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Drying method of imidazolyl fluorine-containing lithium salt

A drying method, imidazole-based technology, applied in the drying field of imidazole-based fluorine-containing lithium salt, can solve the problems of moisture sensitivity, poor thermal stability and chemical stability, etc., achieve mild reaction conditions, shorten vacuum drying time, and avoid reaction side effects The effect of product formation

Active Publication Date: 2021-09-07
JIANGSU LEE & MAN CHEM
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Fluorine-containing lithium salt is the main raw material of lithium battery electrolyte. Currently, the most widely used fluorine-containing lithium salt with the highest market share is LiPF 6 (lithium hexafluorophosphate), but LiPF 6 There are problems such as poor thermal stability and chemical stability, and sensitivity to moisture, so it is necessary to synthesize a new fluorine-containing lithium salt

Method used

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  • Drying method of imidazolyl fluorine-containing lithium salt
  • Drying method of imidazolyl fluorine-containing lithium salt
  • Drying method of imidazolyl fluorine-containing lithium salt

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] Step 1: In a 500ml four-necked flask, add 50g of diaminomaleonitrile and 250ml of anhydrous acetonitrile, then drop in 102g of trifluoroacetic anhydride, raise the temperature to 50°C and stir for 4 hours, then distill off the solvent and by-products under reduced pressure to obtain 77.4 g of 2-trifluoromethyl-4,5-dicyanoimidazole.

[0027] Step 2: In a 500ml four-necked flask, 16.8g of lithium carbonate was made into an aqueous phase suspension, and 77.4g of 2-trifluoromethyl-4,5-dicyanoimidazole prepared in step 1 was added, and the temperature was raised to 40°C. Continue to stir the reaction for 0.5h, the pH test paper test reaction solution is neutral, then add 5g of activated carbon for decolorization, raise the temperature to 70°C, continue to stir for 2h, filter while it is hot, cool to room temperature, and filter again to obtain 2-trifluoromethyl-4, 70.3 g of lithium salt of 5-dicyanoimidazole.

[0028] Step 3: Take 70.3g of 2-trifluoromethyl-4,5-dicyanoimida...

Embodiment 2

[0031] Step 1 and step 2 in Example 1 were repeated, and the recovered absolute ethanol was added in step 3. The obtained lithium salt of 2-trifluoromethyl-4,5-dicyanoimidazole was vacuum-dried at 135° C. for 3 hours, and the water content in the Karl Fischer test was 17 ppm.

Embodiment 3

[0032] Embodiment 3 (comparative example):

[0033] Repeat steps 1, 2, and 4 in Example 1, rinse with absolute ethanol, and dry the lithium salt of 2-trifluoromethyl-4,5-dicyanoimidazole in vacuum at 150°C for 8 hours. Hugh tested for a moisture content of 150ppm.

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Abstract

The invention relates to a drying method of an imidazolyl fluorine-containing lithium salt. The method comprises the following steps: (1) adding diaminomaleonitrile and perfluorinated anhydride into a reaction container, adding a solvent into the container, carrying out a stirring reaction, and after the diaminomaleonitrile is completely reacted, evaporating to remove the reaction solvent and a byproduct to obtain an intermediate product 2-perfluoroalkyl-4, 5-dicyanoimidazole; (2) carrying out a reaction on 2-perfluoroalkyl-4, 5-dicyanoimidazole and a metal salt or hydroxide aqueous phase suspension until the system is neutral to obtain a 2-perfluoroalkyl-4, 5-dicyanoimidazole salt; (3) decolorizing the 2-perfluoroalkyl-4, 5-dicyanoimidazolium salt in pure water by using activated carbon, filtering, and recrystallizing in pure water; (4) rinsing the 2-perfluoroalkyl-4, 5-dicyanoimidazolium salt obtained in the step (3) by using a solvent with water; and (5) filtering the rinsed 2-perfluoroalkyl-4, 5-dicyanoimidazole salt, and carrying out vacuum drying on the filtered 2-perfluoroalkyl-4, 5-dicyanoimidazole salt to obtain a finished product of the 2-perfluoroalkyl-4, 5-dicyanoimidazole lithium salt. According to the invention, the generation of reaction byproducts can be effectively avoided, and the subsequent vacuum drying effect is improved.

Description

technical field [0001] The invention relates to the technical field of drying fluorine-containing lithium salt and removing water, in particular to a drying method of imidazole-based fluorine-containing lithium salt. Background technique [0002] Fluorine-containing lithium salt is the main raw material of lithium battery electrolyte. Currently, the most widely used fluorine-containing lithium salt with the highest market share is LiPF 6 (lithium hexafluorophosphate), but LiPF 6 There are problems such as poor thermal stability and chemical stability, and sensitivity to moisture, so it is necessary to synthesize a new fluorine-containing lithium salt. For the electrolyte, the conductivity of the conductive lithium salt is the first factor to be considered. The anion structure directly affects the performance of the lithium salt. The larger the anion radius, the smaller the lithium salt lattice, the higher the solubility in organic solvents, and the greater the conductivity...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D233/90
CPCC07D233/90Y02E60/10
Inventor 周旺鹰冯娜娜陶哲
Owner JIANGSU LEE & MAN CHEM
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