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Preparation method of high-purity lithium bis(oxalato)borate

A lithium bis-oxalate borate and high-purity technology is applied in the field of preparation of high-purity lithium bis-oxalate borate, and can solve the problems of difficulty in obtaining raw materials for synthesis routes, difficulty in industrial production, and low synthesis efficiency.

Pending Publication Date: 2021-05-18
湖南埃迪特威新材料有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The disadvantage is that the raw materials of the synthetic route are difficult to obtain, the cost is high, and it is not suitable for industrial production; while the Chinese patent CN200510011555.7 uses a solid-phase method to synthesize LiBOB, but this method has the disadvantages of low synthesis efficiency and difficult industrial production

Method used

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  • Preparation method of high-purity lithium bis(oxalato)borate

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Embodiment 1

[0039] A preparation method of high-purity lithium bisoxalate borate comprises the following specific steps:

[0040] S1 ball milling: uniformly mix anhydrous oxalate and boron in a molar ratio of 2:1, put them into a ball mill and mill for 0.5h, then dissolve the mixed powder into ultrapure water at a mass ratio of 1:20 to obtain solution A;

[0041] S2 Dissolving: Lithium powder is dissolved in ethylene carbonate according to the mass ratio of 1:10 to obtain solution B;

[0042] S3 cycle heating; put the A liquid and B obtained in steps S1 and S2 into the tubular reactor according to the mass ratio of 1:2 for heating reaction, the reaction temperature is 60 ° C; micro-negative pressure reaction, the pressure is -0.001Mpa; The moisture generated under negative pressure forms an azeotrope with diethyl carbonate at high temperature and is discharged out of the system under negative pressure; diethyl carbonate and water are separated in the static tank, and diethyl carbonate is ...

Embodiment 2

[0050] A preparation method of high-purity lithium bisoxalate borate comprises the following specific steps:

[0051] S1 ball milling: uniformly mix anhydrous oxalate and boron in a molar ratio of 3.5:1, put them into a ball mill for 1 hour, and then dissolve the mixed powder into ultrapure water at a mass ratio of 1:30 to obtain solution A;

[0052] S2 dissolution: Lithium powder is dissolved in ethylene carbonate according to the mass ratio of 1:15 to obtain solution B;

[0053] S3 cycle heating; put the A liquid and B obtained in steps S1 and S2 into the tubular reactor according to the mass ratio of 1:3 for heating reaction, the reaction temperature is 68 ° C; micro-negative pressure reaction, the pressure is -0.001Mpa; The moisture generated under negative pressure forms an azeotrope with diethyl carbonate at high temperature and is discharged out of the system under negative pressure; diethyl carbonate and water are separated in the static tank, and diethyl carbonate is ...

Embodiment 3

[0061] A preparation method of high-purity lithium bisoxalate borate comprises the following specific steps:

[0062] S1 ball milling: uniformly mix anhydrous oxalate and boron in a molar ratio of 5:1, put them into a ball mill and mill for 1.5 hours, then dissolve the mixed powder into ultrapure water at a mass ratio of 1:50 to obtain solution A;

[0063] S2 Dissolving: Lithium powder is dissolved in ethylene carbonate according to the mass ratio of 1:20 to obtain solution B;

[0064] S3 cycle heating; put the A liquid and B obtained in steps S1 and S2 into the tubular reactor according to the mass ratio of 1:5 for heating reaction, the reaction temperature is 75 °C; slight negative pressure reaction, the pressure is -0.001Mpa; The moisture generated under negative pressure forms an azeotrope with diethyl carbonate at high temperature and is discharged out of the system under negative pressure; diethyl carbonate and water are separated in the static tank, and diethyl carbonat...

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Abstract

The invention discloses a preparation method of high-purity lithium bis(oxalato)borate. The high-purity lithium bis(oxalato)borate is obtained through the steps of S1 ball milling, S2 dissolution, S3 cyclic heating, S4 low-temperature reduced pressure evaporation, S5 vacuum drying, S6 redissolution, S7 suction filtration, S8 crystallization, S9 recrystallization and the like in sequence. The preparation method is few in step, mild in condition and low in equipment requirement, and the final product is low in water content, high in yield and high in purity and can meet the production requirement of lithium ion battery electrolyte.

Description

technical field [0001] The invention belongs to the field of lithium battery electrolyte preparation, and specifically discloses a preparation method of high-purity lithium bisoxalate borate. Background technique [0002] "Lithium battery" is a type of battery that uses lithium metal or lithium alloy as the positive / negative electrode material and uses a non-aqueous electrolyte solution. In 1912, the lithium metal battery was first proposed and studied by Gilbert N. Lewis. In the 1970s, M.S.Whittingham proposed and began to study lithium-ion batteries. Due to the very active chemical properties of lithium metal, the processing, storage and use of lithium metal have very high environmental requirements. With the development of science and technology, lithium batteries have become the mainstream. With the continuous expansion of the use of lithium-ion batteries, the technology of lithium-ion batteries is also improving. Adding some additives to the electrolyte as the "blood...

Claims

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Application Information

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IPC IPC(8): C07F5/02H01M10/0567
CPCC07F5/022H01M10/0567H01M2300/0025Y02E60/10
Inventor 刘晨晖
Owner 湖南埃迪特威新材料有限公司
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