Method for synthesizing diphenyl carbonate through ester exchange reaction of dimethyl carbonate and phenylethyl acetate

A technology of dimethyl carbonate and transesterification, which is applied in the field of synthesizing diphenyl carbonate by transesterification of dimethyl carbonate and phenyl acetate, can solve the problems of low catalyst activity, unstable performance and the like, and achieves high catalyst activity, The effect of stable performance, good economic benefits and social benefits

Inactive Publication Date: 2010-01-20
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In order to solve the problems such as low catalyst activity and unstable performance in the prior art, the invention provides a catalyst system with industrial application prospects, that is, a β-diketone catalyst system, which is used

Method used

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  • Method for synthesizing diphenyl carbonate through ester exchange reaction of dimethyl carbonate and phenylethyl acetate

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0020] Weigh 80.0 grams of phenyl acetate (about 0.58mol), 53.0 grams of dimethyl carbonate (about 0.58mol), and 1.2 grams of titanyl acetylacetonate (about 0.0055mol) into a 250ml autoclave with an intelligent constant temperature controller. Seal with fasteners, and then use nitrogen to confirm the airtightness of the high-pressure airtight reactor. Under normal pressure, stir and heat up to keep the reaction temperature between 150 ° C. After 4 hours of reaction, stop heating. Stir and cool down to room temperature naturally, open the reaction kettle, discharge the liquid material in the kettle, and analyze the liquid material with a gas chromatograph. The conversion rate of dimethyl carbonate is 30.0%, and the selectivity of the catalyst to methyl phenyl carbonate (MPC) and diphenyl carbonate (DPC) is 65.0% and 25.0%, respectively.

Embodiment 2

[0022] Weigh 110.0 grams of phenyl acetate (about 0.80 mol), 36.0 grams of dimethyl carbonate (about 0.40 mol), and 1.5 grams of titanium acetylacetonate (about 0.006 mol) into a 250 ml high-pressure reactor with an intelligent constant temperature controller. Seal with fasteners, and then use nitrogen to confirm the airtightness of the high-pressure airtight reactor. Under normal pressure, stir and heat up to keep the reaction temperature between 175 ° C. After 4.5 hours, the reaction is over and the heating is stopped. Stir and cool down to room temperature naturally, open the reaction kettle, discharge the liquid material in the kettle, and analyze the liquid material with a gas chromatograph. The conversion rate of dimethyl carbonate is 74.0%, and the selectivity of the catalyst to methyl phenyl carbonate (MPC) and diphenyl carbonate (DPC) is 58.0% and 38.0% respectively.

Embodiment 3

[0024] Weigh 110.0 grams of phenyl acetate (about 0.80 mol), 20.0 grams of dimethyl carbonate (about 0.22 mol), and 1.2 grams of titanyl acetylacetonate (about 0.0055 mol) into a 250 ml high-pressure reactor with an intelligent thermostat controller, Seal it with fasteners, and then use nitrogen to confirm the airtightness of the high-pressure airtight reactor. Under normal pressure, stir and heat up to keep the reaction temperature between 180 ° C. After 5 hours of reaction, stop heating. Stir and cool down to room temperature naturally, open the reaction kettle, discharge the liquid material in the kettle, and analyze the liquid material with a gas chromatograph. The conversion rate of dimethyl carbonate was 80.0%, and the selectivity of the catalyst to methylphenyl carbonate (MPC) and diphenyl carbonate (DPC) were 60.0% and 38.0%, respectively.

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Abstract

The invention discloses a method used for synthesizing diphenyl carbonate through ester exchange reaction by using dimethyl carbonate (DMC) and phenylethyl acetate (PA) as raw materials. The method is characterized in that a catalyst system used by the method basically consists of beta-diketone compounds (seen in structural general formulas 1 and 2) belonged to IVB-class metals, and also can be homologous compound thereof. The catalyst system can exist stably in the air, the catalyst has good selectivity and catalytic activity on products comprising methyl phenyl carbonate (MPC) and the diphenyl carbonate (DPC), and the using amount of the catalyst is little. Therefore, the catalyst system can be widely applied to the production of the diphenyl carbonate. In the structural general formulas 1 and 2, M is Ti, Zr and Hf; and R and R' are substituted groups on the beta-diketone compounds, and can be alkyl, alkoxyl and halogen.

Description

technical field [0001] The invention discloses a method for synthesizing diphenyl carbonate by transesterification reaction, which uses dimethyl carbonate (DMC) and phenyl acetate (PA) as raw materials and β-diketone compounds as catalysts to prepare diphenyl carbonate phenyl esters. Background technique [0002] Diphenyl carbonate is non-toxic and non-polluting. It is an important "green" chemical product and can be used to synthesize many important organic compounds and polymer materials. It can especially replace highly toxic phosgene and react with bisphenol A to produce excellent performance. of polycarbonate. [0003] The synthesis methods of diphenyl carbonate mainly include phosgene method, phenol oxidative carbonylation method and transesterification method. Because phosgene is highly toxic and will cause serious environmental pollution, the traditional phosgene method is being phased out. Although the oxidative carbonylation of phenol has simple and easy-to-obta...

Claims

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Application Information

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IPC IPC(8): C07C69/96C07C68/06B01J31/22B01J31/38
Inventor 王公应曹平杨先贵贾树勇唐聪明王越姚洁曾毅刘良明
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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