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Method of preparing waterless lithium terafluoroborate

A technology of lithium tetrafluoroborate and tetrafluoroborate, which is applied to the preparation of lithium ion battery electrolyte anhydrous lithium tetrafluoroborate and the preparation of lithium salt, can solve the problem of reducing the purity of lithium tetrafluoroborate, affecting the effect of dehydration, and increasing cost and other problems, to achieve the effect of complete crystal form, improved purity and low preparation cost

Inactive Publication Date: 2008-12-10
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% (using the national standard GB620-93 method to calibrate the purchased analytical pure hydrofluoric acid, its mass fraction is about 40.87%, and the mass fraction of hydrofluoric acid is generally said to be 48 when using hydrofluoric acid in foreign literature. %, the same below) 209g of hydrogen fluoride aqueous solution was placed in an ice bath and stirred with a magnetic stirrer. After 10 minutes, 66.1g of boric acid was slowly added and the addition was completed in about 50 minutes. After the addition, continue to stir for 30 minutes, then slowly add 40.6g of lithium carbonate to the above mixed solution, add 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. The solid phase is dissolve...

Embodiment 2

[0023] Weigh 104.4 g 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 33 g of boric acid and complete the addition in about 50 minutes. After the addition, continue to stir for 30 minutes, then slowly add 20.3g of lithium carbonate to the above mixed solution, add 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 is placed in a vacuum drying oven. Dry for 5 hours at about 50°C and 560mmHg, then heat to about 80°C, continue drying for 5 hours, remove the solid from the vacuum drying oven, grind, and then put it in the vacuum drying oven again, and dry at about 140°C and 560mmHg for 10 Within hours, white powdery anhydrous...

Embodiment 3

[0025] Weigh 105 g 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 33 g of boric acid and complete the addition in about 50 minutes. After adding, continue to stir for 30 minutes, then add 20.9gLiOH·H 2 O was slowly added to the above mixed solution, 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. The solid phase is dissolved with an appropriate amount of distilled water to dissolve the crystals exactly, and the solution is again placed in a constant temperature water bath at about 30°C. After 72 hours, it is filtered, the filtrate is returned to the mother liquor, and the solid phase is plac...

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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 and the 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 by the reaction of lithium fluoride and boron trifluoride.

Description

Technical field [0001] The invention belongs to the field of chemical engineering, and relates to a preparation method of lithium salt, in particular to a preparation method of anhydrous lithium tetrafluoroborate electrolyte of a lithium ion battery. Background technique [0002] Electrolyte solution is an important part of lithium ion battery, which plays a role in transporting ions and conducting current between the positive and negative electrodes, and is an indispensable part of completing the electrochemical reaction. Choosing a suitable electrolyte is also the key to obtaining a lithium-ion battery 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 the lithium-ion battery. 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 substances. When th...

Claims

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Application Information

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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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