Catalyst for preparing isocyanate by thermal decomposition of aryl (alkyl) carbamic acid ester and use thereof
A technology based on carbamate and carbamate, applied in the field of catalysts, can solve problems such as low product yield and catalyst separation, and achieve the effects of simple process operation, easy separation, and mild reaction conditions
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Embodiment 1
[0026] Add 3.0g of methyl phenylcarbamate and 47.0g of solvent o-dichlorobenzene in the three-necked bottle to form a dispersion with a mass concentration of 6%, and add 0.15g of Bi 2 o 3 Catalyst, the amount added is 5% of the mass of methyl phenylcarbamate, the temperature of the reaction solution is raised to 180°C under nitrogen protection and stirring conditions, the reaction is carried out for 30 minutes, and the formed methanol is evaporated. After the reaction, the catalyst is filtered and reacted with liquid separation. After the reaction solution was treated with di-n-butylamine, it was analyzed by HPLC. The conversion rate of methyl phenylcarbamate was 95.8%, and the yield of phenylisocyanate was 87.6%.
Embodiment 2
[0028] Add 3.0g methyl phenylcarbamate and solvent o-dichlorobenzene 47.0g in three-necked bottle, form the dispersion liquid that mass concentration is 6%, add the Bi of 0.12g after the reaction recovery of example 1 simultaneously 2 o 3 Catalyst, the addition amount is 4% of the mass of methyl phenylcarbamate, the temperature of the reaction solution is raised to 180°C under the condition of nitrogen protection and stirring, the reaction is carried out for 30 minutes, and the formed methanol is distilled off. After the reaction, the catalyst is suction filtered and reacted with liquid separation. After the reaction solution was treated with di-n-butylamine, it was analyzed by HPLC. The conversion rate of methyl phenylcarbamate was 92.2%, and the yield of phenylisocyanate was 81.2%.
Embodiment 3
[0030] Add 3.0g methyl phenylcarbamate and solvent methyl benzoate 30.3g in the three-necked bottle, form the dispersion liquid that mass concentration is 9%, add the Bi of 0.15g simultaneously 2 o 3 Catalyst, the addition amount is 5% of the mass of methyl phenylcarbamate, the temperature of the reaction solution is raised to 195°C under nitrogen protection and stirring conditions, the reaction is carried out for 30 minutes, and the formed methanol is distilled off. After the reaction, the catalyst is suction filtered and reacted with liquid separation. After the reaction solution was treated with di-n-butylamine, it was analyzed by HPLC. The conversion rate of methyl phenylcarbamate was 91.4%, and the yield of phenylisocyanate was 83.2%.
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