Preparation method and preparation device of lithium difluoro(oxalato)borate

A technology of lithium difluorooxalate borate and boron trifluoride, which is applied in chemical instruments and methods, compounds containing elements of group 3/13 of the periodic table, organic chemistry, etc., can solve the problems of low raw material utilization rate, complicated purification process, Problems such as high cost of raw materials, to achieve high product yield, solve the effect of complex purification process and low cost

Inactive Publication Date: 2020-08-14
HAIKE GRP RES INST OF INNOVATION & TECH
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  • Application Information

AI Technical Summary

Problems solved by technology

The advantage of this method is that the raw material is cheap, and does not require a catalyst, and the cost is relatively low, but the disadvantages are that the reaction time is long, generally more than 6 hours, and the products are lithium difluorooxalate borate and lithium tetrafluoroborate. , both are dissolved in purification solvents such as dimethyl carbonate (DMC), and the purification process is complicated
The advantage of this method is that lithium difluorooxalate borate is the only lithium salt in the product, and the purification is relatively simple, but the disadvantage is that the cost of raw materials is high
And both methods all have the problem that raw material utilization rate is low

Method used

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  • Preparation method and preparation device of lithium difluoro(oxalato)borate

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preparation example Construction

[0035] The invention provides a kind of preparation method of lithium difluorooxalate borate, comprising the steps of:

[0036] 1) Mix boron trifluoride complex, solvent and lithium oxalate, and react at 40-110°C for 2-12 hours to obtain a reaction solution containing lithium tetrafluoroborate and lithium difluorooxalate borate;

[0037] 2) The reaction solution containing lithium tetrafluoroborate and lithium difluorooxalate borate obtained in step 1) is subjected to a vacuum distillation until the amount of solvent is reduced by 1 / 3~1 / 2, and the vacuum distillation is completed to obtain primary distillate and primary distillate;

[0038] 3) Condensing and crystallizing the primary distillation residual liquid obtained in the step 2) to obtain primary crude difluorooxalate lithium borate;

[0039] 4) Mix the primary distillate obtained in step 2) with oxalic acid and a catalyst, react at 35-110°C for 4-8 hours, and then carry out secondary vacuum distillation until the prim...

Embodiment 1

[0065] (1) Open the 2# and 11# valves, add DMC to the constant temperature reactor, the amount added is 1 / 3 of the reactor volume; open the 7# valve, turn on the condensation reflux device, and add BF from the liquid feeding port 2# 3 ·O(CH 2 CH 3 ) 2 (DMC and BF 3 ·O(CH 2 CH 3 ) 2 The molar ratio is 1:2), after stirring, close the 11# valve.

[0066] (2) Open the 1# valve of the solid feeding port, and add Li to the mixed solution 2 C 2 o 4 After closing the valve, its BF 3 ·O(CH 2 CH 3 ) 2 The molar ratio was 1:2; the temperature was raised to 100°C, and the reaction was heated under reflux for 6h.

[0067] (3) Close the 7# valve and the condensing reflux device, open the 8# and 9# valves, start the vacuum distillation device (vacuum degree is 100mbar), keep the constant temperature reactor state until the amount of solvent collected in the solvent condenser reaches the added amount 1 / 3, close the 8#, 9# valves and the vacuum distillation device; open the 7#, 4...

Embodiment 2

[0075] (1) Open the 2# and 11# valves, add DMC to the constant temperature reactor, the amount added is 1 / 3 of the reactor volume; open the 7# valve, turn on the condensation reflux device, and add BF from the liquid feeding port 2# 3 ·DMC (DMC and BF 3 ·The molar ratio of DMC is 1:2), after stirring, close the 11# valve.

[0076] (2) Open the 1# valve of the solid feeding port, and add Li to the mixed solution 2 C 2 o 4 After closing the valve, its BF 3 ·The molar ratio of DMC was 1:3; the temperature was raised to 60°C, and the reaction was heated under reflux for 12 hours.

[0077] (3) Close the 7# valve and the condensing reflux device, open the 8# and 9# valves, start the vacuum distillation device (vacuum degree is 300mbar), keep the constant temperature reactor state until the amount of solvent collected in the solvent condenser reaches the amount added 1 / 2, close 8#, 9# valves and vacuum distillation devices; open 7#, 4# and 6# valves, open the condensation reflux d...

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Abstract

The invention discloses a preparation method and a preparation device of lithium difluoro(oxalato)borate, and belongs to the technical field of lithium ion battery electrolyte. The method comprises the following steps: 1) mixing a boron trifluoride complex, a solvent and lithium oxalate, and reacting at 40-110 DEG C for 2-12 hours; 2) carrying out primary vacuum distillation on the reaction liquidcontaining lithium tetrafluoroborate and lithium difluoro(oxalato)borate until the solvent amount is reduced by 1 / 3-1 / 2; 3) condensing and crystallizing the obtained primary distillation residual liquid; 4) mixing the primary distillate with oxalic acid and a catalyst, reacting at 35-110 DEG C for 4-8 hours, carrying out secondary vacuum distillation, and distilling until the primary distillate is reduced by 1 / 3-1 / 2; 5) condensing and crystallizing the secondary distillation residual liquid, and 6) recrystallizing a primary crude product and a secondary crude product of lithium difluoro(oxalato)borate to obtain lithium difluoro(oxalato)borate. The method provided by the invention can reduce side reactions and the number of times of recrystallization, and has the advantages of high yield and high raw material utilization rate.

Description

technical field [0001] The invention relates to the technical field of lithium ion battery electrolyte, in particular to a preparation method and a preparation device of lithium difluorooxalate borate. Background technique [0002] Lithium-ion batteries have the characteristics of high energy density, long cycle life and no pollution, so they are widely used in various electrical appliances and electric equipment. Electrolyte is one of the main components of lithium-ion batteries and one of the key materials affecting the performance of lithium-ion batteries. The current research on new lithium salts mainly focuses on lithium borate complexes and lithium phosphate complexes, among which lithium difluorooxalate borate (LiODFB) attracts the most attention. Its unique chemical structure makes it combine the advantages of lithium bisoxalate borate and lithium tetrafluoroborate, so that it has good high and low temperature performance, rate performance and cycle performance at t...

Claims

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Application Information

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IPC IPC(8): C07F5/02
CPCC07F5/025
Inventor 张在忠鞠署元苗力孝李宏亮王明华牛庆荣张琪
Owner HAIKE GRP RES INST OF INNOVATION & TECH
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