Silicon oxide-immobilized organic tin catalyst for transesterification of dimethyl carbonate and phenol ester, and preparation method thereof

A technology of dimethyl carbonate and silicon oxide is applied in the field of silicon oxide immobilized organotin catalyst and preparation, which can solve problems such as complicated preparation process, and achieve the effect of simple preparation method and good catalytic performance.

Inactive Publication Date: 2017-11-03
CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The preparation process of the above-mentioned silicon oxide immobilized organotin catalyst is relatively cumbersome, mainly because the synthesis of organoti

Method used

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  • Silicon oxide-immobilized organic tin catalyst for transesterification of dimethyl carbonate and phenol ester, and preparation method thereof
  • Silicon oxide-immobilized organic tin catalyst for transesterification of dimethyl carbonate and phenol ester, and preparation method thereof
  • Silicon oxide-immobilized organic tin catalyst for transesterification of dimethyl carbonate and phenol ester, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0018] Add 6g of 3-chloropropylethoxysilane, 2g of magnesium powder and a small amount of iodine to 60mL of diethyl ether, heat to reflux for 3h, then add 6.5g of anhydrous tin tetrachloride, heat at reflux at 130°C for 3h to obtain propyl tri Silane reagent solution of tin chloride; add 25g ethyl orthosilicate to the silane reagent solution of propyltin trichloride, stir and add the solution to 150mL of 20% hydrochloric acid, stir for 2h, filter, wash, 120°C Vacuum drying was carried out to obtain a silica-immobilized organotin catalyst sample 1 whose active component was propyltin trichloride, and the tin loading was 23.5% as measured by an inductively coupled plasma atomic emission spectrometer.

Embodiment 2

[0020] Add 9g of 3-chlorobutylethoxysilane, 3g of magnesium powder and a small amount of iodine to 80mL of diethyl ether, heat to reflux for 2h, then add 4.6g of anhydrous tin tetrachloride, and heat at 130°C for 4h to obtain dibutyl The silane reagent solution of tin dichloride; add 50g of isopropyl silicate to the silane reagent solution of dibutyltin dichloride, after stirring, add the solution to 200mL of 18% ammonia water, stir for 1h, filter, wash, Dry at 120° C. to obtain a silica-immobilized organotin catalyst sample 2 whose active component is dibutyltin dichloride, and the tin loading is 12.8%.

Embodiment 3

[0022] Add 9g of 4-chlorobutylethoxysilane, 3g of magnesium powder and a small amount of iodine to 80mL of ether, heat to reflux for 2h, then add 4.6g of anhydrous tin tetrachloride, and heat at 130°C for 4h to obtain dibutyl The silane reagent solution of tin dichloride; add 10g of mesoporous silicon oxide to the silane reagent solution of dibutyltin dichloride, heat and reflux for 8h, filter, wash, and vacuum dry at 120°C to obtain the active component dibutyl Silicon oxide immobilized organotin catalyst sample 3 of tin dichloride, with a tin loading of 8.4%.

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Abstract

The present invention is a silicon oxide-immobilized organic tin catalyst for transesterification of dimethyl carbonate and phenol ester, and a preparation method thereof, wherein the silicon oxide-immobilized organic tin catalyst is prepared by using the silane reagent of alkyl tin chloride as an organotin precursor, the basic composition comprises alkyl tin chloride and silicon oxide, alkyl tin chloride is used as an active component, and silicon oxide is used as a carrier. According to the present invention, the silicon oxide-immobilized organic tin catalyst shows excellent catalytic performance in the dimethyl carbonate and phenol ester transesterification reaction for synthesis of diphenyl carbonate, wherein the phenol conversion rate is 50.6%, the transesterification selectivity is more than 99.9%, and the catalyst is a heterogeneous catalyst, can reduce the toxicity of organotin, is easily separated and recovered from the reaction system after the reaction, and can be reused.

Description

technical field [0001] The invention discloses a silicon oxide immobilized organotin catalyst for the transesterification of dimethyl carbonate and phenol and a preparation method thereof Background technique [0002] Diphenyl carbonate is a green engineering plastic intermediate, which can synthesize various organic compounds and polymer materials through reactions such as chlorination, nitration, hydrolysis and ammonolysis, especially can replace highly toxic phosgene and bisphenol A by melting Polymerization reaction to synthesize polycarbonate with excellent properties. The transesterification of dimethyl carbonate and phenol to synthesize diphenyl carbonate is considered to be the most promising method for non-phosgene synthesis of diphenyl carbonate. All kinds of organotins as homogeneous catalysts have good catalytic properties for the reaction of transesterification of dimethyl carbonate and phenol to synthesize diphenyl carbonate. Shaikh et al. (Ind Eng Chem Res, ...

Claims

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Application Information

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IPC IPC(8): B01J31/12C07C68/06C07C69/96
CPCB01J31/122B01J2231/49C07C68/06C07C69/96
Inventor 陈彤张元卓王公应张华姚洁
Owner CHENGDU ORGANIC CHEM CO LTD CHINESE ACAD OF SCI
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