Lithium salt compound, preparation method thereof and lithium ion battery electrolyte containing lithium salt compound
A technology of lithium-ion batteries and compounds, applied in the field of lithium-ion batteries, can solve the problems of low flame retardancy and conductivity, few types of lithium salts, and difficulty in large-scale preparation, etc., achieve flame-retardant and conductive performance, low cost, and sufficient source of raw materials reliable effect
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[0053] The embodiment of the present invention provides a kind of preparation method of lithium salt compound, comprises the following steps:
[0054] Step S101, adding dialkyl alkylphosphonite into the protic solvent, mixing evenly, then adding alkyl acrylate while stirring and reacting at 0-80°C for 2-10 hours to obtain compound A; wherein, proton The solvent is any one of methanol, ethanol, formic acid, and acetic acid, and the molar ratio of the protic solvent to the dialkyl alkyl phosphinate is 1:1-1:1.2, and the dialkyl alkyl phosphinate to acrylic acid The molar ratio of alkyl ester is 1:1-1:1.2;
[0055] Step S102, add acid solution A to compound A, heat and reflux at 80-120°C for 4-12 hours, add acetone after the reaction is completed, and crystallize to obtain compound B; wherein, acid solution A is concentrated sulfuric acid or strong Acidic cation exchange resin, the molar dosage of acid solution A is 0.5%-5% of the molar dosage of compound A;
[0056] Step S103,...
Embodiment 1
[0074] Preparation of lithium salt compounds:
[0075] Add 408g (3mol) diethyl methylphosphonite and 180g (3mol) glacial acetic acid into a 1L four-neck flask, lower the temperature to 5°C, and add 300g (3mol) acrylic acid dropwise under nitrogen protection and mechanical stirring Ethyl ester, the rate of addition should be maintained at a temperature not exceeding 25°C. After about 1.5 hours of dropping, the temperature was kept at 25°C for 1 hour. After the reaction, the low boilers were evaporated to obtain 592.8g of compound A in the form of a colorless oily liquid. The yield was 95%, and the GC purity was 97%; 592.8g (2.85mol) of compound A was added in a 2L there-necked flask, and then 500g of water and 5g of concentrated sulfuric acid were added, and stirred and heated to reflux at 100°C for 6 hours. Then the water and the generated ethanol were evaporated, cooled to room temperature, 500g of acetone was added, stirred and dispersed, filtered, and the obtained filter ca...
Embodiment 2
[0080] Preparation of lithium salt compounds:
[0081] Add 204g (1.5mol) diethyl methylphosphonite and 90g (1.5mol) glacial acetic acid into a 1L four-necked flask, and add 192g (1.5mol) tert-acrylic acid dropwise under nitrogen protection and mechanical stirring at room temperature. Butyl ester, the dropping rate is maintained at a temperature not exceeding 70°C. After about 1 hour of dropwise addition, the temperature is kept at 75°C for 3 hours. After the reaction, the low boilers are evaporated to obtain 45.6 g of compound A in the form of a colorless oily liquid. The yield of compound A is The yield was 97.6%, and the GC purity was 97.5%. Add 345.6g (1.46mol) of compound A into a 2L three-necked flask, then add 500g of water and 2g of strong acidic cation exchange resin, stir and heat to reflux at 110°C for 4h, Evaporate the water and the ethanol produced, cool to room temperature, filter, recover the resin, add 500g of acetone, stir and disperse, filter, wash the obtaine...
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