Preparation and application of monodisperse solid catalyst for preparing diphenyl carbonate through interesterification

A technology of diphenyl carbonate and dimethyl carbonate is applied in the field of preparation and application of a monodispersed solid catalyst for preparing diphenyl carbonate by transesterification, and can solve problems such as low activity and selectivity of heterogeneous catalysts, Achieve the effect of solving easy inactivation, avoiding loss, and strong interaction

Active Publication Date: 2019-04-26
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The technical problem to be solved by the present invention is the heterogeneous catalyst activity, selectivity low problem that exists in the prior art, provides a kind of new catalyst that is used for dimethyl carbonate and phenol to prepare diphenyl carbonate, and this catalyst has catalyst The characteristics of low dosage, high activity and not easy to lose

Method used

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  • Preparation and application of monodisperse solid catalyst for preparing diphenyl carbonate through interesterification
  • Preparation and application of monodisperse solid catalyst for preparing diphenyl carbonate through interesterification
  • Preparation and application of monodisperse solid catalyst for preparing diphenyl carbonate through interesterification

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Take 50g of silica balls and add them to 500ml of toluene, heat to reflux and add 0.01mol aminopropyltriethoxysilane, after reflux for 2h, cool, filter and wash with absolute ethanol. Prepare 0.1 mol p-hydroxybenzoic acid solution, add the modified carrier, heat and stir for 8 hours. Filter, wash with ethanol, immerse in an aqueous solution containing 0.1mol tin tetrachloride, stir for 4 hours, add excess phenol, filter, wash with dimethyl carbonate, and dry to obtain catalyst sample S1 for reaction.

Embodiment 2

[0032] Take 50g of activated carbon and add it to 500ml of ethanol, add 0.01mol aminopropyltriethoxysilane after heating to reflux, and after reflux for 2h, cool, filter, and wash with absolute ethanol. Dissolve 0.1 mol of o-hydroxybenzoic acid, add the modified carrier, and heat and stir for 8 hours. After filtering, washing with ethanol, immersing in an aqueous solution containing 0.1 mol of tin nitrate, stirring for 4 hours, adding excess phenol, filtering, washing with dimethyl carbonate, and drying to obtain a reaction catalyst sample S2.

Embodiment 3

[0034] Take 50g of silica balls and add them to 500ml of dichloromethane, heat to reflux and add 0.01mol aminopropyltriethoxysilane, after reflux for 2h, cool, filter and wash with dichloromethane. Dissolve 0.1 mol of p-hydroxybenzoic acid, add the modified carrier, heat and stir for 8 hours. Filter, wash with ethanol, immerse in a chloroform solution containing 0.1 trimethylstannane, stir for 4 hours, add excess phenol, filter, wash with dimethyl carbonate, and dry to obtain a reaction catalyst sample S3.

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PUM

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Abstract

The invention relates to a catalyst for preparing diphenyl carbonate through interesterification of dimethyl carbonate and phenol and a preparation method of the catalyst. The problems of low activityand easy loss of heterogeneous catalysts in the prior art are mainly solved. According to the catalyst, active components are fixedly loaded onto a carrier through chemical bonds, the catalyst is a loaded monodisperse tin catalytic system catalyst, and comprises the carrier and a stannate ester group, the carrier is a substrate, and the stannate ester group is the active center. According to thetechnical scheme of the catalyst, the problem of catalyst loss in a reaction of synthesis of the diphenyl carbonate through interesterification of the phenol and the dimethyl carbonate is well solved,and the catalyst can be used for industrial production of the diphenyl carbonate.

Description

technical field [0001] The invention relates to a catalyst for preparing diphenyl carbonate by transesterification between phenol and dimethyl carbonate, its preparation and application. Background technique [0002] Diphenyl carbonate (DPC) is a raw material for the preparation of polycarbonate by non-phosgene method. The traditional preparation method is phosgene method, which is subject to policy restrictions due to the potential harm of highly toxic phosgene to the environment and safe production. The process of synthesizing diphenyl carbonate by transesterification of phenol (PhOH) and dimethyl carbonate (DMC) under the action of a catalyst avoids the use of highly toxic raw material phosgene, and the main by-product methanol can also be recycled for the starting raw material carbonic acid The synthesis of dimethyl ester is the most promising green process route for industrialization. [0003] At present, the transesterification of dimethyl carbonate and phenol to synt...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07C68/06C07C69/96
CPCB01J31/2213B01J2231/49B01J2531/42C07C68/06C07C69/96
Inventor 戈军伟何文军金照生
Owner CHINA PETROLEUM & CHEM CORP
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