A nitrogen-heterocyclic carbene functionalized porous organic polymer-supported copper catalyst and its preparation method and application

A nitrogen-heterocyclic carbene and porous polymer technology, applied in the field of catalyst preparation, can solve the problems of corrosion of reaction equipment, easy loss of active components, poor recycling performance, etc., and achieve good application prospects and strong coordination ability , Excellent recycling performance

Active Publication Date: 2021-07-13
贵州宇源新能科技有限公司
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the solubility of CuCl in methanol is poor, the reaction efficiency is low, and chloride ions are highly corrosive to stainless steel reactors.
Chinese patent CN1197792A adds MgCl in the reaction solution 2 and other additives, which increase the solubility of cuprous chloride in methanol, thereby improving the catalytic performance, but still do not solve the problems such as the corrosion of reaction equipment
However, the supported catalyst prepared by surface covalent bond modification often leads to the easy loss of active components and poor recycling performance due to the uneven distribution of active components and the distribution of active components on the surface of the carrier.

Method used

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  • A nitrogen-heterocyclic carbene functionalized porous organic polymer-supported copper catalyst and its preparation method and application
  • A nitrogen-heterocyclic carbene functionalized porous organic polymer-supported copper catalyst and its preparation method and application
  • A nitrogen-heterocyclic carbene functionalized porous organic polymer-supported copper catalyst and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] Example 1 An application of a nitrogen heterocyclic carbon functionalized porous organic polymer load copper catalyst in a liquid alcohol oxide reaction, as follows:

[0048] (1) Preparation of vector (PNHC-1)

[0049] 10 g of 1-butyl-3-methylimidazole salt and 2.5 g of deionized water were thoroughly stirred at room temperature to obtain a 1-butyl-3-methylimidazole solution, and then sequentially added to the solution. 0.461 g of two (1-imidazolyl) methane and 0.739 g of 1,3,5-tris (bromomethyl) benzene, the reaction was stirred at room temperature (25 ° C, the following) was stirred for 2 hours, and then the reaction Liquid lifting to 100 ° C, stirring at 100 ° C for 36 hours, and the reaction was completed, and the lump solid was obtained, and the resulting block solid was washed 6 times with water, and then washed with anhydrous ethanol 3 times, filtered, resulting solid After vacuum dried overnight at 60 ° C, the porous polymer carrier (named PNHC-1) was obtained, and ...

Embodiment 2

[0056] Example 2 An application of a nitrogen heterocyclic cartridge functionalized porous organic polymer load copper catalyst in a liquid alcohol oxide, the steps are as follows:

[0057] (1) Preparation of vector (PNHC-2)

[0058] 15 g of 1-propyl-3-methylimidazol bromorine salt and 3.0 g of deionized water were thoroughly stirred at room temperature to give 1-propyl-3-methylimidazol bromine solution, and then add 0.953 to the solution. G of the b (1-imidazolyl) methane and 1.447 g of 1,2,4,5-tetra (bromomethyl) benzene, pre-polymerization was performed at room temperature stirring for 1 hour, and then the reaction liquid temperature was raised to 90 ° C, The reaction was carried out at 90 ° C for 48 hours; after the reaction was completed, the bulk solid was obtained, and the bulk solid was washed 6 times with water, and then the resulting solid was filtered, the resulting solid was dried overnight after drying overnight with ethanol. The polymer carrier (PNHC-2), the mass of ...

Embodiment 3

[0064] Example 3 A nitrogen heterocyclic carbin functionalized porous organic polymer load copper catalyst in a liquid alcoholytic carbyllation reaction, as follows:

[0065] (1) Preparation of the vector (PNHC-3)

[0066] 20 g of 1-hexyl-3-methylimidazole nitrate and 2.8 g of deionized water were thoroughly stirred at room temperature to give 1-hexyl-3-methylimidazole nitrate solution, and then add 0.960 g from the solution. 2 (1-imidazolyl) methane and 1.540 g of 1,3,5-tris (bromomethyl) benzene, the reaction was stirred at room temperature for 1 hour, then the reaction liquid was raised to 115 ° C, at 115 ° C The mixture was stirred for 24 hours; after the reaction was completed, the bulk solid was obtained, and the bulk solid was washed 6 times with water, and then the resulting solid was purified 3 times, filtered, the resulting solid was dried in vacuo to overnight, and the porous polymer carrier was obtained. PNHC-3), the mass of PNHC-3 was 2.52 g, and the elemental analysi...

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Abstract

The invention relates to the technical field of catalyst preparation, in particular to a nitrogen-heterocyclic carbene functionalized porous organic polymer-supported copper catalyst and a preparation method and application thereof. Use imidazole ionic liquid as solvent, water as co-solvent, bis(1-imidazolyl)methane and polybromomethyl aromatic hydrocarbon as comonomers, pre-polymerize at room temperature for 0.5-3 hours, then polymerize at 80-140°C 12-48 hours to obtain a porous polymer containing imidazolium salt; then, using the porous polymer to support cuprous salt under alkaline conditions to obtain azacyclic carbene functionalized porous organic polymer-supported copper catalyst. The porous catalyst has the characteristics of large specific surface area and wide pore size distribution, and can efficiently catalyze the oxidative carbonylation of methanol and ethanol to synthesize dialkyl carbonate. Compared with traditional supported catalysts, the catalyst has high activity, is not easy to lose, and has a long cycle life, and is expected to be used in practical industrial production.

Description

Technical field [0001] The present invention relates to the preparation of catalysts, and more particularly to a nitrogen-ring cofbin functionalized porous organic polymer load copper catalyst and a preparation method thereof and a carbylcarbonization reaction in a liquid alcohol. Background technique [0002] Organic carbonate is a kind of "green" chemical product with high value, can replace highly toxic and carcinogeneous photomics, dimethyl sulfate as a methylated reagent, carbonylation reagent, and the like to produce many high value-added chemical products, There are many uses in organic synthesis, pharmaceutical, pesticides, solvents, fuel additives. Industrial preparation of diethylene carbonate is photomiggery, ester exchange method, and carbarbonylation method (including liquid phase method and gas phase). Among them, the carbarbonylation method is carried out using alcohol, oxygen, and carbon monoxide under the action of catalyst. This process has the characteristics o...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22B01J35/10C07C69/96C07C68/00
CPCY02P20/54
Inventor 雷以柱李志王毅红陈定梅万亚荔田茂军兰国松
Owner 贵州宇源新能科技有限公司
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