A kind of preparation method and application of magnetic complex-based catalyst

A catalyst and material-based technology, applied in the field of preparation of Fe3O4MOFAg, can solve the challenges of high energy consumption of production equipment, hindering application, long preparation time, etc., and achieve the effect of improving preparation efficiency, high catalytic activity, and avoiding agglomeration

Inactive Publication Date: 2016-07-06
UNIV OF JINAN
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, its limitation is that the preparation time is relatively long, and high temperature and high pressure steps are required. The challenge of production equipment and high energy consumption hinders the application of this method in industrial production.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0030] Embodiment 1 A kind of surface sulfhydrylated Fe 3 o 4 Preparation method of microspheres

[0031] Add 1.40g of ferric chloride hexahydrate and 4.0g of ammonium acetate to 50mL of ethylene glycol, ultrasonically disperse for 5min, transfer the dispersion to a polytetrafluoroethylene autoclave, raise the temperature to 200°C, keep it warm for 6h, and cool to room temperature, a black viscous liquid was obtained, which was dissolved and washed 3 times with 30 mL of water and ethanol mixture with a volume ratio of 1:1, and was separated by magnet adsorption each time, and dried to obtain Fe 3 o 4 Microspheres;

[0032] Take Fe 3 o 4 Add 0.32 g of microspheres, add 20 mL of ethanol mixed solution of thioglycolic acid with a mass fraction of 0.6%, shake at room temperature for 24 hours, separate by magnetic adsorption, wash with ethanol, and obtain surface thiolated Fe 3 o 4 Microspheres; the surface thiol Fe 3 o 4 Microspheres with a particle size of 170nm.

Embodiment 2

[0033] Embodiment 2 A kind of surface sulfhydrylated Fe 3 o 4 Preparation method of microspheres

[0034] Add 1.50g of ferric chloride hexahydrate and 4.2g of ammonium acetate to 60mL of ethylene glycol, ultrasonically disperse for 5min, transfer the dispersion to a polytetrafluoroethylene autoclave, raise the temperature to 200°C, and keep it warm for 6-8h , cooled to room temperature, to obtain a black viscous liquid, with a volume ratio of 1:1 water and ethanol mixture 30mL stripping and washing 3 times, each time separated by magnetic adsorption, dried to obtain Fe 3 o 4 Microspheres;

[0035] Take Fe 3 o 4 Add 0.32 g of microspheres, add 30 mL of ethanol mixed solution of thioglycolic acid with a mass fraction of 0.6%, shake at room temperature for 24 hours, separate by magnetic adsorption, and wash with ethanol to obtain surface thiolated Fe 3 o 4 Microspheres; the surface thiol Fe 3 o 4 Microspheres with a particle size of 150nm.

Embodiment 3

[0036] Embodiment 3 A kind of surface sulfhydrylated Fe 3 o 4 Preparation method of microspheres

[0037] Add 1.45g of ferric chloride hexahydrate and 4.1g of ammonium acetate to 55mL of ethylene glycol, ultrasonically disperse for 5min, transfer the dispersion to a polytetrafluoroethylene autoclave, raise the temperature to 200°C, and keep it warm for 6-8h , cooled to room temperature, to obtain a black viscous liquid, with a volume ratio of 1:1 water and ethanol mixture 30mL stripping and washing 3 times, each time separated by magnetic adsorption, dried to obtain Fe 3 o 4 Microspheres;

[0038] Take Fe 3 o 4 Add 0.32 g of microspheres, add 25 mL of ethanol mixed solution of thioglycolic acid with a mass fraction of 0.6%, shake at room temperature for 24 h, separate by magnetic adsorption, and wash with ethanol to obtain surface thiolated Fe 3 o 4 Microspheres; the surface thiol Fe 3 o 4 Microspheres with a particle size of 160nm.

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Abstract

The invention relates to a preparation method of a magnetic complex-based catalyst, which belongs to the technical field of material science, nano-material, chemical industry and catalysis. According to the invention, surface-sulfhydrylated Fe3O4 microspheres and an organic compound HL are prepared to obtain Fe3O4@MOF under room temperature through ultrasonic treatment; Fe3O4@MOF is used for dipping a silver nitrate solution, ultraviolet lamp light is used for irradiation, so that the magnetic complex-based catalyst with surface cured with nano Ag can be prepared, which is Fe3O4@MOF@Ag. The magnetic complex-based catalyst has excellent catalytic reduction performance for the nonsaturated organic compound, an applied magnetic field is used for realizing high efficiency separating of the catalyst and the liquid phase reaction system and cycle use, production and usage cost can be reduced, and the magnetic complex-based catalyst has good application prospect in a reduction reaction.

Description

technical field [0001] The invention relates to a method for preparing a magnetic complex-based catalyst and its application, in particular to a Fe 3 o 4 The preparation method and application of MOFAg belong to the technical fields of material science, nanometer material, metal organic complex, chemical industry, catalysis and the like. Background technique [0002] Nanomaterials have attracted more and more attention because of their special properties and wide applications. Among them, due to the quantum size effect, surface interface effect, small size effect and macroscopic quantum tunneling effect of nano-silver, it has a wide range of applications in many technical fields such as catalysis. Because preparation is the premise and foundation of application, the preparation of nano-silver is one of the key research contents of workers in the technical fields of material science, nano-materials, metal-organic complexes, chemical industry, and catalysis. [0003] Due to...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/28C07C211/52C07C209/36H01F1/42C02F1/70C02F101/38
Inventor 王志玲陈元俊徐在香余珍李相宏崔玉杨小风刘志连郑鲁沂
Owner UNIV OF JINAN
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