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Method for preparing lithium tetrafluoroborate

A technology of lithium tetrafluoroborate and fluoroboric acid, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as harsh operating conditions, difficult control, and high process risk, and is beneficial to industrial production and reduces equipment costs. Difficulty, the smooth effect of the reaction process

Inactive Publication Date: 2018-05-18
顾飞
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Lithium tetrafluoroborate, the appearance is white or yellowish fluid powder, the melting point is 293-300 ℃, easy to absorb water, stable chemical properties, can be used as a primary lithium battery (pacemaker battery, lithium manganese battery, etc.) or secondary Lithium-ion battery electrolyte conductive salt can improve the high temperature, low temperature and battery safety performance of the battery, and also has excellent passivation ability to aluminum foil, which can be used as a film-forming additive, but lithium tetrafluoroborate alone as the electrolyte salt has great big limitations
[0004] At present, there are few researches on the preparation of lithium tetrafluoroborate in China. The existing Chinese patent CN104692405A discloses a preparation method of lithium tetrafluoroborate, which uses hydrofluoric acid as a solvent, and the preparation process requires high process equipment. , the risk of the process is high, and the reaction is not easy to control; in addition, it needs to be concentrated in a vacuum state, and the operating conditions are relatively harsh; Chinese patent CN104326482A also discloses a method for preparing lithium tetrafluoroborate, first preparing lithium metaborate, Mixing reaction with ammonium fluoride or ammonium bifluoride also needs to be carried out under vacuum conditions. This method is not only harsh, but also the reaction is extremely unstable and difficult to control. Purification is extremely complicated, which is not conducive to ensuring the quality of the product and is not conducive to industrialization

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] A method for rapidly preparing lithium tetrafluorophosphate, the specific steps are as follows:

[0022] (1) Synthesis:

[0023] After mixing the 40% mass concentration of analytically pure fluoboric acid aqueous solution and the 55% mass concentration of hydrogen fluoride aqueous solution according to the mass ratio of 1:0.01, the temperature was raised to 40 ° C; the method of continuous feeding was added to the mixed solution Solid powder lithium carbonate, the add-on of lithium carbonate is to ensure that the mass ratio of mixed solution and lithium carbonate is 1:0.16; Control the feeding time of lithium carbonate to be 3h, react 1h after feeding;

[0024] (2) Concentration:

[0025] The mixture obtained in step (1) is heated to 110°C for concentration, and when the mixture is concentrated to 1 / 3 to 1 / 4 of its original volume, the mother liquor is released, cooled and crystallized under normal temperature industrial water, and finally centrifuged to obtain a water...

Embodiment 2

[0031] A method for rapidly preparing lithium tetrafluorophosphate, the specific steps are as follows:

[0032] (1) Synthesis:

[0033] After mixing the 40% mass concentration of analytically pure fluoboric acid aqueous solution and the 55% mass concentration of hydrogen fluoride aqueous solution according to the mass ratio of 1:0.05, the temperature was raised to 50 ° C; the method of continuous feeding was added to the mixed solution Solid powder lithium carbonate, the add-on of lithium carbonate is to ensure that the mass ratio of mixed solution and lithium carbonate is 1:0.19; Control the feeding time of lithium carbonate to be 6h, react 2h after feeding;

[0034] (2) Concentration:

[0035] The mixture obtained in step (1) is heated to 150°C for concentration, and when the mixture is concentrated to 1 / 3 to 1 / 4 of its original volume, the mother liquor is released, cooled and crystallized under normal temperature industrial water, and finally centrifuged to obtain a water...

Embodiment 3

[0041] A method for rapidly preparing lithium tetrafluorophosphate, the specific steps are as follows:

[0042] (1) Synthesis:

[0043] After mixing the 40% mass concentration of analytically pure fluoboric acid aqueous solution and the 55% mass concentration of hydrogen fluoride aqueous solution according to the mass ratio of 1:0.02, the temperature was raised to 60 ° C; the method of continuous feeding was added to the mixed solution Solid powdery lithium carbonate, the add-on of lithium carbonate is to ensure that the mass ratio of mixed solution and lithium carbonate is 1:0.17; Control the feeding time of lithium carbonate to be 4h, react 1h after feeding;

[0044] (2) Concentration:

[0045] The mixture obtained in step (1) is heated to 120°C for concentration, and when the mixture is concentrated to 1 / 3 to 1 / 4 of its original volume, the mother liquor is released, cooled and crystallized under normal temperature industrial water, and finally centrifuged to obtain a wate...

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Abstract

The invention relates to a method for preparing lithium tetrafluoroborate. The method comprises (1) synthesis: uniformly mixing a fluoboric acid aqueous solution and a hydrogen fluoride aqueous solution, heating the mixed solution, adding solid powdery lithium carbonate into the mixture and carrying out a reaction process for 1 to 2 hours, (2) concentration: heating to concentrate the mixture, andcentrifuging the concentrate to obtain lithium tetrafluoroborate crystals with water content of 20-30%, (3) drying: putting the lithium tetrafluoroborate crystals into a rotary dryer and drying the lithium tetrafluoroborate crystals to obtain crude lithium tetrafluoroborate, and (4) purification. The method uses an aqueous solution as a medium, reduces the difficulty of the equipment and the danger of the production process, is stable and does not produce side reactions and by-products in the process. The prepared lithium tetrafluoroborate has high purity and the quality level reaching to thehigh purity level.

Description

technical field [0001] The invention relates to a preparation method of lithium tetrafluoroborate. Background technique [0002] Lithium-ion battery, as an environmentally friendly and clean energy, has become the main battery of electric vehicles in the 21st century together with fuel cells. The broad development prospects of lithium-ion batteries have brought huge development space for the lithium-ion battery material industry. The inorganic electrolyte salts used in lithium-ion batteries mainly include LiPF6, LiCLO4, LiAsF6, LiBOB, LiBF4, etc. Among them, the LiPF6 electrolyte system has the advantages of high conductivity and high electrochemical stability, and has become the main electrolyte in the field of lithium-ion batteries. product. However, LiPF6 electrolyte is easy to decompose when exposed to water, and its thermal stability is poor, so it is difficult to meet the needs of high-performance lithium-ion batteries. Lithium tetrafluoroborate, with its advantages ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455
CPCC01B25/455C01P2006/80
Inventor 顾飞
Owner 顾飞