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Magnetic metal-organic framework material with mesoporous structure and preparation and catalysis reaction thereof

A magnetic metal and organic framework technology, which is applied in the preparation of organic compounds, organic chemistry, organic compound/hydride/coordination complex catalysts, etc., can solve the problems of difficult catalyst reuse, troublesome separation of catalyst and product, etc., to achieve Improve reuse efficiency, reduce separation costs, and save energy

Inactive Publication Date: 2015-04-29
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when MILs 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 20g of sodium silicate solution with a mass concentration of 10% and hexadecyltrimethyl bromide with a mass concentration of 0.2% at the same time under stirring conditions at a water bath temperature of 30°C Ammonium chloride (CTAB) ethanol solution 10g, after the ...

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 relates to a magnetic metal-organic framework material with a mesoporous structure and preparation and catalysis reaction thereof, belonging to the technical field of magnetic metal-organic framework materials. The preparation comprises the steps of firstly, preparing superparamagnetic Fe3O4 cores, forming a mesoporous SiO2 shell layer on the surface of each magnetic Fe3O4 core by adopting ultrasonic methods through taking cetyl trimethyl ammonium bromide as a template agent and taking sodium silicate as a silicon resource, drying, and then, removing the template agent, so as to obtain magnetic SiO2@Fe3O4 nanospheres; then, carrying out in-situ self-assembly on Cr, Fe or Al ions and terephthalic acid ligand on the surface of magnetic-core SiO2@Fe3O4 by adopting the ultrasonic methods, thereby preparing a magnetic MILs (Materials of Institute Lavoisier Frameworks)@SiO2@Fe3O4 material, of which the surface has an MILs metal-organic framework structure. During liquid-phase catalytic reaction, the material disclosed by the invention can be very easily separated from a reaction product by using an external magnetic field, so that the reuse efficiency of a catalyst is increased, and the separation cost is reduced.

Description

technical field [0001] The invention relates to a magnetic metal organic framework material with a mesoporous structure, a rapid preparation method and a catalytic application thereof, and belongs to the technical field of magnetic metal organic framework materials. Background technique [0002] Metal-organic frameworks (Materials of Institute Lavoisier Frameworks, MILs) materials with mesoporous structure are a kind of porous crystalline materials with mesoporous structure generated by self-assembly of metal ions and binary organic acid or ternary organic acid ligands. It has the characteristics of nano-scale skeleton-type regular pore structure, large specific surface area and porosity, and is widely used in catalysis, adsorption, and separation (Li Qingyuan, Ji Shengfu, Hao Zhimou. Metal-organic framework materials and their use in catalytic reactions Applications in. Advances in Chemistry, 2012,24(8):1506-1518). Discover MIL-101 series as catalysts such as Maksimchuk, h...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/28B01J13/02H01F1/01B82Y40/00B82Y30/00C07C255/41C07C253/30
Inventor 季生福蒋赛刘想李庆远
Owner BEIJING UNIV OF CHEM TECH