature, and decomposition at 80°C, which lead to its working conditions being severely affected. Large limitations, easy to decompose and pro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F5/02
CPCC07F5/022
Inventor 舒伟锋贾雪枫叶阳李锐张响飞肖遥
Owner HUBEI HONGYUAN PHARMA