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Sulfonic functionalized mesoporous silicon dioxide microsphere loaded metal oxide catalyst and preparation method and application of catalyst

A technology of mesoporous silica and silica, which can be used in physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., and can solve the problems of loose bonding, uneven distribution, and low loading. , to achieve the effect of improving the degree of binding, the preparation method is simple and practical, and reducing the operating cost

Active Publication Date: 2015-05-27
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The object of the invention is to provide a kind of catalyst for hydrogen peroxide (H 2 o 2 ) oxidation reaction of sulfonic acid functionalized mesoporous silica microsphere-supported catalyst and its preparation method, using this method to solve the problems of low loading, uneven distribution and two The prepared catalytic material has high oxidation reaction activity and stability, and expands the scope of application of the reaction.

Method used

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  • Sulfonic functionalized mesoporous silicon dioxide microsphere loaded metal oxide catalyst and preparation method and application of catalyst
  • Sulfonic functionalized mesoporous silicon dioxide microsphere loaded metal oxide catalyst and preparation method and application of catalyst
  • Sulfonic functionalized mesoporous silicon dioxide microsphere loaded metal oxide catalyst and preparation method and application of catalyst

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Experimental program
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Effect test

Embodiment 1

[0031] Mesoporous SiO 2 Sulfonic acid functionalization preparation of nanospheres:

[0032] Dissolve 0.7042g sodium N-lauroyl sarcosinate (Sar-Na) completely in 80ml dilute HCl solution (the concentration of HCl is 0.1mol / L); Propyltriethoxysilane mixture was added to the above solution, and then poured into the reaction kettle and left in an oven at 60°C for 15 hours. The obtained product was centrifuged, washed with deionized water and dried in vacuum to obtain white SiO 2 nanospheres.

[0033] A high-temperature calcination method is used to remove the surfactant in the pores. The dried 1.0g SiO2 The nano-microspheres were slightly ground, placed in a muffle furnace, and the temperature was programmed to rise to 600 ° C for 6 hours to obtain mesoporous SiO 2 nanospheres.

[0034] The prepared mesoporous SiO 2 Nanospheres (1.0g) were completely submerged in 15ml CH 2 Cl 2 solution, after ultrasonic dispersion, add 4ml of chlorosulfonic acid to the above mixture, ult...

Embodiment 2

[0040] MnO 2 / mesoporous SO 3 H-SiO 2 Preparation of microspheres:

[0041] 1.0 g of mesoporous SO prepared in Example 1 3 H-SiO 2 Microsphere samples were dispersed in 100 mL of deionized water, 0.629 g of anhydrous manganese acetate solid (mass fraction of manganese ions accounted for 20% of the carrier) was added, stirred, transferred to a reaction kettle, and placed at 60°C for 8 hours. After cooling, centrifuge, wash the solid with deionized water, and dry it in a vacuum oven; take it out, grind it with a mortar, put it in a muffle furnace, and heat it up to 180 ° C for 6 hours to obtain a solid sample MnO 2 / mesoporous SO 3 H-SiO 2 Microspheres.

Embodiment 3

[0043] Cu 2-x mn x o 3 Loaded mesoporous SO 3 H-SiO 2 Preparation of nanospheres:

[0044] With SO prepared in embodiment 1 3 H-SiO 2 Mesoporous nanospheres were used as the carrier, and 1.0 g of the carrier was uniformly dispersed in 100 mL of deionized water, and 0.528 g of copper nitrate trihydrate and 0.189 g of anhydrous manganese acetate solid were added (the molar ratio of Cu to Mn was 2:1, and the total metal ions The mass fraction accounts for 20% of the carrier), and after stirring, it is transferred to a reaction kettle, and placed at a temperature of 60° C. for 8 hours. After cooling, centrifuge, wash the solid with deionized water, and dry it in a vacuum oven; take it out, grind it with a mortar, put it in a muffle furnace, and heat it up to 180°C for 6 hours to obtain a powdery solid sample Cu 2-x mn 0.5x o 2 / SO 3 H-SiO 2 Microspheres.

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Abstract

The invention discloses a sulfonic functionalized mesoporous silicon dioxide microsphere loaded metal oxide catalyst and a preparation method and application of the catalyst. According to the invention, sulfonic mesoporous silicon dioxide nano-microspheres are prepared by using a sulfonic grafting method; then, by taking sulfonic acid functionalized mesoporous silicon dioxide microspheres which are provided with uniform channels, and are large in specific surface area and good in thermal stability as carriers, transition metal ions are connected to functional groups of the channels under the action of covalent bonds; and under the hydrothermal-roasting condition, the transition metal ions adsorbed in the channels grow into nano metal oxides through in-situ growth. The preparation method disclosed by the invention is simple and practical; the prepared catalyst has a good catalytic activity in the catalytic activation of a hydrogen peroxide oxidation reaction, and the consumption of the catalyst is low, the reaction conditions are mild, and the catalyst can be repeatedly used for multiple times, and therefore, the catalyst has good industrial application potential.

Description

technical field [0001] The invention relates to a functionalized supported catalytic material and its preparation method and application, in particular to a sulfonic acid functionalized mesoporous silica microsphere supported metal oxide heterogeneous catalyst and its preparation method and application, belonging to inorganic The technical field of metal catalytic material preparation and catalytic application. Background technique [0002] At present, hydrogen peroxide catalytic oxidation technology has been widely used in petrochemical, pharmaceutical, environmental protection, agriculture and other fields. However, the development of high-performance supported catalysts has become the key to accelerate the catalytic oxidation of hydrogen peroxide. In recent years, silica series porous materials as catalyst supports have the advantages of large specific surface area, good thermal and chemical stability, three-dimensional ordered pore structure, non-toxicity and high biocom...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/043B01J35/10C02F1/72C02F101/30
Inventor 张国亮秦磊吴玉娇
Owner ZHEJIANG UNIV OF TECH
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