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Heterogeneous catalyst for synthesizing diphenyl carbonate, and preparation method thereof

A technology of diphenyl carbonate and heterogeneous catalyst, applied in the fields of catalytic chemistry and organic chemistry, can solve problems such as difficult separation and difficult recycling, and achieve the effect of promoting the reaction, not easy to break or fall off, and ensuring catalytic activity

Active Publication Date: 2020-01-03
湖北三宁碳磷基新材料产业技术研究院有限公司 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The invention provides a heterogeneous catalyst for synthesizing diphenyl carbonate and a preparation method thereof, which can solve the problems of difficult separation and recycling of existing catalysts, and has the characteristics of high activity and high selectivity

Method used

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  • Heterogeneous catalyst for synthesizing diphenyl carbonate, and preparation method thereof
  • Heterogeneous catalyst for synthesizing diphenyl carbonate, and preparation method thereof
  • Heterogeneous catalyst for synthesizing diphenyl carbonate, and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] Dissolve 2.84g (0.01mol) of tetraisopropyl titanate in anhydrous methanol, stir and mix evenly, add 6.63g of MCM-41 molecular sieve (mass ratio 30:70), filter after hydrothermal synthesis reaction at 105°C for 24h, and Air-dry the filtered mixture for 2 hours, then dry in an oven for 8 hours at a drying temperature of 80°C to obtain a catalyst intermediate; then dissolve the catalyst intermediate in anhydrous methanol, stir for about 2 hours, and slowly add chlorine dropwise in an ice-water bath 0.005 mol of sulfonic acid, then stirred at room temperature for 2 days, filtered and washed until neutral, and the obtained solid was dried in an oven at 60°C for 20 hours to obtain Catalyst 1.

[0026] Phenol and dimethyl carbonate are transesterified under the above catalyst. In a four-necked flask equipped with a gas guide tube, a thermometer and a rectifying column, the molar ratio of dimethyl carbonate to phenol is 1:1, and the catalyst dosage is 1wt. %, the reaction time ...

Embodiment 2

[0028] Dissolve 2.48g (0.01mol) titanocene dichloride in anhydrous methanol, stir and mix evenly, add 5.79g MCM-41 molecular sieve (mass ratio 30:70), filter after hydrothermal synthesis at 105°C for 24h, and The mixture obtained by filtration was air-dried for 2 hours, then dried in an oven for 8 hours at a drying temperature of 80°C to obtain a catalyst intermediate; then dissolved the catalyst intermediate in anhydrous methanol, stirred for about 2 hours, and slowly added chlorosulfur in an ice-water bath Acid 0.005mol, then stirred at room temperature for 2 days, filtered and washed until neutral, and the obtained solid was dried in an oven at 60°C for 20 hours to obtain Catalyst 2.

[0029] Phenol and dimethyl carbonate are transesterified under the above catalyst. In a four-necked flask equipped with a gas guide tube, a thermometer and a rectifying column, the molar ratio of dimethyl carbonate to phenol is 1:1, and the catalyst dosage is 1wt. %, the reaction time is 10h,...

Embodiment 3

[0031] Dissolve 2.80g (0.01mol) of dicyclopentadienyl dimethyltitanium in anhydrous methanol, stir and mix evenly, add 6.53g of MCM-41 molecular sieve (mass ratio 30:70), after 24 hours of hydrothermal synthesis reaction at 105°C Filter, and air-dry the filtered mixture for 2 hours, then dry in an oven for 8 hours at a drying temperature of 80°C to obtain a catalyst intermediate; then dissolve the catalyst intermediate in anhydrous methanol, stir for about 2 hours, and slowly Add 0.005 mol of chlorosulfonic acid dropwise, then stir at room temperature for 2 days, filter and wash until neutral, and dry the obtained solid in an oven at 60°C for 20 hours to obtain catalyst 3.

[0032] Phenol and dimethyl carbonate are transesterified under the above catalyst. In a four-necked flask equipped with a gas guide tube, a thermometer and a rectifying column, the molar ratio of dimethyl carbonate to phenol is 1:1, and the catalyst dosage is 1wt. %, the reaction time is 10h, and the react...

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Abstract

The invention discloses a heterogeneous catalyst for synthesizing diphenyl carbonate, and a preparation method thereof, wherein the catalyst comprises a carrier, a titanium source and an organic acid,a mass ratio of the titanium source to the carrier is 10-70:90-30, a molar ratio of the titanium to the organic acid is 0.05-5:1, the titanium source is tetrabutyl titanate, tetraisopropyl titanate,titanyl sulfate, titanocene dichloride, tetraethyl titanate or dicyclopentadiene dimethyl titanium, the carrier is a ZSM-5 molecular sieve, an HZSM-5 molecular sieve, a TS-1 molecular sieve, an MCM-41molecular sieve or SiO2, and the organic acid is acetic acid, succinic acid, adipic acid, sebacic acid, terephthalic acid, benzoic acid or chlorosulfonic acid. The specific preparation method comprises: 1) dissolving a titanium source by adopting a solvent, adding a carrier, carrying out a hydrothermal synthesis reaction for 10-48 h at a temperature of 80-120 DEG C, filtering, and drying the carrier to obtain a catalyst intermediate; and 2) dissolving the catalyst intermediate in a solvent, adding an organic acid in an ice-water bath in a dropwise manner, stirring for 2-4 days at a normal temperature, filtering, washing, and drying to obtain the catalyst. The catalyst of the invention has characteristics of high activity and high selectivity.

Description

technical field [0001] The invention relates to the fields of catalytic chemistry and organic chemistry, and relates to a heterogeneous catalyst for synthesizing diphenyl carbonate and a preparation method thereof. Background technique [0002] Diphenyl carbonate is an important carbonylation intermediate. It is non-toxic, non-polluting, and an environmentally friendly chemical product. It is not only a raw material for the synthesis of polycarbonate, but also widely used as a solvent and plasticizer And pharmaceutical intermediates, etc. With the promotion and application of polycarbonate clean production technology in the world, as well as the domestic introduction of technology and self-developed large-scale polycarbonate equipment into production, the market demand for diphenyl carbonate will increase rapidly, thus making the clean production of diphenyl carbonate Ester technology has become a hot spot in research and development. [0003] The catalysts for the reactio...

Claims

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Application Information

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IPC IPC(8): C07C68/06C07C69/96B01J31/22B01J29/03B01J29/04B01J29/40B01J37/10
CPCC07C68/06B01J31/1633B01J29/0308B01J29/041B01J29/40B01J37/10B01J31/2208B01J31/2295B01J2229/18C07C69/96Y02P20/584
Inventor 魏天荣孙苏红於国伟张小元李善华陈坤徐保明
Owner 湖北三宁碳磷基新材料产业技术研究院有限公司
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