Preparation method of dimethyl carbonate
A technology of dimethyl carbonate and ethylene carbonate, which is applied in the field of synthesis of new ionic liquid riveting type and new strong alkaline ionic liquid, can solve the problems of easy deactivation, poor thermal stability, weak alkalinity, etc., and achieve optimal Catalytic activity, high stability effect
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Embodiment 1
[0128] Selecting a series of typical and commercialized ionic liquids, the acidic ionic liquid 1-ethyl-3-methylimidazolium ethyl sulfate salt ([Emim]C 2 h 5 SO 4 ), 1-ethyl-3-methylimidazolium hexafluoroantimony ester salt ([Emim]SbF 6 ), 1-ethyl-3-methylimidazolium p-toluenesulfonate ([Emim]ToS), 1-butyl-3-methylimidazolium tetrafluoroborate ([Bmim]BF 4 ), 1-ethyl-3-methylimidazolium tetrafluoroborate ([Emim]BF 4 ), 1-butyl-3-methylimidazolium hexafluorophosphate ([Bmim]PF 6 ), 1-ethyl-3-methylimidazolium hexafluorophosphate ([Emim]PF 6 ), 1-butyl-3-methylimidazolium chloride ([Bmim]Cl), 1-ethyl-3-methylimidazolium chloride ([Emim]Cl), 1,3-dimethylimidazolium chloride ([Mmim]Cl), 1-butyl-3-methylimidazolium bromide ([Bmim]Br), 1-ethyl-3-methylimidazolium bromide ([Emim]Br), 1-butyl- 3-methylimidazolium iodide ([Bmim]I) and 1-ethyl-3-methylimidazolium iodide ([Emim]I), 1,3-dimethylimidazolium iodide ([Mmim]I) The influence of ethylene carbonate (EC) and methanol (MeOH) ...
Embodiment 2
[0134] The specific preparation method of 1-ethyl-3-methylimidazolium imidazolium salt: dissolve 0.5mol imidazole in 60mL ethanol solvent, add equimolar potassium ethoxide to a three-necked flask, stir vigorously at 60°C for 6h, and the reaction is over Finally, under the condition of 65°C in an oil bath, the solvent ethanol and the product ethanol were removed by rotary evaporation under reduced pressure for 2 hours, and dried in a vacuum drying oven for 12 hours to constant weight to prepare imidazole potassium salt. 0.5 mol of commercially purchased [EmIm]Br was added into a three-necked flask, and potassium imidazole was added in an equimolar ratio under the condition of ethanol with water as a solvent, and the reaction was stirred at room temperature for 24 hours. After the reaction was completed, the resulting white solid KBr was removed by filtration, and the solvent was removed by rotary evaporation under reduced pressure for 2 hours in an oil bath at 65°C, and dried in...
Embodiment 3
[0137] Table 2 is the data that the ionic liquid synthesized in the laboratory is used for EC and MeOH transesterification reaction, the preparation method of ionic liquid in table 2 is the same as the preparation method of 1-ethyl-3-methylimidazolium imidazolium salt in embodiment 2, difference The reason is that the corresponding raw materials are used. Catalyst evaluation conditions are reaction temperature 68°C, reaction time 5min, raw material molar ratio EC:MeOH=1:10, catalyst content 0.3% of raw material mass fraction.
[0138] Table 2 Effects of synthesized ionic liquids on the transesterification activity of EC and MeOH
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[0141] Reaction conditions: The molar ratio of raw materials EC and MeOH is 1:10, the amount of catalyst added is 0.3wt%, and the reaction temperature is 68°C
[0142] From the data in Table 1, it can be seen that the strongly basic ionic liquids all exhibited excellent catalytic activity, and the selectivities of DMC and EG ...
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