Catalytic synthesis method of lithium tetrafluoroborate

A technology of lithium tetrafluoroborate and a synthesis method, which is applied in the fields of new energy material preparation and chemical industry, can solve the problems of reducing the purity of lithium tetrafluoroborate, low yield of lithium tetrafluoroborate, and high cost of high-purity lithium fluoride, and achieves the convenience of The effect of industrialization, reduction of production cost and easy operation

Inactive Publication Date: 2017-01-18
LUOYANG HEMENG TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Patent CN103236562A discloses a method of preparing lithium tetrafluoroborate by passing CO2 through lithium carbonate suspension, mixing with anhydrous hydrofluoric acid and adding boric acid solution to react to prepare lithium tetrafluoroborate. This method has simple process, low cost and time-consuming Short, but in the drying process of this method, it is easy to cause overheating due to solid melting and wrapping, which reduces the purity of lithium tetrafluoroborate, and the drying time is short, which affect

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] 1. First, replace all the production reaction vessels with high-purity nitrogen, then pass in high-purity nitrogen, and add materials under the protection of high-purity nitrogen;

[0031] 2. Add 42.39 kilograms of anhydrous lithium chloride and 110 kilograms of anhydrous sodium tetrafluoroborate after drying into a 1000-liter stainless steel stirring reactor equipped with 300 kilograms of dimethyl carbonate, and stir to dissolve;

[0032] 3. Then add 0.7 kg of 1,8-diazabicyclo[5.4.0]undec-7-ene into the stirred reactor as a catalyst; heat while stirring, control the reaction temperature to 60°C, fully 6 hours of reaction;

[0033] 4. Filter the insoluble by-product sodium chloride through a filter press to obtain a dimethyl carbonate filtrate containing lithium tetrafluoroborate;

[0034] 5. Evaporate the dimethyl carbonate filtrate containing lithium tetrafluoroborate until the filtrate is stopped until white solid particles are formed, then lower the temperature to ...

Embodiment 2

[0036] 1. First, replace all the production reaction vessels with high-purity nitrogen, then pass in high-purity nitrogen, and add materials under the protection of high-purity nitrogen;

[0037]2. Add 42.39 kilograms of anhydrous lithium chloride and 111 kilograms of anhydrous sodium tetrafluoroborate after drying into a 1000-liter stainless steel stirring reactor equipped with 300 kilograms of dimethyl carbonate, and stir to dissolve;

[0038] 3. Then add 0.8 kg of 1,5-diazabicyclo[4,3,0]nonene-5 into the stirred reactor as a catalyst; heat while stirring, control the reaction temperature to 70°C, and fully react 7 hours;

[0039] 4. Filter the insoluble by-product sodium chloride through a filter press to obtain a dimethyl carbonate filtrate containing lithium tetrafluoroborate;

[0040] 5. Evaporate the dimethyl carbonate filtrate containing lithium tetrafluoroborate until the filtrate is stopped until white solid particles are formed, then lower the temperature to crysta...

Embodiment 3

[0042] 1. First, replace all the production reaction vessels with high-purity nitrogen, then pass in high-purity nitrogen, and add materials under the protection of high-purity nitrogen;

[0043] 2. Add 42.39 kilograms of anhydrous lithium chloride and 105 kilograms of anhydrous ammonium tetrafluoroborate after drying into a 1000-liter stainless steel stirring reactor equipped with 300 kilograms of dimethyl carbonate, and stir to dissolve;

[0044] 3. Then add 0.7 kg of 1,5-diazabicyclo[4,3,0]nonene-5 into the stirred reactor as a catalyst; heat while stirring, control the reaction temperature to 70°C, and fully react 7 hours;

[0045] 4. Filter the insoluble by-product ammonium chloride through a filter press to obtain a dimethyl carbonate filtrate containing lithium tetrafluoroborate;

[0046] 5. Evaporate the dimethyl carbonate filtrate containing lithium tetrafluoroborate until the filtrate is stopped until white solid particles are formed, then lower the temperature to c...

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PUM

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Abstract

The invention relates to a catalytic synthesis method of lithium tetrafluoroborate and belongs to the technical field of new energy material preparation. The method comprises the specific steps that 1, all production reaction vessels are subjected to high-purity nitrogen displacement and then put under the protection of high-purity nitrogen, and materials are added; 2, dry quantitative anhydrous tetrafluoroborate and quantitative anhydrous lithium chloride are added into an organic solvent in a stirring reactor to be dissolved, and a solution is prepared; 3, a quantitative catalyst is added into the stirring reactor, and heating and stirring are carried out at specified temperature for a sufficient reaction of the materials; 4, after the reaction is completed, filtering is conducted, solid byproducts are separated, and an organic solution of lithium tetrafluoroborate is obtained; 5, the organic solution of lithium tetrafluoroborate is concentrated, the organic solvent is separated, and high-purity lithium tetrafluoroborate crystals are obtained after recrystallization purification and vacuum drying. The catalytic synthesis method of lithium tetrafluoroborate is safe, simple, high in yield and good in quality, simplifies the technological process and has good application prospects in the field of new energy materials.

Description

technical field [0001] The invention relates to a catalytic synthesis method of lithium tetrafluoroborate, belonging to the technical fields of new energy material preparation and chemical industry. Background technique [0002] In recent years, lithium-ion batteries have been widely used in electronic communication fields such as mobile phones, notebook computers, and digital cameras, and have occupied a dominant position. With the rapid growth of electric bicycles and new energy vehicles, the application of lithium-ion batteries has become a research hotspot all over the world. [0003] Electrolyte is one of the four key materials of lithium-ion batteries. It is the "blood" of lithium-ion batteries. Electrolyte is responsible for the transmission of charges between the positive and negative electrodes in the battery. Overfill, inflation, stability, cycle efficiency and safety performance are very important. Therefore, in order to improve the safety of the battery, the de...

Claims

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Application Information

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IPC IPC(8): C01B35/06H01M10/0563H01M10/0525
CPCC01B35/066H01M10/0525H01M10/0563Y02E60/10
Inventor 李绍通
Owner LUOYANG HEMENG TECH CO LTD
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