Preparation method of catalyst used for synthesizing diphenyl carbonate through ester exchange
A technology of diphenyl carbonate and catalyst, which is applied in the field of preparation of catalysts for synthesizing diphenyl carbonate by transesterification, can solve the problems of low transesterification activity, and achieve the effects of high activity, easy separation and good catalytic activity
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[0025] Example 1
[0026] 8g of tetrabutyl titanate was weighed and dissolved in 20ml of absolute ethanol, the solution was added to 20ml of water at room temperature, ultrasonicated for 1h, rotary evaporated at 90°C for 1h, and calcined at 130°C for 7h to obtain the catalyst.
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[0027] Example 2
[0028] Carry out the transesterification of dimethyl carbonate and phenol with the catalyst prepared in Example 1
[0029] (1) In the there-necked flask that is connected with nitrogen conduit and thermometer, constant pressure dropping funnel and is equipped with rectifying column, add the catalyst 0.8g of embodiment 1, 15g phenol.
[0030] (2) Heating to 175°C, dimethyl carbonate was added dropwise, the amount of dimethyl carbonate added was 13.5ml, and the reaction was carried out for 9 hours. During the reaction, the mixed fraction of methanol and dimethyl carbonate was continuously distilled from the rectifying column.
[0031] (3) The mixed fraction and the reaction solution containing the products methyl phenyl carbonate and diphenyl carbonate were all analyzed by Shimadzu GC-14B gas chromatograph, and quantified by the calibration normalization method. The conversion of phenol was 46.0%, the yields of methylphenyl carbonate and diphenyl carbonate were
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[0032] Example 3
[0033] Weigh 3 g of titanocene dichloride and dissolve it in 40 ml of anhydrous ethanol, add 60 ml of an alcohol aqueous solution with a volume ratio of alcohol to water of 9 to the solution of titanocene dichloride and ethanol at room temperature, and ultrasonically treat it for 0.5 h for 85 The catalyst was obtained by rotary evaporation at °C for 1 h and calcination at 160 °C for 3 h. Use the obtained catalyst to carry out the transesterification of dimethyl carbonate and phenol, the reaction conditions are the same as those in Example 2, the conversion rate of phenol is 33.5%, and the yields of methyl phenyl carbonate and diphenyl carbonate are respectively 17.9 % and 15.6%, the total selectivity of transesterification is 99.9%.
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