Porous ionic polymer heterogeneous catalyst and method for catalytically synthesizing N-formamide by using porous ionic polymer heterogeneous catalyst

An ionic polymer, heterogeneous catalyst technology, applied in organic compound/hydride/coordination complex catalysts, physical/chemical process catalysts, chemical instruments and methods, etc. Repeated use and other problems, to achieve the effects of good physical and chemical stability, low cost of raw materials, and simple product separation and purification process

Inactive Publication Date: 2021-01-05
GUANGDONG UNIV OF PETROCHEMICAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] The purpose of the present invention is to provide a method with a high specific surface area for the problems of metal catalysts, harsh reaction conditions, complex separation and purification of products, difficult recovery and reuse of catalysts,

Method used

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  • Porous ionic polymer heterogeneous catalyst and method for catalytically synthesizing N-formamide by using porous ionic polymer heterogeneous catalyst
  • Porous ionic polymer heterogeneous catalyst and method for catalytically synthesizing N-formamide by using porous ionic polymer heterogeneous catalyst
  • Porous ionic polymer heterogeneous catalyst and method for catalytically synthesizing N-formamide by using porous ionic polymer heterogeneous catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037] Embodiment 1: preparation of porous ionic polymer catalyst

[0038] (1) Add 5mmol of 1,1'-bi-2-naphthol, 20mmol of anhydrous ferric chloride and 20mL of anhydrous 1,2-dichloroethane into a 50mL Schlenk tube, and repeatedly Replace the air in the tube, add 20mmol of dimethylformal under nitrogen condition, after sealing, put the reaction system at room temperature and stir for 30min, then heat the oil bath to 100°C to carry out the first contact reaction, after 24h, cool and pass Filtration, washing, Soxhlet extraction and vacuum drying to obtain a porous organic polymer containing phenolic hydroxyl groups;

[0039] (2) Add 300 mg of phenolic hydroxyl-containing porous organic polymer obtained in step (1), 414 mg of potassium carbonate and 634 mg of bromobutyltriethylammonium bromide to 15 mL of anhydrous N,N'-dimethylformamide , heated to 140°C and continued to stir and react for 24 hours, filtered the obtained precipitate, washed the filter cake with demethanol, aceto...

Embodiment 2

[0040] Embodiment 2: preparation of porous ionic polymer catalyst

[0041] (1) Add 10mmol of 2,3-dihydroxynaphthalene, 20mmol of anhydrous ferric chloride and 40mL of anhydrous chloroform into a 100mL Schlenk tube, and repeatedly replace the air in the tube with nitrogen. Add 20mmol of dimethylformal, after sealing, place the reaction system at room temperature and stir for 30min, then heat the oil bath to 80°C for the first contact reaction, after 36h, cool, filter, wash, Soxhlet extraction and vacuum Dry to obtain a porous organic polymer containing phenolic hydroxyl groups;

[0042] (2) Add 150 mg of the porous organic polymer containing phenolic hydroxyl groups obtained in step (1), 360 mg of sodium carbonate and 380 mg of 1-(4-bromoethyl) pyridinium chloride into 20 mL of anhydrous tetrahydrofuran, and heat to 100 Continue to stir and react at ℃ for 48 hours, filter the obtained precipitate, wash the filter cake with demethanol, acetone and ionized water successively for...

Embodiment 3

[0043] Embodiment 3: preparation of porous ionomer catalyst

[0044] (1) Add 2mmol of 4,4′-isopropylidene biphenol, 10mmol of anhydrous aluminum trichloride and 20mL of anhydrous dichloromethane into a 100mL Schlenk tube, and repeatedly replace the air in the tube with nitrogen, After sealing under nitrogen, the reaction system was stirred at room temperature for 30 minutes, and then heated to 80 ° C in an oil bath for the first contact reaction. After 48 hours, it was cooled, filtered, washed, Soxhlet extracted and dried in vacuo to obtain Porous organic polymers of phenolic hydroxyl groups;

[0045] (2) Add 200 mg of the phenolic hydroxyl-containing porous organic polymer obtained in step (1), 580 mg of potassium carbonate and 620 mg of bromobutyltriethylammonium bromide to 25 mL of anhydrous N,N'-dimethylformamide , heated to 80°C and continued to stir and react for 48 hours, filtered the obtained precipitate, washed the filter cake with demethanol, acetone and ionized wat...

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Abstract

The invention discloses a porous ionic polymer heterogeneous catalyst and a method for catalytically synthesizing N-formamide by using the porous ionic polymer heterogeneous catalyst, and provides a method for preparing an N-formamide compound by using the porous ionic polymer catalyst as a heterogeneous catalyst to catalyze carbon dioxide, organic amine and hydrogen-containing silane epoxide to carry out N-formylation reaction. The preparation method is green, environment-friendly, simple, efficient and low in raw material cost; the catalyst has an excellent pore channel structure, good physical and chemical stability, strong carbon dioxide enrichment capability and highly dispersed ionic liquid active centers; the catalyst is simple and efficient in technological process, very mild in condition and safe to operate; no organic solvent or additive is added in the catalytic reaction process so that the catalyst is environment-friendly; low-concentration carbon dioxide can be directly used as a raw material so that the cost and the energy consumption for obtaining high-purity carbon dioxide are reduced; the product separation and purification process is simple, the catalyst is easy to recover and has good stability, and repeated recycling can be achieved.

Description

technical field [0001] The invention relates to a heterogeneous catalytic method for N-formamide compounds, in particular to a method for preparing N-formamide compounds by using carbon dioxide and organic amines as raw materials and porous ionic polymers as heterogeneous catalysts. Background technique [0002] Carbon dioxide is a major greenhouse gas, and its massive emission has led to the aggravation of the greenhouse effect. At the same time, carbon dioxide is also a cheap, abundant and safe carbon resource. With the popularization of the concept of sustainable development, the rational resource utilization of carbon dioxide has received more and more attention in recent years. In recent years, the carbon dioxide capture, conversion, utilization and storage (CCUS) strategy has gradually developed into a mainstream way of artificially recycling carbon resources (Acc. Chem. Res. 2017, 50, 472-475). In particular, the use of chemical methods to convert carbon dioxide int...

Claims

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Application Information

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IPC IPC(8): B01J31/06B01J35/10C07C233/03C07C231/10
CPCB01J31/06B01J35/10C07C231/10Y02P20/584
Inventor 陈亚举纪红兵任清刚
Owner GUANGDONG UNIV OF PETROCHEMICAL TECH
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