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Magnetic zeolite imidazate metal organic skeletal material, preparation thereof and application to liquid phase condensation catalytic reaction

A metal-organic framework and zeolite imidazolate technology, which is applied in organic compound/hydride/coordination complex catalysts, preparation of organic compounds, organic chemistry, etc., can solve problems such as difficulty in reusing catalysts, troublesome separation of catalysts and products, etc. , to achieve the effect of improving reuse efficiency, reducing separation cost, and good application prospects

Inactive Publication Date: 2014-03-19
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when ZIFs are used as catalysts for liquid-phase reactions, the separation of catalysts and products after the reaction is troublesome, which brings certain difficulties to the reuse of catalysts.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Weigh 13.4g FeCl 3 ·6H 2 O was dissolved in 86.6g of deionized water to make a solution, and 4.1g of sodium acetate was weighed and dissolved in 45.9g of ethylene glycol to make a solution. At the temperature of a water bath at 30°C and under stirring conditions, it was added dropwise to the solution containing N 2 In the protected reactor, after the dropwise addition, the mixed solution was put into an autoclave, crystallized at 180°C for 8 hours, then cooled naturally, washed with deionized water and ethanol three times, and dried in vacuum at 60°C for 8 hours. The obtained magnetic Fe 3 o 4 particles.

[0020] (2) Weigh the prepared magnetic Fe 3 o 4 Add 5.8g of granules to 44.2g of ethanol, add dropwise 20g of sodium silicate solution with a mass concentration of 5% and cetyltrimethyl bromide with a mass concentration of 0.2% at the same time at a water bath temperature of 30°C under stirring conditions Ammonium chloride (CTAB) ethanol solution 5g, after t...

Embodiment 2

[0025] (1) Weigh 20.3g FeCl 3 ·6H 2 O was dissolved in 79.7g of deionized water to make a solution, and 6.2g of sodium acetate was weighed and dissolved in 43.8g of ethylene glycol to make a solution. At the temperature of a water bath at 30°C and under stirring conditions, it was added dropwise to the solution containing N 2 In the protected reactor, after the dropwise addition, the mixed solution was put into an autoclave, crystallized at 180°C for 8 hours, then cooled naturally, washed with deionized water and ethanol three times, and dried in vacuum at 60°C for 8 hours. The obtained magnetic Fe 3 o 4 particles.

[0026] (2) Weigh the prepared magnetic Fe 3 o 4 Add 6.9g of granules to 43.1g of ethanol, add dropwise 20g of sodium silicate solution with a mass concentration of 10% and cetyltrimethyl bromide with a mass concentration of 0.2% at the same time at a water bath temperature of 30°C under stirring conditions Ammonium chloride (CTAB) ethanol solution 10g, after...

Embodiment 3

[0031] (1) Weigh 27.0g FeCl 3 ·6H 2 O was dissolved in 73.0g deionized water to make a solution, and 8.2g of sodium acetate was weighed and dissolved in 41.8g of ethylene glycol to make a solution, which was added dropwise at the temperature of a water bath at 30°C under stirring conditions 2 In the protected reactor, after the dropwise addition, the mixed solution was put into an autoclave, crystallized at 180°C for 8 hours, then cooled naturally, washed with deionized water and ethanol three times, and dried in vacuum at 60°C for 8 hours. The obtained magnetic Fe 3 o 4 particles.

[0032] (2) Weigh the prepared magnetic Fe 3 o 4 Add 9.3g of granules to 40.7g of ethanol, add dropwise 15g of sodium silicate solution with a mass concentration of 15% and cetyltrimethyl bromide with a mass concentration of 0.2% at the same time at a water bath temperature of 30°C under stirring conditions Ammonium chloride (CTAB) ethanol solution 15g, after the dropwise addition, ammonia so...

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Abstract

The invention provides a magnetic zeolite imidazate metal organic skeletal material, preparation thereof and application to liquid phase condensation catalytic reaction, and the invention belongs to the field of magnetic zeolite imidazate metal organic skeletal material technology. The invention employs FeCl3.6H2O to prepare Fe3O4 core with superparamagnetism, and cetyl trimethyl ammonium bromide is used as a template, and sodium silicate is used as silicon source of SiO2 casing layer, and a SiO2 casing layer with meso pores is formed on Fe3O4 using supersonic wave, and template is roasted and removed under N2 after drying, and magnetic SiO2@Fe3O4 nanospheres are prepared. imidazate metal organic skeletal structure is formed on surface of magnetic core SiO2@Fe3O4 with Zn or Co metal ions and 2-methylimidazole or benzimidazole ligand by in-situ self assembly using supersonic wave, and the magnetic ZIFs@SiO2@Fe3O4 material is obtained. The ZIF material is used for liquid phase condensation reaction catalysis.

Description

technical field [0001] The invention relates to a magnetic zeolite imidazolate metal-organic framework material, a rapid preparation method and application thereof, and belongs to the technical field of magnetic zeolite imidazolate metal-organic framework materials. Background technique [0002] Zeolitic imidazolate metal-organic frameworks (Zeolitic Imidazolate Frameworks, ZIFs) materials are a class of porous crystal materials with a zeolite-like pore structure generated by self-assembly of metal ions and imidazole (or imidazole derivatives) organic ligands. Its skeleton-type regular pore structure, large specific surface area, and porosity are widely used in catalysis, adsorption, and separation (Li Qingyuan, Ji Shengfu, Hao Zhimou. Metal-organic framework materials and their applications in catalytic reactions . Advances in Chemistry, 2012,24(8):1506-1518). For example, Zakzeski et al. used Co-ZIF-9 as a catalyst to show excellent catalytic performance in the selective ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28C07C255/35C07C253/30
Inventor 季生福李庆远蒋赛施达
Owner BEIJING UNIV OF CHEM TECH
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