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Preparation method of lithium difluoro(oxalato)borate

A technology of difluorooxalate lithium borate and lithium oxalate, which is applied in chemical instruments and methods, compounds containing elements of group 3/13 of the periodic table, organic chemistry, etc., can solve the problems of using many types of solvents and complex reactions, etc., and achieve Overcoming the effects of many reaction steps, simple preparation method and cost saving

Inactive Publication Date: 2016-03-16
CNOOC TIANJIN CHEM RES & DESIGN INST +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the reaction of this method is complicated, and there are too many types of solvents

Method used

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  • Preparation method of lithium difluoro(oxalato)borate
  • Preparation method of lithium difluoro(oxalato)borate
  • Preparation method of lithium difluoro(oxalato)borate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Example 1: At room temperature, add 101.9g of lithium oxalate and 1300g of HF into a fluorine-lined reaction vessel with a jacket, and stir until the lithium oxalate is completely dissolved in HF. then BF 3 143.02g of gas was slowly passed into the reactor, and the gas export rate was controlled at 2L / Min. During the process, attention was paid to the temperature change at all times, and the temperature was controlled at about 30°C. After the gas was introduced, the stirring was continued for 4 hours. After filtration, 300.12 g of the product was obtained by evaporation and crystallization, and 254.13 g of the crude product were obtained after rapid drying (drying under vacuum for 1 hour, then heating up to 80° C., and drying under vacuum for 3 hours). Finally, the resulting thick product is added to 300gDMC, dissolved and filtered, dried (cold N 2 The temperature was raised to 50°C, and hot N was continuously introduced 2 After three hours, the N 2 After heating up ...

Embodiment 2

[0020] Example 2: At room temperature, 101.9 g of lithium oxalate and 1300 g of HF were added to reaction vessel 1 with a jacket, and stirred until the lithium oxalate was completely dissolved in HF. then BF 3 143.12g of gas was slowly passed into the reactor, and the gas export rate was controlled at 2L / Min. During the process, attention was paid to temperature changes at all times, and the temperature was controlled below 30°C. After the gas was introduced, the stirring was continued for 4 hours. After filtration, 298.34 g of crude product was obtained by evaporation and crystallization, and 250.12 g of crude product was obtained after rapid drying. Finally, add 300 g of diethyl ether to the obtained crude product, dissolve, filter, and dry to obtain a product quality of 189.27 g, wherein the theoretical yield is 193.79 g, and the product yield reaches 97.66%. The product purity of the obtained product is 99.93%, the water content is 4.8ppm, and the acid content is 20ppm. ...

Embodiment 3

[0023] Example 3: At room temperature, 101.9 g of lithium oxalate and 1300 g of HF were added to reaction vessel 1 with a jacket, and stirred until the lithium oxalate was completely dissolved in HF. then BF 3 144.28g of gas was slowly passed into the reactor, and the gas export rate was controlled at 2L / Min. During the process, attention was paid to the temperature change at all times, and the temperature was controlled at about 40°C. After the gas was introduced, the stirring was continued for 8 hours. After filtration, 301.21 g of the product was obtained by evaporation and crystallization, and 252.27 g of the product were obtained after rapid drying. Finally, add 400g of ethanol to the obtained product, dissolve, filter and dry to obtain a product quality of 187.23g, wherein the theoretical yield is 193.79g, and the product yield reaches 97.61%. The product purity of the obtained product is 99.87%, the water content is 5.2 ppm, and the acid content is 23 ppm.

[0024] Ta...

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Abstract

The invention discloses a preparation method of lithium difluoro(oxalato)borate. The method comprises the following steps: adding lithium oxalate and anhydrous HF to a fluorine lining reaction kettle, and fully stirring to make lithium oxalate be fully dissolved in HF; introducing a boron trifluoride gas to the reaction kettle, controlling the flow velocity of boron trifluoride to be 0.5-2L / min, the reaction temperature to be 0-90DEG C, the reaction pressure to be 0-0.5MPa and the molar ratio of boron trifluoride to lithium oxalate to be 2.2-2:1, continuously stirring and reacting for 2-24h after introduction of the boron trifluoride gas is finished, and evaporating and crystallizing the above obtained reaction product o obtain crude lithium difluoro(oxalato)borate; and fast drying, adding an organic solvent, dissolving, filtering, and drying to obtain the lithium difluoro(oxalato)borate product, wherein the organic solvent adopts one or more of esters, ethers, alcohols and nitriles, the use amount of the organic solvent guarantees that lithium tetrafluoroborate can be completely dissolved in the organic solvent, and lithium difluoro(oxalato)borate cannot be completely dissolved in the organic solvent. The method is simple and practical, and can realize large-scale industrial production of lithium difluoro(oxalato)borate.

Description

technical field [0001] The invention relates to a method for preparing lithium difluorooxalate borate which can be used as an additive for non-aqueous electrolyte of lithium ion battery. Background technique [0002] Lithium difluorooxalate borate is mainly used as an additive for nonaqueous electrolyte batteries such as lithium ion batteries and lithium ion capacitors. After adding this kind of additive, the electrolyte has excellent high and low temperature performance, and can form a more stable SEI film structure on the surface of the negative electrode material of the electrode material, which can significantly improve the cycle performance of the battery. The currently known preparation methods of this additive mainly include the following types. [0003] It is reported in EP1308449A2 that LiBF4, oxalic acid react with silicon tetrachloride and aluminum trichloride as auxiliary agents in carbonate solvents, or take LiBF4, LiF, oxalic acid as raw materials, boron trich...

Claims

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Application Information

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IPC IPC(8): C07F5/02
CPCC07F5/025
Inventor 王坤刘红光叶学海刘大凡袁莉孙培亮赵庆云
Owner CNOOC TIANJIN CHEM RES & DESIGN INST
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