Novel disulfonic acid type alkyl imidazole ionic liquid, preparation and uses thereof
A technology of alkylimidazole and ionic liquid, which is applied in the field of new bissulfonic acid acidic ionic liquid and its preparation, can solve the problems that the reaction conditions are not very friendly to the environment and cannot be surpassed, and achieve high reaction yield and low dosage , good catalytic activity
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[0060] Example 1
[0061] [(HSO 3 -p) 2 im][HSO 4 ](n=1, Y=HSO 4 )Synthesis:
[0062] Trimethylsilimidazole (14.0g0.1mol) was added to a 100mL three-necked flask, and 1,3-propane sultone (24.4g0.2mol) was slowly added dropwise under ice bath conditions. Stirring was continued for half an hour under ice bath conditions, about 1.8 mL (0.1 mol) of water was added dropwise, stirring was continued for 2 hours, water and trimethylsilanol were removed by distillation under reduced pressure to obtain an intermediate zwitterionic compound. Sulfuric acid (10.0g0.1mol) was added dropwise to the about 2mol / L aqueous solution of the obtained zwitterionic compound, and refluxed for 8 hours after the addition was completed. Finally, the solvent water was removed under reduced pressure at 90°C to obtain a light yellow transparent ion. Liquid 38.9g, yield 95%.
Example Embodiment
[0063] Example 2
[0064] [(HSO 3 -p) 2 im][HSO 4 ](n=1, Y=HSO 4 )Synthesis:
[0065] Trimethylsilimidazole (14.0g0.1mol) was added to a 100mL three-necked flask, and 1,3-propane sultone (24.4g0.19mol) was added dropwise slowly under ice bath conditions. Stirring was continued for half an hour under ice bath conditions, about 1.8 mL (0.1 mol) of water was added dropwise, stirring was continued for 2 hours, water and trimethylsilanol were removed by distillation under reduced pressure to obtain an intermediate zwitterionic compound. Add sulfuric acid (9.0g0.09mol) dropwise to the about 2mol / L aqueous solution of the obtained zwitterionic compound, reflux for 8 hours after the dropwise addition is complete, and finally remove the solvent water under reduced pressure at 80°C to obtain light yellow transparent ion Liquid 32.76g, yield 80%.
Example Embodiment
[0066] Example 3
[0067] [(HSO 3 -b) 2 im][HSO 4 ](n=2, Y=HSO 4 )Synthesis
[0068] Add trimethylsilimidazole (14.0g0.1mol) into a 100ml three-necked flask, and slowly add 1,4-butane sultone (27.2g0.2mol) dropwise under ice bath conditions. Stirring is continued for half an hour under ice bath conditions, about 1.8ml (0.1mol) of deionized water is added dropwise, stirring is continued for 2h, water and trimethylsilanol are removed by vacuum distillation to obtain an intermediate zwitterionic compound. Add 50ml of deionized water to the obtained zwitterionic compound and stir evenly, and add sulfuric acid (10.0g0.1mol) dropwise. After the addition is complete, heat and reflux at 90℃ for 6 hours, and finally remove it under reduced pressure at 90℃. Solvent water, 40.7 g of light yellow transparent ionic liquid was obtained, with a yield of 94%.
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