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Magnetically-separable mesoporous nano catalyst with core-shell structure and preparation method of magnetically-separable mesoporous nano catalyst

A nano-catalyst, core-shell structure technology, applied in chemical instruments and methods, preparation of hydroxyl compounds, preparation of carboxylic acids by ozone oxidation, etc., to solve the effects of poor stability, improve activity, and increase contact area

Inactive Publication Date: 2014-07-23
HEBEI UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, it has an important problem, it is difficult to separate from the reaction solution, and its reusability is poor, which increases the cost to a certain extent, pollutes the environment, and affects its wide application in industry.

Method used

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  • Magnetically-separable mesoporous nano catalyst with core-shell structure and preparation method of magnetically-separable mesoporous nano catalyst
  • Magnetically-separable mesoporous nano catalyst with core-shell structure and preparation method of magnetically-separable mesoporous nano catalyst
  • Magnetically-separable mesoporous nano catalyst with core-shell structure and preparation method of magnetically-separable mesoporous nano catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Example 1 : Fe 3 o 4 nSiO 2 mSiO 2 Preparation and Application of Ni-Co-B Catalyst

[0029] a. 0.7 g of 20 nm Fe 3 o 4 After the microspheres were ultrasonically treated with dilute hydrochloric acid and washed, a mixture containing 2.5 ml of ammonia water, 140 ml of ethanol, and 35 ml of water was added, placed in an ultrasonic processor and mixed evenly, and finally 1 ml of ethyl orthosilicate was added dropwise, and mechanically stirred 5 h, magnetic separation;

[0030] b, to the Fe prepared above 3 o 4 nSiO 2 Add a mixture containing 0.75 g cetyltrimethylammonium bromide, 2.5 ml ammonia water, 150 ml ethanol, and 200 ml water to the nanoparticles, mix them in an ultrasonic processor, and finally add 1 ml orthosilicone dropwise. Acetate ethyl ester, continue to stir for 5 h, magnetically separate, and wash with ethanol 3-6 times;

[0031] The obtained nanoparticles were mixed with 200 ml ethanol solution of ammonium nitrate with a concentration of 6 g / ml...

Embodiment 2

[0045] Example 2 : Fe 3 o 4 nSiO 2 mZrO 2 Preparation and Application of Ni-Cr-B Catalyst

[0046] a. 0.7 g of 20 nm Fe 3 o 4 After the microspheres were ultrasonically treated with dilute hydrochloric acid and washed, a mixture containing 2.5 ml of ammonia water, 140 ml of ethanol, and 35 ml of water was added, placed in an ultrasonic processor and mixed evenly, and finally 1 ml of ethyl orthosilicate was added dropwise, and the stirring was continued. 5 h, magnetic separation;

[0047] b, to the Fe prepared above 3 o 4 nSiO 2 Add a mixed solution containing 0.45 g cetyltrimethylammonium bromide, 2.3 ml ammonia water, 90 ml ethanol, and 120 ml water to the nanoparticles, mix them in an ultrasonic processor, and finally add 1 ml dropwise at a concentration of 0.92 g / ml zirconium oxychloride aqueous solution, mechanically stirred for 10 h, magnetically separated, washed with ethanol for 3-6 times;

[0048] The obtained nanoparticles were mechanically stirred with 20...

Embodiment 3

[0057] Example 3 : Fe 3 o 4 nSiO 2 mSiO 2 Preparation and Application of Ni-La-B Catalyst

[0058] In this embodiment, steps a and b are the same as those in Embodiment 1.

[0059] c. Add 0.506 g NiCl 2 ·6H 2 O, 0.051 g La(NO 3 ) 3 ·6H 2 O was prepared into a homogeneous solution, and the above-prepared 0.5 g Fe 3 o 4 nSiO 2 mSiO 2 Fully soak in the solution and dry at low temperature;

[0060] d. Add 0.07 g NaOH, 0.46 g KBH 4 Add it to 8.6 ml of water to dissolve and configure it as a reducing agent;

[0061] e. Add c to 4.0 mL water to make a suspension;

[0062] f. Add the solution in d dropwise to e at a speed of 0.7 ml / min through a convection pump. At this time, a black reduced Ni species appears in e. After the dropwise addition of the liquid in d is completed, add the catalyst and The mother liquor was magnetically separated and stored in absolute ethanol for future use.

[0063] application:

[0064] Add 6 g of benzophenone, 0.8 g of catalyst, and ...

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Abstract

The invention discloses a magnetically-separable mesoporous nano catalyst with a core-shell structure and a preparation method of the magnetically-separable mesoporous nano catalyst. The core-shell structure is Fe3O4@nSiO2@mSiO2(or mZrO2)@Ni-X-B, wherein X is doped metal. The method comprises the following steps: micro-balling Fe3O4, adding diluted hydrochloric acid, and performing ultrasonic oscillation treatment for 5-15min; washing by using ethyl alcohol, and adding ammonium hydroxide mixed liquor and tetraethyl orthosilicate for stirring and magnetic separation; adding mixed liquor formed by cetyl trimethyl ammonium bromide and the like into Fe3O4@nSiO2 particles, and uniformly mixing to remove the cetyl trimethyl ammonium bromide; putting Fe3O4@nSiO2@mSiO2(or mZrO2) in a metal salt solution, soaking and drying; reducing by using an alkaline solution of hydroboron. The prepared catalyst is high in activity, high in selectivity, high in stability, low in preparation cost, and environmentally friendly.

Description

technical field [0001] The invention relates to a magnetic mesoporous nanometer material and a preparation method thereof, in particular to a magnetically separable core-shell structure mesoporous nanometer catalyst and a preparation method thereof. current technology [0002] Ordered mesoporous materials have two-dimensional or three-dimensional ordered pores, and the pore diameter is between 2-50nm. It has unique properties, such as adjustable pore size, large specific surface area and pore volume, and controllable composition, etc., which make it have great potential in the fields of catalysis, adsorption, separation, dye cells, sensors, and enzyme immobilization. application prospects. Core-shell materials first appeared in the 1990s. Later, in order to meet the needs of human beings for material functions, more and more people began to pay attention to the preparation of materials, and core-shell materials developed rapidly. Among them, magnetic core-shell materials a...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J23/86B01J23/83B01J23/78B01J35/10C07C57/30C07C51/36C07C33/24C07C29/145C07C61/08
Inventor 白国义刘晓芳
Owner HEBEI UNIVERSITY