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Mesoporous silicon dioxide-loaded metal phthalocyanine catalyst and preparation method thereof

A mesoporous silica and metal-loaded technology, which is applied in metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, chemical instruments and methods, etc. Few types of phthalocyanines, fixed pore structure, etc., to achieve the effect of highlighting the effect of biological multiplication modification, rich types of metal ions, and mild catalytic reaction conditions

Active Publication Date: 2017-05-31
SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Due to the disadvantages of easy formation of dimers that reduce the catalytic ability and secondary pollution caused by difficult recycling, many scholars have studied the loading of metal phthalocyanines. The loading carriers are generally traditional molecular sieves, cellulose, and sol-gel. The dispersibility of phthalocyanine increases the efficiency of catalyst use; on the other hand, the supported metal phthalocyanine prepared by using traditional support supports has disadvantages such as low loading rate, low catalytic activity, and difficult separation.
For example, Fan Yafang et al. first activated the Y-type molecular sieve at high temperature, and then Fe 2+ Substitution of Na + The method is prepared into metal Fe 2+ Ion-modified Y-type molecular sieves were finally synthesized in situ to prepare Y-type molecular sieve-supported iron phthalocyanines, but due to Fe 2+ Replacement is difficult and the content is low, and the pore structure is fixed, the prepared supported metal phthalocyanine species are few, the catalytic selectivity is low, and it cannot meet the practical requirements

Method used

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  • Mesoporous silicon dioxide-loaded metal phthalocyanine catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment l

[0019] 1) Dissolve 10 g of tetraethyl orthosilicate and 0.5 g of Tween-80 in 5 mL of ethanol to form a solution, and then slowly add it to 30 mL of a solution containing 10 g of copper disulfonic acid phthalocyanine and 0.5 g of Tween-80 Stir in deionized water for 2 hours at room temperature, then transfer the mixture to an autoclave, crystallize at 120°C for 72 hours, cool to room temperature, filter, wash with deionized water for 3 times, and dry the solid in a vacuum dryer at 60°C After 12 hours, it was calcined in a muffle furnace at 550° C. for 3 hours to obtain copper (II) ion-modified mesoporous silica microspheres.

[0020] 2) After mixing 20 g copper(II) ion-modified mesoporous silica microspheres with 0.001 g ammonium molybdate, 1 g phthalic anhydride, 1 g ammonium chloride, and 3 g urea, place In a reaction kettle containing 70 mL of xylene, reflux reaction at 130°C for 2 hours under slow stirring conditions, after cooling to room temperature, suction filtration, w...

Embodiment 2

[0022] 1) Dissolve 10 g of tetraethyl orthosilicate and 0.5 g of Tween-80 in 5 mL of ethanol to form a solution, and then slowly add it to 30 mL of a solution containing 10 g of cobalt disulfonic acid phthalocyanine and 0.5 g of Tween-80 Stir in deionized water for 2 hours at room temperature, then transfer the mixture to an autoclave, crystallize at 120°C for 72 hours, cool to room temperature, filter, wash with deionized water for 3 times, and dry the solid in a vacuum dryer at 60°C After 12 hours, it was calcined in a muffle furnace at 550° C. for 3 hours to obtain cobalt (II) ion-modified mesoporous silica microspheres.

[0023] 2) Mix 20 g of cobalt(II) ion-modified mesoporous silica microspheres with 0.001 g of ammonium molybdate, 1 g of phthalic anhydride, 1 g of ammonium chloride, and 3 g of urea, and place In a reaction kettle containing 70 mL of xylene, reflux reaction at 130°C for 2 hours under slow stirring conditions, after cooling to room temperature, suction fil...

Embodiment 3

[0025] 1) Dissolve 10 g of tetraethyl orthosilicate and 0.5 g of Tween-80 in 5 mL of ethanol to form a solution, and then slowly add it to 30 mL of detoxification solution containing 18 g of copper tetrasulfonate phthalocyanine and 1.0 g of Tween-80 Stir in deionized water for 2 hours at room temperature, then transfer the mixture to an autoclave, crystallize at 120°C for 72 hours, cool to room temperature, filter, wash with deionized water for 3 times, and dry the solid in a vacuum dryer at 60°C After 12 hours, it was calcined in a muffle furnace at 550° C. for 3 hours to obtain copper (II) ion-modified mesoporous silica microspheres.

[0026] 2) Mix 20 g copper(II) ion-modified mesoporous silica microspheres with 0.08 g ammonium molybdate, 1.5 g phthalic anhydride, 1.5 g ammonium chloride, and 5 g urea, and place In a reaction kettle filled with 70 mL of xylene, reflux at 130°C for 2 hours under slow stirring, cool to room temperature, filter with suction, wash with deionize...

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Abstract

The invention discloses a mesoporous silicon dioxide-loaded metal phthalocyanine catalyst and a preparation method thereof. The preparation method comprises the following steps of: in the preparation process, using a certain amount of tetra alkyl silicate and emulsifying agent to prepare an ethyl alcohol solution, gradually adding into a deionized water solution containing a certain amount of the template agent and the emulsifying agent, and stirring for 2h at room temperature; transferring into a reaction kettle, crystallizing for a period of time, cooling to room temperature, filtering and washing, drying, and calcining at high temperature, so as to obtain metal ion-modified mesoporous silicon dioxide microspheres; (2) mixing the mesoporous silicon dioxide microspheres, the catalyst, phthalic anhydride, ammonium chloride and urea according to a certain ratio, putting into a reaction kettle containing an organic solvent, heating to reach the reflux conditions, stirring and reacting for 2h, sucking and filtering, washing until the filtrate is in a neutral state, and drying, so as to obtain the mesoporous silicon dioxide-loaded metal phthalocyanine. The mesoporous silicon dioxide-loaded metal phthalocyanine catalyst is characterized in that the types of metal ions are rich, the content is high, the selectivity on catalyzing primer is high, the catalyzing speed is high, and the reaction condition is mild.

Description

technical field [0001] The invention relates to catalytic materials, in particular to a mesoporous silica-supported metal phthalocyanine catalyst and a preparation method thereof, belonging to the technical field of functional materials. Background technique [0002] Metal phthalocyanine has a good rigid conjugated plane, and the axial position of the central ion can coordinate with small molecular substances to carry out intermolecular electron transfer, causing changes in the structure of the coordination substance to act as a catalyst. It has the advantages of good stability, low toxicity and low cost, and is widely used in fields such as organic reactions, degradation of industrial wastewater, and simulated biological enzymes. Due to the disadvantages of easy formation of dimers that reduce the catalytic ability and secondary pollution caused by difficult recycling, many scholars have studied the loading of metal phthalocyanines. The loading carriers are generally tradit...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/72B01J23/745B01J23/75B01J31/22B01J35/10
CPCB01J23/72B01J23/745B01J23/75B01J31/183B01J2531/025B01J35/60
Inventor 李明田聂鑫附青山崔学军杨瑞嵩曾宪光金永中
Owner SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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