Preparation method and application of diphenyl carbonate synthesis catalyst

A diphenyl carbonate and catalyst technology, which is applied in the field of preparation of diphenyl carbonate synthesis catalysts, can solve the problems of low selectivity of catalytically active target products, low selectivity of target products, low industrial application value, etc., and achieve non-corrosiveness , easy separation, high selectivity

Active Publication Date: 2013-12-25
昆明理工大学设计研究院有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Organic titanates are sensitive to moisture, have poor stability, and have low industrial application value; alkali or alkali metal compounds and Lewis acid catalysts have low catalytic activity and target product selectivity, and are corrosive, making it difficult to achieve industrial applications; Mg -Al hydrotalcite has high catalytic activity, but because the basicity of the catalyst promotes the formation of anisole at the same time, the selectivity of the target product is low; the microporous molecular sieve with a small silicon-aluminum ratio has strong acidity and good catalytic activity, but It also makes the by-product anisole easier to generate, therefore, the target product selectivity of the transesterification reaction is also very low

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0014] Example 1: The preparation method of this diphenyl carbonate synthesis catalyst, concrete operations are as follows:

[0015] (1) According to the ratio of adding 20ml of distilled water to 1mmol of the total molar amount of zinc and copper metal ions, dissolve zinc nitrate hexahydrate and copper nitrate trihydrate in distilled water, wherein the molar ratio of zinc to copper is 1:1. Add 20ml of absolute ethanol to trimellitic acid Dissolve trimesic acid in absolute ethanol;

[0016] (2) Mix the above two solutions under stirring so that the molar ratio of trimesic acid to zinc and copper ions is 1:1, then transfer the mixed solution into a crystallization kettle and react at 100°C for 24 hours;

[0017] (3) After the reaction is completed, filter, wash the solid three times with dimethylformamide, and dry at 160°C for 15 hours to obtain a diphenyl carbonate synthesis catalyst;

[0018] (4) The catalyst is used to catalyze the synthesis of diphenyl carbonate from meth...

Embodiment 2

[0019] Example 2: The preparation method of this diphenyl carbonate synthesis catalyst, concrete operations are as follows:

[0020] (1) According to the ratio of adding 40ml distilled water to 1mmol of the total molar amount of zinc and copper metal ions, dissolve zinc nitrate hexahydrate and copper nitrate trihydrate in distilled water, wherein the molar ratio of zinc to copper is 1:5. Add 40ml of absolute ethanol to trimellitic acid Dissolve trimesic acid in absolute ethanol;

[0021] (2) Mix the above two solutions under stirring so that the molar ratio of trimesic acid to zinc and copper ions is 1:3, then transfer the mixed solution into a crystallization kettle and react at 90°C for 36 hours;

[0022] (3) After the reaction is completed, filter, wash the solid with dimethylformamide for 3 times, and dry at 160°C for 10 hours to obtain a diphenyl carbonate synthesis catalyst;

[0023] (4) The catalyst is used to catalyze the synthesis of diphenyl carbonate from methyl ...

Embodiment 3

[0024] Example 3: The preparation method of this diphenyl carbonate synthesis catalyst, concrete operations are as follows:

[0025] (1) Add 80ml of distilled water to 1mmol of the total molar amount of zinc and copper metal ions, and dissolve zinc nitrate hexahydrate and copper nitrate trihydrate in distilled water, wherein the molar ratio of zinc to copper is 1:9. Add 80ml of absolute ethanol to trimellitic acid Dissolve trimesic acid in absolute ethanol;

[0026] (2) Mix the above two solutions under stirring so that the molar ratio of trimesic acid to zinc and copper ions is 1:5, then transfer the mixed solution into a crystallization kettle, and react at 130°C for 12 hours;

[0027] (3) After the reaction is completed, filter, wash the solid with dimethylformamide for 4 times, and dry at 200°C for 12 hours to obtain a catalyst for the synthesis of diphenyl carbonate;

[0028] (4) The catalyst is used to catalyze the synthesis of diphenyl carbonate from methyl carbamate...

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PUM

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Abstract

The invention discloses a preparation method of a diphenyl carbonate synthesis catalyst. The catalyst belongs to metal organic framework compounds. In the catalyst, an organic framework catalyst is formed by coordinating organic ligand trimesic acid and zinc-copper bimetal ions, and corrosion and pollution are avoided; the catalyst is used for catalyzing the synthesis of diphenyl carbonate from methyl carbamate and phenol, and the selectivity on a target product is relatively high; the catalyst has good stability, is easy to regenerate and can be repeatedly used for more than three times without obviously reducing the yield of diphenyl carbonate; the framework structure is basically kept complete and is easy to separate and recover; the application prospect is good.

Description

technical field [0001] The invention relates to a preparation method and application of a catalyst for synthesizing diphenyl carbonate, in particular to a zinc-copper bimetal organic framework catalyst for synthesizing diphenyl carbonate from methyl carbamate and phenol and a preparation method thereof. Background technique [0002] Diphenyl carbonate is an important intermediate in the synthesis of polycarbonate, which can be used in the synthesis of isocyanate, polyparacarbonyl benzoate, polyaryl carbonate, and can also be used as a plasticizer, solvent and heat carrier for polyester, etc. . At present, the main methods of synthesizing diphenyl carbonate are: phosgene method, oxidative carbonylation method, transesterification method and so on. The raw material phosgene of the phosgene method is highly toxic and corrosive, and it is used for the synthesis of diphenyl carbonate. Difficult to remove; transesterification methods mainly include dimethyl carbonate and phenol ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/22C07C69/96C07C68/00
CPCY02P20/582
Inventor 赵文波覃显业刘艳娜李艳红孙彦琳
Owner 昆明理工大学设计研究院有限公司
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