Sulfur-containing ionic liquid, and preparation method and application thereof
An ionic liquid and electrolyte technology, applied in the field of lithium-ion batteries, can solve the problems of unfavorable lithium-ion battery electrolytes, reduced stability of ionic liquids, narrowed electrochemical windows, etc., and achieves cheap and easy-to-obtain raw materials and good thermal stability. , the effect of high decomposition voltage
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[0041] A preparation method of the above-mentioned sulfur-containing ionic liquid, the preparation process is as follows:
[0042]
[0043] Wherein RY is methyl trifluoromethanesulfonate, ethyl trifluoromethanesulfonate, propyl trifluoromethanesulfonate, butyl trifluoromethanesulfonate, methyl trifluoroacetate, ethyl trifluoroacetate, trifluoroacetic acid Propyl ester or butyl trifluoroacetate; R is an alkyl group with 1 to 4 carbon atoms, Y - for CF 3 SO 3 - or CF 3 CO 2 - .
[0044] Specifically include the following steps:
[0045] Step S1: Under the protection of an inert atmosphere, add dimethyl sulfide and the alkylating agent RY to an organic solvent in a molar ratio of 1:1 to 1.2:1, the mass ratio of the organic solvent to the dimethyl sulfide is The ratio is 0.8:1 to 1.4:1, and the reaction is stirred for 5 hours to 30 hours at a temperature of 5°C to 35°C.
[0046] Wherein, the alkylating reagent RY is methyl trifluoromethanesulfonate, ethyl trifluorometh...
Embodiment 1
[0077] Add 70g of chloroform, (68.3g, 1.1mol) dimethyl sulfide, (164.1g, 1.0mol) methyl trifluoromethanesulfonate into a 500mL flask respectively, and raise the temperature to 25°C under a nitrogen atmosphere, and stir the reaction for 20 Hour. Stand to cool, carry out vacuum distillation at a temperature of 100°C and a pressure of 3.0Pa to remove excess reactants, collect the colorless liquid and wash it three times with 50ml methyl tert-butyl ether, and then wash it at a temperature of 80°C , vacuum-dried under the condition of 0.01MPa vacuum to obtain colorless liquid trimethylsulfonium trifluoromethanesulfonate with a yield of 87%.
[0078] Its hydrogen spectrum data are as follows:
[0079] 1 H NMR (CDCl 3 , 400MHz, ppm): 3.24(s, 9H)
[0080] Under inert atmosphere protection, take out 10g, trimethylsulfonium trifluoromethanesulfonate, then add the mixed solvent of 50g ethylene carbonate (EC), propylene carbonate (PC) and ethyl methyl carbonate (EMC) wherein, Among t...
Embodiment 2
[0082] Add 50g tetrahydrofuran, (62.1g, 1.0mol) dimethyl sulfide, (178.1g, 1.0mol) ethyl trifluoromethanesulfonate into a 500mL flask respectively, and raise the temperature to 10°C under a nitrogen atmosphere, and stir for 30 Hour. Stand to cool, carry out vacuum distillation at a temperature of 80°C and a pressure of 0.1Pa to remove excess reactants, collect the colorless liquid and wash it three times with 50ml of methyl tert-butyl ether, and then wash it at a temperature of 60°C , vacuum-dried under the condition of vacuum degree of 0.01MPa to obtain colorless liquid dimethylethylsulfonium trifluoromethanesulfonate with a yield of 88%.
[0083] Its hydrogen spectrum data are as follows:
[0084] 1 H NMR (CDCl 3 , 400MHz, ppm): 3.38(m, 2H), 3.25(s, 6H), 2.29(s, 3H).
[0085] Under the protection of an inert atmosphere, take out 10g of dimethyl ethyl sulfonium trifluoromethanesulfonate, then add 100g of ethylene carbonate (EC), propylene carbonate (PC) and ethyl methyl c...
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