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Preparation method of core-shell structure CeO2@SiO2 load metalloporphyrin catalyst prepared by double wrapping method

A metal-loaded, shell-structured technology, applied in chemical instruments and methods, physical/chemical process catalysts, organic compounds/hydrides/coordination complex catalysts, etc., to promote activity, improve activity and selectivity, and improve stability Effect

Inactive Publication Date: 2012-04-11
HUNAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, there is no CeO with double-wrapped core-shell structure at home and abroad. 2 SiO 2 Published literature and patent applications for preparation methods of supported metalloporphyrin catalysts

Method used

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  • Preparation method of core-shell structure CeO2@SiO2 load metalloporphyrin catalyst prepared by double wrapping method
  • Preparation method of core-shell structure CeO2@SiO2 load metalloporphyrin catalyst prepared by double wrapping method
  • Preparation method of core-shell structure CeO2@SiO2 load metalloporphyrin catalyst prepared by double wrapping method

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0017] Synthesis of monocarboxyporphyrins. In a 500ml three-necked flask, add 200ml of propionic acid, 1.51g of benzaldehyde and 2.08g of 4-carboxybenzaldehyde, heat to reflux, and slowly drop in 1.36g of pyrrole with a constant pressure dropping funnel, control the flow rate, and complete the addition in 20 minutes. Under the condition of reflux, the reaction was continued for 30 minutes to complete. After the reaction solution was cooled, it was placed in the refrigerator overnight, filtered by suction, and separated by a silica gel column, and the monocarboxyporphyrin was synthesized.

[0018] Synthesis of monocarboxycobalt porphyrins. In a 250ml three-neck flask, add 100ml DMF, 0.5g monocarboxyporphyrin, heat to reflux, add 2.54g CoCl in batches within 1h 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 distill...

Embodiment 2

[0020] Double wrapped core-shell structure CeO 2 SiO 2 Synthesis of silica spheres. Weigh 5.996g Ce(NO 3 ) 3 ·6H 2 O, make a 250ml solution with deionized water. Under 500r / min mechanical stirring, NaOH solution was slowly added dropwise to Ce(NO 3 ) 3In the solution, adjust the pH value to 13, continue to stir for 30 minutes, filter with suction, disperse the filter cake in deionized water, and wash it twice with ultrasonic dispersion, and then disperse the filter cake in absolute ethanol, and wash it twice with ultrasonic. The resulting sample was dried under vacuum at 70 °C for 1 h. Transfer the dried cerium oxide powder into 200ml of 0.3mol / L sodium citrate solution, heat it in a water bath to 90°C for 3 hours under mechanical stirring at 500r / min, filter it with suction, and obtain the surface-modified nano Cerium oxide particles. In a 500ml three-neck flask, add 0.3g of nano-cerium oxide modified by sodium citrate on the surface, 40ml of deionized water, 160ml o...

Embodiment 3

[0022] Weigh 0.050g CoTMCPP, 3.50g core-shell structure CeO prepared by double wrapping method 2 SiO 2 , added to a 250ml three-necked flask with 100ml DMF solution, refluxed for 12 hours, evaporated 70ml DMF, added 70ml deionized water after cooling, filtered, washed with deionized water until colorless, and then washed with dichloromethane until Colorless, it is directly transferred to the Soxhlet extractor after being drained, and dichloromethane is used as the extracting solution to extract until it is colorless, and then dried to obtain the core-shell structure CeO prepared by the double encapsulation method. 2 SiO 2 Supported metalloporphyrin catalysts.

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Abstract

The invention relates to a preparation method of core-shell structure CeO2@SiO2 load metalloporphyrin catalyst prepared by double wrapping method, and provides a system for forming the core-shell structure CeO2@SiO2 load metalloporphyrin multi-phase catalyst by double wrapping method. The preparation method comprises the following steps of: stirring and dispersing nanometer cerium oxide particles with surfaces modified by sodium citrate, and adding tetraethyl orthosilicate (TEOS) dropwise to obtain once wrapped core-shell structure CeO2@SiO2; stirring and dispersing the once wrapped core-shell structure CeO2@SiO2 and hexadecyl ammonium bromide; adding mixed solution of the TEOS and 3-aminopropyl triethoxy silicane (APTES) to obtain doubly wrapped core-shell structure CeO2@SiO2; and linking cobalt monocarboxyl porphyrin (CoTMCPP) to a doubly wrapped core-shell structure CeO2@SiO2 carrier by amidation reaction so as to obtain the core-shell structure CeO2@SiO2 load metalloporphyrin catalyst prepared by double wrapping method. The catalyst provided by the invention has higher catalytic activity and stability for selective catalytic oxidation reaction of molecular oxygen on diphenylmethane in the absence of solvent, and the preparation method is simple and product quality is easily controlled, so that the catalyst is suitable for use in the fields such as selective oxidation reaction of hydrocarbon alkyl and synthesis of medicine intermediate and the like.

Description

technical field [0001] The invention belongs to the field of catalysts, in particular to CeO with core-shell structure prepared by a double wrapping method 2 SiO 2 Preparation method of supported metal porphyrin catalyst. Background technique [0002] Benzophenone is a commonly used fine chemical product, which is widely used as pharmaceutical intermediates, fragrance fixatives, ultraviolet absorbers for polymer materials, photosensitizers for film coatings, etc. Industrially, the synthesis routes of benzophenone mainly include Friedel-Crafts acylation method, carbonylation method, nitric acid oxidation method, etc. The acylation method requires absolute anhydrous in the reaction process, and 2-3 times the stoichiometric halogenated Brown's acid or Lewis acid is used. The equipment is seriously corroded, and the catalyst cannot be recovered; the carbonylation method not only needs to use toxic raw materials (phosgene ), it also needs to react under high temperature and hi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/26B01J35/10C07C49/786C07C45/36
Inventor 刘志刚李媛媛郭翔吉琳韬沈丹华
Owner HUNAN UNIV
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