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A kind of amine-functionalized mesoporous silica microsphere-supported heterogeneous catalyst and its preparation method and application

A heterogeneous catalyst, silica technology, applied in physical/chemical process catalysts, chemical instruments and methods, chemical/physical processes, etc., can solve the problems of uneven distribution, loose bonding, low loading, etc. To achieve the effect of simple and practical preparation method, enhanced dispersion, and reduced operating cost

Active Publication Date: 2017-03-01
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] The object of the invention is to provide a kind of catalyst for hydrogen peroxide (H 2 o 2 ) oxidation reaction supported catalyst and its preparation method, using this method to solve the existing problems of low loading of nanometer metal clusters on the mesoporous silica material, uneven distribution and loose combination of the two, the prepared catalyst The material has high oxidation reaction activity and stability, expanding the scope of application of the reaction

Method used

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  • A kind of amine-functionalized mesoporous silica microsphere-supported heterogeneous catalyst and its preparation method and application
  • A kind of amine-functionalized mesoporous silica microsphere-supported heterogeneous catalyst and its preparation method and application
  • A kind of amine-functionalized mesoporous silica microsphere-supported heterogeneous catalyst and its preparation method and application

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Mesoporous NH 2 -SiO 2 Preparation of nanospheres:

[0029] Dissolve 0.7042g sodium N-lauroyl sarcosinate (Sar-Na) completely in 80ml dilute HCl solution (the concentration of HCl is 0.1mol / L); Add the propyltriethoxysilane mixture to the above solution, pour it into the reaction kettle and let it stand in an oven at 60°C for 18h. The resulting product was centrifuged, washed with deionized water, and dried in vacuum to obtain white SiO 2nanospheres.

[0030] The surfactant in the pores is removed by ion exchange. The dried 1.0g SiO 2 Nanospheres were dispersed in 30mL ethanol solvent, heated to reflux overnight and then centrifuged. The solid was washed with deionized water three times and then dried in a vacuum oven to obtain amine-based mesoporous silica nanospheres, referred to as mesoporous NH 2 -SiO 2 nanospheres.

[0031] to mesoporous NH 2 -SiO 2 The specific surface area of ​​the nano-microsphere sample is analyzed, and the BET specific surface area i...

Embodiment 2

[0037] CuO / NH 2 -SiO 2 Preparation of Nanospheres

[0038] With the NH prepared in Example 1 2 -SiO 2 Mesoporous nanospheres are used as the carrier, 1.0g carrier is evenly dispersed in 100ml deionized water, 0.5663g copper nitrate trihydrate solid is added (the mass fraction of copper ions accounts for 15% of the carrier), transferred to the reaction kettle, and placed at a temperature of 50°C Let stand for 6h. After cooling, centrifuge, wash the solid with deionized water, and dry it in a vacuum oven to obtain a powdery solid sample CuO / NH 2 -SiO 2 Microspheres.

Embodiment 3

[0040] Fe 2-x Cu 1.5x o 3 / NH 2 -SiO 2 Preparation of nanospheres:

[0041] With the NH prepared in Example 1 2 -SiO 2 Mesoporous nano-microspheres are used as the carrier, 1.0g carrier is evenly dispersed in 100ml deionized water, 0.6886g ferric nitrate nonahydrate and 0.2059g copper nitrate trihydrate solid are added (the molar ratio of Fe to Cu is 2:1, the total metal ions The mass fraction accounts for 15% of the carrier), stirred for 2 hours, transferred to a 200ml reactor, and placed at a temperature of 50°C for 6 hours. After cooling, centrifuge, wash the solid with deionized water, and dry it in a vacuum oven to obtain a powdery solid sample Fe 2-x Cu 1.5x o 3 / NH 2 -SiO 2 Microspheres.

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Abstract

The invention discloses an amino functionalized mesoporous silica micro-sphere loaded type heterogeneous catalyst as well as a preparation method and application thereof. An amino mesoporous silica nano micro-sphere with a large specific surface area and good thermal stability is prepared by adopting a one-step method and is used as a carrier; then transition metal ions are connected onto a functional group of a pore channel through a coordinate bond effect; and finally, the metal ions adsorbed in the pore channel grow in situ under hydrothermal treatment to form a nano metal oxide cluster. The preparation method is simple, convenient and practical and does not cause secondary pollution to the environment. Compared with a traditional catalyst, the catalyst disclosed by the invention has good catalytic activity when hydrogen peroxide is used for reaction of oxidizing and degrading organic dyestuff; the use amount of the catalyst is less and reaction conditions are moderate; and the catalyst can be circularly used for a plurality of times and has a very good industrial application prospect.

Description

technical field [0001] The invention relates to an organic functionalized inorganic catalyst and its preparation method and application, in particular to an amine-based functionalized mesoporous silica microsphere-loaded nano metal cluster heterogeneous catalyst and its preparation method and application, belonging to inorganic metal The technical field of catalytic material preparation and catalytic application. Background technique [0002] At present, green catalytic oxidation technology has been widely used in petrochemical, pharmaceutical, environmental protection, agriculture and other fields. Among them, hydrogen peroxide (H 2 o 2 ) as a green oxidant is used in a variety of catalytic oxidation reactions, and its reaction products are non-toxic and harmless. Compared with oxygen, H 2 o 2 Oxidation activity is higher and easier to control. When hydrogen peroxide is used as an oxidant, a catalyst is generally required for catalytic oxidation. However, existing cata...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/24B01J35/08A62D3/38
Inventor 张国亮秦磊孟琴
Owner ZHEJIANG UNIV OF TECH