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Supported cupric iodide catalyst for oxidation and carbonylation and preparation method thereof

A catalyst and iodide technology, which is applied in the field of supported copper iodide catalyst and its preparation, can solve the problems of difficult separation and recycling, low catalyst activity, etc., and achieve the effects of easy recycling, high catalytic efficiency, and small catalyst loss

Inactive Publication Date: 2010-06-23
HUAZHONG UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to overcome the shortcomings of the existing carbonylation synthesis of organic carbonates, such as low catalyst activity and difficult separation and recycling, and provide a high-selectivity, long-life catalyst with high reaction efficiency, simple preparation process, and easy separation and recycling. Supported catalyst prepared by iodide, copper salt, Schiff base complex and carrier

Method used

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  • Supported cupric iodide catalyst for oxidation and carbonylation and preparation method thereof
  • Supported cupric iodide catalyst for oxidation and carbonylation and preparation method thereof
  • Supported cupric iodide catalyst for oxidation and carbonylation and preparation method thereof

Examples

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example 1

[0032] in N 2 Under protection, the chloromethyl polystyrene that will be swelled in N, N-dimethylformamide for 24 hours is added to the N, N-dimethylformamide containing 5-aminophenanthrene phenanthroline as 20wt%. In the solution, the relative content of 5-aminophenanthroline and chloromethyl polystyrene is 50wt%; heating, stirring and refluxing, after reacting for 48 hours, filtering while hot to obtain 5-aminophenanthroline grafted Chloromethyl polystyrene. in N 2 Under protection, 8.0 g of chloromethyl polystyrene grafted with 5-aminophenanthroline prepared in the above steps was added to the methanol solution of CuI and HI, and the relative content of CuI and methanol solvent was 15Wt%; CuI: The molar ratio of HI: 5-aminophenanthroline is 1:0.5:1; heating, stirring and reflux for 18 hours, and after drying, the supported catalyst with a copper content of 7.0.0-9.8wt% of the present invention can be obtained.

[0033] In the autoclave of 150ml, add 50ml methyl alcohol,...

example 2

[0035] in N 2 Under protection, the MCM-48 modified by the silane coupling agent that has been swelled in toluene for 36 hours is added to the toluene solution containing 10Wt% of 5-aminophenanthroline, and the 5-aminophenanthrene and silane coupling The relative content of the MCM-48 modified by the joint agent is 20wt%. Heating, stirring and refluxing, reacting for 38 hours, and filtering while hot to obtain the MCM-48 grafted with 5-aminophenanthroline. in N 2 Under protection, 6.0 g of the 5-aminophenanthroline grafted MCM-48 prepared in the above steps was added to the methanol solution of CuCl and KI, the relative content of CuCl and methanol solvent was 25wt%; CuCl: KI: 5 - The molar ratio of aminophenanthroline is 1:0.1:4; heating, stirring and refluxing for 10 hours, and drying to obtain the supported catalyst of the present invention with a copper content of 2.0-4.2 wt%.

[0036] In the autoclave of 150ml, add 50ml methyl alcohol, 4.6g above-mentioned supported cat...

example 3

[0038] in N 2 Under protection, the silane coupling agent-modified MCM-41 that has been swollen in ethanol for 12 hours is added to the ethanol solution containing 4-aminopyridine as 25Wt%, and the MCM modified by 4-aminopyridine and silane coupling agent The relative content of -41 is 10wt%. Heating, stirring and reflux, reacting for 68 hours, and filtering while hot to obtain 4-aminopyridine-grafted MCM-41. in N 2 Under protection, 10.0g of 4-aminopyridine-grafted MCM-41 prepared by the above steps was added to the ethanol solution of CuBr and NaI, and the relative content of CuBr and ethanol solvent was 20Wt%; CuBr: NaI: 4-aminopyridine The molar ratio is 1:1:0.8; heated, stirred and refluxed for 24 hours, and dried to obtain the supported catalyst of the present invention with a copper content of 2.8-5.8wt%.

[0039] In the autoclave of 150ml, add 50ml ethanol, 6.0g above-mentioned supported catalysts, press pressure ratio CO at room temperature: O 2 Pass a 6:1 mixed ga...

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Abstract

The invention provides a supported catalyst prepared by iodide, cupric salt, a Schiff alkali complex and a carrier as well as a preparation method and an application method thereof, aiming to overcome the disadvantages of low homogeneous phase catalyst activity and difficult separation recycle of the traditional carbonylation synthesis organic carbonate. The catalyst is prepared by preparing the carrier which is in grafting with the Schiff alkali complex in advance, and then preparing the supported catalyst with the copper content of 3-10wt% through reaction in alcoholic solution of the cupric salt and the iodide. The catalyst has the advantages of high catalysis efficiency, long service life, little corrosion, little catalyst loss, easy recovery and recycle of the catalyst and the like and has favorable industrial application prospect in the process of synthesizing methyl-carbonate, diethyl ester, dipropyl and glyceride.

Description

technical field [0001] The invention relates to a supported copper iodide catalyst for oxidative carbonylation reaction and a preparation method thereof, in particular to a catalyst prepared from iodide, copper salt and Schiff base complexes for synthesizing organic carbonates and Its preparation method and application method. Background technique [0002] Organic carbonate is an important green organic chemical product, which has many uses in organic synthesis, medicine, pesticide, solvent, fuel additive and so on. The process methods for synthesizing organic carbonates are mainly transesterification and oxidative carbonylation. Among them, the oxidative carbonylation method is a reaction using alcohol, oxygen, and carbon monoxide under the action of a catalyst. The process has the advantages of easy-to-obtain raw materials, simple process and low cost. Catalysts are key to this reaction. The Enichem company in Italy first developed the CuCl catalytic system for this re...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/122C07C69/96C07C68/00
CPCY02P20/584
Inventor 李光兴莫婉玲熊辉白荣献朱大建胡江林
Owner HUAZHONG UNIV OF SCI & TECH
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