Method of preparing waterless lithium terafluoroborate

A technology of lithium tetrafluoroborate and tetrafluoroborate, which is applied in the directions of tetrafluoroborate and boron halide compounds, can solve the problems of reducing the purity of lithium tetrafluoroborate, affecting the effect of dehydration, and increasing costs, achieving complete crystal form and improving The effect of purity, low preparation cost

Inactive Publication Date: 2010-03-10
QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method does not use boron trifluoride, and the amount of hydrogen fluoride used is small, and basically enters into the product. Therefore, the raw materials of this method are easy to obtain, and the primary lithium salt product of the salt lake can be used. The cost is low, and the production process has low energy consumption. Environmentally friendly, but it is easy to cause solid melting and wrapping during the drying process, which affects the dehydration effect and reduces the purity of the synthesized lithium tetrafluoroborate, and because a large amount of ethanol is used as the extraction agent, it has certain pollution to the environment, and Increased the cost of production, so this method has not been used in actual production

Method used

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  • Method of preparing waterless lithium terafluoroborate
  • Method of preparing waterless lithium terafluoroborate
  • Method of preparing waterless lithium terafluoroborate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Weigh the mass fraction to be about 40% (the analytically pure hydrofluoric acid purchased is calibrated by the national standard GB620-93, and its mass fraction is about 40.87%. When hydrofluoric acid is used in foreign literature, it is generally said that the mass fraction is 48% %, the same below), put 209g of hydrogen fluoride aqueous solution into an ice bath, and stir with a magnetic stirrer. After 10 minutes, slowly add 66.1g of boric acid, and finish adding in about 50 minutes. Continue to stir for 30 minutes after the addition, then slowly add 40.6g of lithium carbonate to the above mixed solution, finish adding in about 30 minutes, filter, and concentrate the filtrate under an infrared lamp to make the content of lithium tetrafluoroborate about 70% . Put the concentrated solution in a constant temperature water bath at about 40°C, filter it after 12 hours, and return the filtrate to the mother liquor. Dissolve the solid phase with an appropriate amount of di...

Embodiment 2

[0023] Weigh 104.4g of hydrogen fluoride aqueous solution with a mass fraction of about 40%, put it in an ice bath, and stir it with a magnetic stirrer. After 10 minutes, slowly add 33g of boric acid, and finish adding in about 50 minutes. Continue to stir for 30 minutes after adding, then slowly add 20.3g of lithium carbonate to the above mixed solution, finish adding in about 30 minutes, filter, and concentrate the filtrate under an infrared lamp to make the content of lithium tetrafluoroborate about 70% . Put the concentrated solution in a constant temperature water bath at about 5°C, filter after 2 hours, and return the filtrate to the mother liquor. The solid phase was placed in a vacuum oven. Dry at about 50°C and 560mmHg for 5 hours, then raise the temperature to about 80°C, continue to dry for 5 hours, take the solid out of the vacuum drying oven, grind it, and then put it in the vacuum drying oven again, and dry it at about 140°C and 560mmHg for 10 hours hour, the w...

Embodiment 3

[0025] Weigh 105g of hydrogen fluoride aqueous solution with a mass fraction of about 40%, put it in an ice bath, and stir with a magnetic stirrer. After 10 minutes, slowly add 33g of boric acid, and finish adding in about 50 minutes. Stirring was continued for 30 minutes after the addition, and then 20.9gLiOH·H 2 O was slowly added to the above mixed solution, and the addition was completed in about 30 minutes, filtered, and the filtrate was concentrated under an infrared lamp, so that the content of lithium tetrafluoroborate was about 70%. Put the concentrated solution in a constant temperature water bath at about 40°C, filter it after 12 hours, and return the filtrate to the mother liquor. Dissolve the solid phase with an appropriate amount of distilled water to completely dissolve the crystals, and place the solution again in a constant temperature water bath at about 30°C. Filter after 72 hours, return the filtrate to the mother liquor, and put the solid phase into a vac...

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Abstract

The invention relates to a method for preparing an anhydrous lithium tetrafluoroborate which comprises the following steps: a lithium source including lithium hydroxide, lithium carbonate, and the like, reacts with fluorine hydride and boric acid to obtain lithium tetrafluoroborate solution, then the lithium tetrafluoroborate solution is condensed, crystallized and recrystallized, ground, and vacuum dried to obtain the anhydrous lithium tetrafluoroborate. The method of the invention adopts a staged temperature rise control, the process of the preparation is simple, raw materials are cheap andthe preparation cost is low, no organic solvent is used during the synthetic process, no poison is produced, therefore, the method accords with the concept of green environmental protection, the anhydrous lithium tetrafluoroborate prepared by the method is determined by a X-ray diffraction map, the diffraction peak is clear and sharp and completely matches the standard card, which shows that the product prepared by the method of the invention is anhydrous LiBF4 with complete crystal form, the quality of the product is equal to the quality of the anhydrous lithium tetrafluoroborate prepared bythe reaction of lithium fluoride and boron trifluoride.

Description

technical field [0001] The invention belongs to the field of chemical industry, and relates to the preparation of a lithium salt, in particular to a preparation method of anhydrous lithium tetrafluoroborate for lithium ion battery electrolyte. Background technique [0002] The electrolyte solution is an important part of the lithium-ion battery, which plays the role of transporting ions and conducting current between the positive and negative electrodes, and is an indispensable part to complete the electrochemical reaction. Selecting a suitable electrolyte is also the key to obtaining lithium-ion batteries with high energy density and power density, long cycle life and good safety performance. Its performance directly affects the optimization and improvement of the performance of lithium-ion batteries. The lithium salt used in lithium-ion batteries is generally LiPF 6 、LiBF 4 , LiClO 4 , LiAsF 6 、LiCF 3 SO 3 , LiN(CF 3 SO 2 ) 2 or LiC(CF 3 SO 2 ) 3 and other subs...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01B35/06
CPCC01B35/066
Inventor 周园张昕岳邓小宇乌志明曹国进
Owner QINGHAI INST OF SALT LAKES OF CHINESE ACAD OF SCI
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