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Metal-organic framework materials with magnetic cores and preparation and application thereof

A metal-organic framework and magnetic technology, applied in the fields of organic chemistry, microsphere preparation, inorganic material magnetism, etc., can solve the problems of troublesome separation of catalysts and products, difficult reuse of catalysts, etc., to improve reuse efficiency, reduce separation costs, The effect of shortening the time

Inactive Publication Date: 2014-01-22
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, when MOFs 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, add ammoni...

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Abstract

The invention provides metal-organic framework materials with magnetic cores and preparation and application thereof, and belongs to the technical field of magnetic metal-organic framework materials. FeCl3 6H2O is adopted for preparing superparamagnetic Fe3O4 cores, cetyl trimethyl ammonium bromide is used as a template agent, sodium silicate is used as silicon sources of SiO2 shell layers, mesoporous SiO2 shell layers are formed on the surfaces of the Fe3O4 cores by adopting an ultrasonic wave method, the template agent is removed by roasting under protection of N2 after drying, and magnetic SiO2@Fe3O4 nanospheres are prepared. The SiO2@Fe3O4 nanospheres are used as cores, an in-situ self-assembly mesh structure IRMOFs is carried out on the surfaces of the SiO2@Fe3O4 cores through Zn metal ions and organic carboxylic acid ligands by adopting the ultrasonic wave method. The novel MOFs materials can be used as catalysts of liquid phase catalysis reaction, and also have application values in the aspects of adsorption, separation, biological medicine and the like.

Description

technical field [0001] The invention relates to a metal organic framework material with a magnetic core, a rapid preparation method and application thereof, and belongs to the technical field of magnetic metal organic framework materials. Background technique [0002] Metal-organic frameworks (Metal-Organic Frameworks, MOFs) materials are a class of porous crystal materials with a multi-dimensional network structure generated by the self-assembly process of metal ions and organic ligands. Its specific surface area and porosity are widely used in catalysis, adsorption, separation, etc. (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, Phan et al. used MOF-5 as a catalyst to show excellent catalytic performance in the Friedel-Crafts alkylation reaction of toluene and benzyl bromide (Nam T.S.Phan, Ky K.A.Le, Tuan D.Phan.MOF-5as an efficient heterog...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/28B01J13/02B82Y40/00B82Y30/00H01F1/01C07C15/16C07C2/88
Inventor 季生福李庆远蒋赛施达
Owner BEIJING UNIV OF CHEM TECH
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