Preparation method of lithium difluorophosphate

A technology of lithium difluorophosphate and lithium hexafluorophosphate, which is applied in chemical instruments and methods, phosphorus compounds, inorganic chemistry, etc., can solve problems such as unfavorable safety production, energy saving and emission reduction, high requirements for reaction conditions, inconvenient control, etc., and is easy to realize , high yield, cost-saving effect

Active Publication Date: 2017-06-13
武汉海斯普林科技发展有限公司
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  • Abstract
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  • Claims
  • Application Information

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Problems solved by technology

[0005] However, the above-mentioned methods have their disadvantages. Some have higher requirements on reaction conditions (such as heating to more than 300 ° C), which is not conducive to safe production, energy saving and emission reduction, and some are inconvenient to control, low yield, low conversion rate (such as hydrolysis method)

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  • Preparation method of lithium difluorophosphate

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Set up the reaction device, first pass dry nitrogen to replace the air, stop nitrogen, immediately put 45.57g lithium hexafluorophosphate (about 0.3mol) into a 500mL four-neck round bottom flask, add 227.85g ethyl acetate to dissolve lithium hexafluorophosphate, turn on nitrogen and Heat and stir to raise the temperature of the solution to 40°C, and then add 55.67 g of TMSB (about 0.2 mol) dropwise. During the dropwise addition, bubbles appear in the solution and solids are precipitated. The dropwise addition process takes 50 minutes. After the dropwise addition, the temperature was slowly raised to 65°C, and the bubbles in the solution contained in the four-neck round-bottomed flask increased significantly, so the nitrogen flow rate was reduced to stabilize the gas flow rate in the tail gas absorption device. With the gradual progress of the reaction, the amount of bubbles observed in the four-necked round-bottom flask decreased, and the nitrogen flow was increased. At ...

Embodiment 2

[0030] Set up the reaction device, first feed dry nitrogen to replace the air, stop feeding nitrogen, immediately drop into 45.57g lithium hexafluorophosphate (about 0.3mol) into the 500mL four-neck round bottom flask, then add 200g of ethyl acetate recovered in Example 1, Turn on the nitrogen gas, and slowly add 61.24g TMSB (about 0.22mol) dropwise after the solution is heated to 35°C. Bubbles appear in the solution and solids are precipitated during the dropwise addition process. The dropwise addition process takes 40 minutes. Continue to heat up to 70°C, the bubbles in the solution will increase significantly, and the solid matter precipitated in the solution will also increase significantly. Adjust the flow of nitrogen to stabilize the flow of gas in the tail gas absorption device. After reacting for a certain period of time, the amount of bubbles that can be observed in the four-necked round-bottom flask decreases, and the nitrogen flow is increased to prevent the tail gas...

Embodiment 3

[0033] Set up the reaction device, first replace the air with dry nitrogen, stop nitrogen, immediately put 50.13g of lithium hexafluorophosphate (about 0.33mol) into a 500mL four-neck round bottom flask and add 227.85g of 1,4-dioxane to dissolve and put in Lithium hexafluorophosphate, turn on nitrogen, heat to keep the solution at 30°C, at this time there is still a small amount of lithium hexafluorophosphate undissolved, slowly add 62.91g TMSP (about 0.2mol) dropwise, bubbles gradually appear in the solution. After 60 minutes, the dropwise addition of TMSP was completed, and the temperature of the solution was slowly raised to 60°C. The bubbles in the solution gradually increased, and the precipitated solids in the flask also increased significantly. Reduce the nitrogen flow rate to stabilize the gas flow rate in the tail gas absorption device. After reacting for a period of time, the amount of bubbles observed in the flask decreases, and the nitrogen flow is increased to avoi...

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Abstract

The invention belongs to the technical field of chemical synthesis and in particular to a preparation method of lithium difluorophosphate. In the method, lithium difluorophosphate is obtained by reaction of lithium hexafluorophosphate with substrate. The preparation method comprises the following steps: 1) under the protection of protective gas, adding lithium hexafluorophosphate into an organic solvent; 2) heating the solution to a dissolving temperature to obtain solution, then dropwise adding tri(trimethylsilane)borate or tri(trimethylsilane)phosphate into the solution, and forming precipitates; and 3) heating the solution to a reaction temperature, stirring at the reaction temperature and reacting, and after the reaction is finished, sequentially filtering, washing and drying precipitates, so that pure lithium difluorophosphate is obtained. The preparation method provided by the invention can be carried out under relatively mild conditions and has relatively high yield of lithium difluorophosphate, and batch production can be carried out without requiring complex operation.

Description

technical field [0001] The invention belongs to the technical field of chemical synthesis, and in particular relates to a preparation method of lithium difluorophosphate. Background technique [0002] In recent years, due to the widespread use of mobile smart devices and the country's vigorous promotion of new energy vehicles, the demand for lightweight and high-performance batteries and accumulators has also increased dramatically. [0003] As a conductive salt, lithium difluorophosphate can form a film on the electrode interface to improve high and low temperature cycle performance and effectively reduce the amount of lithium hexafluorophosphate used in batteries and batteries. Therefore, in the context of the continuous expansion of the market size of portable mobile devices and new energy vehicles, the demand for lithium difluorophosphate as an additive for high-performance batteries and battery electrolytes will also increase accordingly. [0004] At present, there are...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C01B25/455
CPCC01B25/455
Inventor 周永妍陈杰陈丹熊伟潘君王文
Owner 武汉海斯普林科技发展有限公司
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