Pyridine acrylate crystal, preparation method and application of pyridine acrylate crystal in preparation of methyl ethyl carbonate
A technology of pyridine acrylate and ethyl methyl carbonate, applied in the field of preparation of ethyl methyl carbonate, preparation, pyridine acrylate crystals, can solve the problems of difficulty in catalyst reuse, poor reaction selectivity, high temperature, etc., and achieve novel crystal structure, The effect of mild reaction conditions and low cost
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[0033] 1) Preparation of crystal catalyst
[0034] Dissolve 3-pyridinebenzaldehyde and malonic acid with pyridine, toluene, and aniline, heat, pass condensed water until complete reaction, and remove the organic solvent by vacuum rotary evaporation, then add K 2 CO 3 solution and ethyl acetate solution, which was stirred. The organic layer was neutralized with hydrochloric acid solution, filtered and dried. Obtain trans-3(3-pyridyl)acrylic acid (HL 2 ).
[0035]
[0036] Add zinc chloride and trans-3(3-pyridyl)acrylic acid into distilled water, and stir for 15 minutes to obtain a mixed solution. Seal the mixed solution in a stainless steel reaction kettle lined with polytetrafluoroethylene, the filling degree of the reaction kettle is 80%, and then put the stainless steel reaction kettle in an oven at 150°C to heat and crystallize for 4 days, and then cool at room temperature, that is A crystal catalyst of pyridine acrylate was obtained. The molar ratio of zinc chlori...
Embodiment 1
[0043] 1) Catalyst preparation
[0044]Dissolve 0.029g of trans-3 (3-pyridyl)acrylic acid and 0.037g of zinc chloride in 10ml of distilled water, stir for 15min, seal the resulting mixture into a stainless steel reactor lined with polytetrafluoroethylene, and fill the reactor with The temperature is 80%, and then the stainless steel reactor is placed in an oven at 150° C. to heat and crystallize for 4 days, and then cooled at room temperature to obtain the pyridine acrylate crystal catalyst.
[0045] 2) Test experiment of transesterification reaction activity (with temperature as experimental variable)
[0046] Add 0.2 mol dimethyl carbonate, 0.2 mol diethyl carbonate and 5% of the above-mentioned catalyst to the mass of dimethyl carbonate in a 50 mL flask and stir for reaction. The reaction temperature is 70°C, 75°C, 80°C, 85°C, 90°C, 95°C, 100°C, and the reaction time is 2h. After the reaction was completed, the catalyst was filtered off, and the content of ethyl methyl ca...
Embodiment 2
[0048] 1) Catalyst preparation
[0049] Prepare with catalyst in embodiment 1
[0050] 2) Test experiment of transesterification reaction activity (with reaction time as variable)
[0051] Add 0.2 mol dimethyl carbonate and 0.2 mol diethyl carbonate and 5% of the mass of dimethyl carbonate into the 50 mL flask and stir for reaction. The reaction temperature is 90°C, and the reaction time is 1h, 2h, 4h, 6h. After the reaction was completed, the catalyst was filtered off, and the content of ethyl methyl carbonate was measured by gas chromatography, and the yields of ethyl methyl carbonate were about 37.1%, 51.3%, 51.0%, and 51.2%.
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