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Preparation method of monatomic dispersion catalyst with high catalytic performance

A catalyst and atomic technology, which is applied in the field of preparation of SiO2 microsphere-supported highly dispersed metal cobalt atom catalysts, to achieve the effect of improving activity and selectivity, high stability and good catalytic performance

Inactive Publication Date: 2014-02-12
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there are no public documents and patent applications about the method of preparing highly dispersed cobalt atom catalysts by metalloporphyrin immobilization method at home and abroad.

Method used

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  • Preparation method of monatomic dispersion catalyst with high catalytic performance
  • Preparation method of monatomic dispersion catalyst with high catalytic performance
  • Preparation method of monatomic dispersion catalyst with high catalytic performance

Examples

Experimental program
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Embodiment 1

[0017] Synthesis of monocarboxyporphyrins. In a 500 mL three-neck flask, add 250 mL of propionic acid, 5.565 g of benzaldehyde and 2.625 g of 4-carboxybenzaldehyde, heat to reflux, slowly drop 4.69 g of pyrrole into the flask with a constant pressure dropping funnel, control the flow rate, add 20 min use up. Under the condition of reflux, the reaction was continued for 30 min. After the reaction solution was cooled, it was placed in the refrigerator overnight, filtered with suction, and separated by a silica gel column to synthesize monocarboxyporphyrin.

[0018] Synthesis of monocarboxycobalt porphyrins. In a 250 mL three-neck flask, add 100 mL DMF, 1.0 g monocarboxyporphyrin, heat to reflux, add 2.54 g CoCl in batches within 1 h 2 ·6H 2 O. After the addition, point the plate to monitor the reaction progress, and stop the reaction when the raw material point disappears. After the reaction solution is cooled, add 2-3 times the volume of distilled water, let it stand overn...

Embodiment 2

[0020] Amino modified SiO 2 Synthesis of silica spheres.

[0021] Weigh 1 g SiO 2 Disperse in 30 mL toluene, ultrasonically disperse for 10 min, stir magnetically, raise the temperature to 60 °C, slowly add the mixed solution of (12 mL APTES + 15 mL toluene) dropwise, and react for 24 h. Wash twice with 30 mL of toluene and 30 mL of methanol, and dry under vacuum at 80 °C overnight. The resulting product is referred to as SiO 2 -NH 2 .

Embodiment 3

[0023] Weigh 0.010 g CoTPCPP, 0.1 g amino-modified SiO 2 Microspheres, added to a solution containing 20 mL CH 2 Cl 2 solution in a 50 mL one-necked flask, reflux for 24 h, cool, and then use 30 mL CH 2 Cl 2 and 30 mL ethanol twice, at 80 o C was dried in vacuum for 12 h, and the obtained catalyst was abbreviated as SiO 2 -NH 2 -CoTPCPP. Weigh 0.01 g SiO 2 -NH 2 -CoTPCPP is installed in the reaction tube, and the temperature is raised to 800 o C, calcined for 1 h, and N was passed through the whole process 2 protection, and then naturally cooled to room temperature, the resulting product is referred to as SiO 2 -NH 2 -CoTPCPP / AC.

[0024] Similarly, the prepared SiO 2 -NH 2 / AC, SiO 2 -NH 2 -Co 2+ / AC and CoTPCPP / AC.

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Abstract

The invention belongs to the technical field of catalysis and relates to a method for preparing a monatomic cobalt catalyst by roasting silicon dioxide pellets and immobilizing metalloporphyrin. The method is realized by adopting the following technical scheme: namely stirring and dispersing nano silicon dioxide particles, dropwise adding 3-aminopropyl triethoxy silane, so as to obtain amino modified SiO2 pellets, then linking monocarboxyl metalloporphyrin (CoTPCPP) onto an amino modified SiO2 carrier through organic complexing, carbonizing porphyrin through high-temperature calcination in an inert atmosphere, and loading highly dispersed cobalt atoms onto the amino modified SiO2 pellets, thus an amino modified silicon dioxide pellet loaded monatomic cobalt catalyst is obtained. The monatomic dispersion catalyst has high catalytic activity and stability on a molecular oxygen selective ethylbenzene catalytic oxidation reaction in absence of solvent; meanwhile, a preparation method is simple, and product quality can be easily controlled, so that the monatomic dispersion catalyst is applicable to the fields of alkane selective oxidation reactions and synthesis of medical intermediates.

Description

technical field [0001] The invention belongs to the field of catalysts, in particular to modified SiO 2 The invention discloses a preparation method of a highly dispersed metal cobalt atom catalyst supported by microspheres. Background technique [0002] Usually, the active centers of solid catalysts are limited to the exposed atoms on the surface, while a large number of bulk atoms cannot participate in the reaction, resulting in low catalyst activity and waste of active components. Therefore, in order to improve the activity of catalysts and reduce the amount of active ingredients used, in some catalyst preparation processes, the active ingredients can be distributed in a single layer as much as possible by selecting carriers with high specific surface area, such as silica gel, molecular sieves, and activated carbon. However, in the actual catalyst preparation process, due to the high energy of single atoms, agglomeration is prone to occur during calcination or reaction, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/75C07C27/12C07C33/22C07C29/50C07C49/78C07C45/36
Inventor 刘志刚吉琳韬汪秋安
Owner HUNAN UNIV
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