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Method for preparing anhydrous high-purity lithium tetrafluoroborate

A technology of high-purity lithium tetrafluoroborate and lithium tetrafluoroborate, which is applied in the field of lithium-ion batteries, can solve problems such as low production efficiency, uneven reaction, and performance degradation of electrolyte materials, and achieve low moisture content, high product purity, and production The effect of cost reduction

Inactive Publication Date: 2010-10-20
CHINA NAT OFFSHORE OIL CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The conventional preparation methods of lithium tetrafluoroborate include aqueous solution method, solid phase-gas phase contact method, and non-aqueous solution method, etc. The solid phase-gas phase contact method requires high equipment, strict control of the process, uneven reaction, and low production efficiency. , and in the process of synthesizing lithium tetrafluoroborate by the aqueous solution method, since lithium tetrafluoroborate appears in the form of monohydrate or trihydrate in the aqueous solution, it is very difficult to remove water after subsequent drying, which reduces the overall performance of the electrolyte material. Finally, it affects the capacity and cycle life of lithium-ion batteries

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] First, 63.09g of industrial boric acid with a purity of 98% and SO 3 Content is 9% oleum is mixed, and oleum is excessive 300%, obtains the mixed acid solution containing boron, then adds the calcium fluoride of 118.30g, then heats up to 80 ℃, controls reaction temperature at 83 ℃, obtains High-purity gaseous boron trifluoride (BF 3 ), using a compressor to press the obtained boron trifluoride gas into ethyl acetate containing 26.20 g of lithium fluoride for contact reaction, the reaction time is 5 hours, until the suspension is clear, the reaction solution is reduced at 70 ° C Pressure distillation and crystallization to obtain a wet product of lithium tetrafluoroborate. The wet product of lithium tetrafluoroborate was washed and purified with ether, and the obtained product was dried at 60°C for 6 hours, and then vacuum-dried at 100°C for 10 hours to obtain a white powder anhydrous high-purity lithium tetrafluoroborate.

Embodiment 2

[0030] First, 62.45g of industrial boric acid with a purity of 99% and SO 3 Content is 15% oleum mixed, and oleum excess 200%, obtains the boron-containing mixed acid solution, then feeds 20.01g of hydrogen fluoride gas, then heats up to 80°C, controls the reaction temperature at 90°C, and obtains High-purity gaseous boron trifluoride (BF 3 ), using a compressor to press the obtained boron trifluoride gas into ethyl acetate containing 26.00 g of lithium fluoride for contact reaction, the reaction time is 7 hours, until the suspension is clear, the reaction solution is reduced at 65 ° C Distillation and crystallization under pressure to obtain a wet product of lithium tetrafluoroborate. The wet product of lithium tetrafluoroborate was washed and purified with dimethyl carbonate, and the obtained product was dried at 70°C for 4 hours, and then vacuum-dried at 150°C for 7 hours to obtain Anhydrous high-purity lithium tetrafluoroborate in the form of white powder.

Embodiment 3

[0032] First, 62.14g of industrial boric acid with a purity of 99.5% and SO 3 Content is 20% oleum mixed, and oleum excess 150%, obtains the boron-containing mixed acid solution, then adds 42.85g of sodium fluoride, then heats up to 80 ℃, controls the reaction temperature at 76 ℃, obtains High-purity gaseous boron trifluoride (BF 3 ), using a compressor to press the obtained boron trifluoride gas into ethyl acetate containing 26.47g of lithium fluoride for contact reaction, the reaction time is 5 hours, until the suspension is clear, the reaction solution is reduced at 60°C Pressure distillation and crystallization to obtain a wet product of lithium tetrafluoroborate. The wet product of lithium tetrafluoroborate was washed and purified with tetrahydrofuran, and the obtained product was dried at 80°C for 2 hours, and then vacuum-dried at 120°C for 8 hours to obtain a white powder anhydrous high-purity lithium tetrafluoroborate.

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Abstract

The invention discloses a method for preparing anhydrous high-purity lithium tetrafluoroborate, which is characterized by comprising the following steps of: mixing 1 to 3mol of 98 to 99.55 percent of industrial boric acid and 2.5 to 12mol of excessive 150 to 300 percent fuming sulfuric acid with 9 to 20 percent of SO3 to obtain boron-containing mixed acid solution, adding 1 to 3mol of fluorine-containing compound into the boron-containing mixed acid solution, heating the solution to 80 DEG C to obtain high-purity gaseous boron trifluoride (BF3), compressing the obtained boron trifluoride gas into lithium fluoride-containing ethyl acetate by using a compressor to perform contact reaction for 2 to 7 hours till the suspension is clarified, distilling and crystallizing the reaction solution at the temperature of between 60 and 70 DEG C under reduced pressure to obtain a wet lithium tetrafluoroborate product, washing and purifying the wet lithium tetrafluoroborate product by using washing and purifying agents, and drying the product to obtain the anhydrous high-purity lithium tetrafluoroborate.

Description

technical field [0001] The invention relates to the field of lithium ion batteries, and relates to a preparation method of lithium tetrafluoroborate, a novel electrolyte material for lithium ion batteries. technical background [0002] The voltage of lithium-ion batteries is 3.6 volts, about three times that of nickel-cadmium batteries and nickel-hydrogen batteries, and the energy density per unit volume and unit weight is high. In addition, electronic devices using lithium-ion batteries can also be further miniaturized and lightweight direction development. Lithium-ion batteries, as latecomers, are largely replacing nickel-cadmium and nickel-metal hydride batteries in portable electronic devices. Lithium-ion batteries have become the mainstream of the future development of small secondary batteries. [0003] Lithium salts used in lithium-ion battery electrolytes are generally divided into lithium perchlorate (LiClO 4 ), lithium tetrafluoroborate (LiBF 4 ), lithium hexaf...

Claims

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Application Information

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IPC IPC(8): C01B35/12H01M10/056
CPCY02E60/10
Inventor 宁延生郭西凤许寒赵庆云孙新华
Owner CHINA NAT OFFSHORE OIL CORP
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