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Preparation and application of ordered mesoporous phenolic resin polymer silver-loaded catalyst

A technology of phenolic resin and silver catalyst, applied in the field of chemical catalytic materials and chemical applications, can solve the problems of complex preparation process of catalyst carrier, application limitation of homogeneous catalyst, application limitation of metal catalyst, etc. Good chemical stability and good catalytic activity

Active Publication Date: 2018-08-17
EAST CHINA NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the further application of homogeneous catalysts is limited due to problems such as difficult recovery, troublesome separation, or metal contamination.
Previously, some supported metal catalysts have been reported for the reaction of carbon dioxide and terminal alkynes, but the further application of these metal catalysts has been limited due to factors such as low catalytic yield, harsh reaction conditions, or complex preparation process of catalyst supports.

Method used

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  • Preparation and application of ordered mesoporous phenolic resin polymer silver-loaded catalyst
  • Preparation and application of ordered mesoporous phenolic resin polymer silver-loaded catalyst
  • Preparation and application of ordered mesoporous phenolic resin polymer silver-loaded catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0026] (1) Chloromethylation of ordered mesoporous materials

[0027] Under the conditions of ice-water bath and argon protection, mix and stir 4g FDU mesoporous phenolic resin and 20g chloromethyl methyl ether, and add 29g of anhydrous aluminum chloride in three times, react under ice-water bath conditions for 24 hours, and the reaction ends Then add deionized water to quench the unreacted anhydrous aluminum chloride, wash with 300ml deionized water and 200ml acetone alternately three times after suction filtration, and then dry in a vacuum oven at 80°C for 24 hours to obtain chloromethyl FDU mesoporous phenolic resin.

[0028] (2) Amine functionalization of chloromethylated FDU mesoporous phenolic resin

[0029] Mix 4g of chloromethylated FDU mesoporous phenolic resin with 20g of methylamine, add 100ml of acetonitrile solution, and react at 83°C for 8 hours. After the reaction, the filtrate is alternately washed three times with 200ml of acetone and 300ml of deionized water...

Embodiment 2

[0036] (1) Chloromethylation of ordered mesoporous materials

[0037] Under the conditions of ice-water bath and argon protection, mix and stir 4g FDU mesoporous phenolic resin and 20g chloromethyl methyl ether, and add 29g of anhydrous aluminum chloride in three times, react under ice-water bath conditions for 24 hours, and the reaction ends Then add deionized water to quench the unreacted anhydrous aluminum chloride, wash three times alternately with 300ml deionized water and 200ml acetone after suction filtration, and then dry in a vacuum oven at a temperature of 80°C for 24 hours to obtain chloromethyl FDU mesoporous phenolic resin.

[0038] (2) Amine functionalization of chloromethylated FDU mesoporous phenolic resin

[0039] Mix 4g of chloromethylated FDU mesoporous phenolic resin with 20g of dimethylamine, add 100ml of acetonitrile solution, and react at 83°C for 8 hours. After the reaction, the filtrate is alternately washed three times with 200ml of acetone and 300ml...

Embodiment 3

[0046] 489mg (1.5mmol) cesium carbonate and 50mg (0.1mol%) the silver nano-loaded metal catalyst (FDU-Ag) that embodiment 1 prepares is put into the three-necked flask of 50ml, and carbon dioxide is filled in the balloon, to device Vacuumize and ventilate three times to fully remove the air in the device, then weigh 102 mg of phenylacetylene (1 mmol) with a syringe and extract 10 ml of anhydrous DMF solution into the device, heat to 50 ° C, and react for 18 hours. The reaction structure is:

[0047]

[0048] CO during the reaction 2 Pressure is atmospheric pressure all the time, after reaction finishes, flask is cooled to room temperature, mixed solution is carried out suction filtration and washes and separates catalyst with the deionized water of 20ml, adds the dichloromethane of 90ml in filtrate and carries out extraction three times and takes water layer, in separated Add dilute hydrochloric acid to the water layer to adjust the pH to 1, then extract with 60ml of ethyl ...

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Abstract

The invention discloses preparation and application of an ordered mesoporous phenolic resin polymer silver-loaded catalyst. The preparation of the ordered mesoporous phenolic resin polymer silver-loaded catalyst is characterized in that the catalyst takes FDU mesoporous phenolic resin introduced with chloromethyl as a carrier, the carrier is connected with amido or sulfo adsorption immobilized silver ions in a covalent bond mode, and the silver ions are reduced in situ to generate a nulvalent-silver loaded type metal catalyst. Compared with the prior art, the preparation of the ordered mesoporous phenolic resin polymer silver-loaded catalyst has the advantages that catalytic activity is good, separation is facilitated, the catalytic yield is quite high during reaction under gentle conditions, moreover, the multi-phase catalyst is easy to recycle, can be reused and is pollution-free for the environment, preparation is simple, reaction conditions are gentle, and heavy metal pollution inheterogeneous catalytic reaction of carbon dioxide and a terminal alkyne compound is solved well.

Description

technical field [0001] The invention relates to the technical field of chemical catalytic materials and chemical applications, in particular to the preparation and application of an ordered mesoporous phenolic resin polymer-loaded silver catalyst. Background technique [0002] With the acceleration of the world's industrialization, the reserves of fossil fuels, which are the main energy source of human society and the source of chemical raw materials, are decreasing day by day. The development of renewable resources has become the only way for the sustainable development of human society. Carbon dioxide is a non-toxic, harmless, abundant, cheap and easy-to-obtain carbon 1 resource. Using chemical methods to convert carbon dioxide into high value-added products has become a goal pursued by industry and academia. Among the many chemical pathways for carbon dioxide fixation, the reaction of carbon dioxide directly forming carbon-carbon bonds with terminal alkynes to form carbox...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/10B01J31/06C07C51/15C07C57/42C07C59/64C07C57/60C07C57/18C07C57/26C07D333/24
CPCB01J31/06B01J31/10C07C51/15C07C2601/14C07D333/24C07C57/42C07C59/64C07C57/60C07C57/18C07C57/26Y02P20/584
Inventor 吴海虹梅宇吴鹏
Owner EAST CHINA NORMAL UNIV
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