A kind of preparation method of high-purity imidazole acetate ionic liquid
The technology of imidazole acetate and methylimidazole acetate is applied in the field of preparation of high-purity ionic liquid, can solve the problems of high raw material alkoxide price, serious environmental pollution, harsh reaction conditions, etc. The effect of high product purity and moderate reaction speed
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Embodiment 1
[0043] Preparation of 1-ethyl-3-methylimidazolium acetate ionic liquid:
[0044] Dissolve 1.0 mol of 1-ethyl-3-methylimidazolium chloride in 48 g of water to obtain solution A, and dissolve 1.2 mol of lithium perchlorate in 254 g of water to obtain solution B; mix solution A and solution B, 575g of dichloromethane was added, and the reaction was mechanically stirred for 12 hours; the liquid was separated, and the water phase was separated into a waste liquid, which was recovered, and the organic phase was washed with 260g of pure water each time, and washed 5 times, using AgNO 3 No precipitation was detected in the solution; the organic phase was vacuum rotary evaporated at 80 °C to obtain 193 g of 1-ethyl-3-methylimidazolium perchlorate ionic liquid intermediate in a yield of 91.9%; 579 g of ethanol was added, and under vigorous stirring, Slowly add a total of 90.1g of potassium acetate in 4 batches. During the addition process, solids are dissolved and separated out, and the...
Embodiment 2
[0046] Preparation of 1-butyl-3-methylimidazolium acetate ionic liquid:
[0047] Dissolve 1.0 mol of 1-butyl-3-methylimidazolium bromide in 58 g of water to obtain solution A, and dissolve 0.8 mol of lithium perchlorate in 170 g of water to obtain solution B; mix solution A and solution B, 531g of dichloromethane was added, and the reaction was mechanically stirred for 12 hours; the liquid was separated, and the organic phase was washed with 278g of pure water each time, and washed 3 times with AgNO 3 No precipitation was detected in the solution; the organic phase was vacuum rotary evaporated at 80°C to obtain 178.4g of 1-butyl-3-methylimidazolium perchlorate ionic liquid intermediate, the yield was 93.7%; 446g of ethanol was added, and under vigorous stirring, A total of 79.8 g of potassium acetate was slowly added in 4 batches. During the addition, solids were dissolved and precipitated continuously, and the reaction was continued for 12 hours; the stirring was stopped, fro...
Embodiment 3
[0049] Preparation of 1-octyl-3-methylimidazolium acetate ionic liquid:
[0050] Dissolve 1.0 mol of 1-octyl-3-methylimidazolium chloride in 78 g of water to obtain solution A, and dissolve 2.0 mol of lithium perchlorate in 426 g of water to obtain solution B; mix solution A and solution B, 841g of dichloromethane was added, and the reaction was mechanically stirred for 12 hours; the liquid was separated, and the water phase was separated into a waste liquid, which was recovered, and the organic phase was washed with 256g of pure water each time, and washed 3 times, using AgNO 3 No precipitation was detected in the solution; the organic phase was vacuum rotary-evaporated at 80°C to obtain 193 g of 1-octyl-3-methylimidazolium perchlorate ionic liquid intermediate with a yield of 91.9%; 965 g of ethanol was added, and under vigorous stirring, the A total of 90.1g of potassium acetate was slowly added in 4 batches. During the addition process, solids were dissolved and precipitat...
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