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Hollow metallic ball with mesopore structure and preparation method and application thereof

A mesoporous structure and metal sphere technology, applied in the field of metal catalysts, can solve problems such as hollow structure damage, and achieve the effects of low cost, simple preparation process, and easy control of conditions

Inactive Publication Date: 2008-10-08
SHANGHAI NORMAL UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although there are reports of hollow metal preparation methods in the existing literature, the method is to deposit metal atoms on silicon spheres or metals, and then remove the template by etching or replacement reaction. The defects of this method are: in the process of removing the template In the middle, due to the violent reaction, the hollow structure will be destroyed

Method used

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  • Hollow metallic ball with mesopore structure and preparation method and application thereof
  • Hollow metallic ball with mesopore structure and preparation method and application thereof
  • Hollow metallic ball with mesopore structure and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0025] 1) At 15 ~ 30 ℃, to Bu t PdCl was added dropwise to PBr surfactant aqueous solution 2 Aqueous solution, after dropping, continue stirring for 5-15 minutes to obtain a turbid solution, wherein: the molar ratio of surfactant to metal salt is 20:1, and the molar ratio of metal salt to rare earth metal salt is 9:0;

[0026] 2) At 25°C, quickly add KBH to the above mixed solution 4 Aqueous solution, stirred vigorously for 10 minutes, black particles are gradually formed in the solution, and gas emerges, wherein: the molar ratio of metal borohydride compound to metal salt in the water phase is 4:1;

[0027] 3) Filter the black particles generated in step 2), and then wash with deionized water and absolute ethanol for 3 to 5 times respectively to obtain the target object-hollow Pd spheres with a mesoporous structure, represented by Pd (hollow).

[0028] figure 1 For the N of the sample prepared in this embodiment 2 Adsorption-desorption isotherm, from the shape of the isot...

Embodiment 2

[0031] 1) At 15 ~ 30 ℃, to Bu t PdCl was added dropwise to PBr surfactant aqueous solution 2 Aqueous solution and Ce(NO 3 ) 3 The mixed solution of the aqueous solution, after dropping, was continued to stir for 5 to 15 minutes to obtain a turbid solution, wherein: the molar ratio of the surfactant to the metal salt was 20:1, and the molar ratio of the metal salt to the rare earth metal salt was 9:1;

[0032] 2) At 25°C, quickly add KBH to the above mixed solution 4 Aqueous solution, stirred vigorously for 20 minutes, black particles are gradually formed in the solution, and gas emerges, wherein: the molar ratio of metal borohydride compound to metal salt in the water phase is 4:1;

[0033] 3) filter the black particles generated in step 2), then wash with deionized water and absolute ethanol for 3 to 5 times respectively to obtain the target object-hollow Pd-Ce spheres with mesoporous structure, use Pd-Ce (hollow )express.

[0034] image 3 For the N of the sample prepa...

Embodiment 3

[0037] The difference between this example and Example 2 is that the molar ratio of the surfactant to the metal salt used is 2:1, and the rest of the content is the same as that described in Example 2.

[0038] The N of the sample prepared by this embodiment 2The adsorption-desorption isotherm can be determined to be that the obtained sample has a mesoporous structure; it can be seen from the TEM photo of the sample prepared in this embodiment that the obtained sample is a hollow sphere, the outer diameter of the spherical shell is 10nm, and the wall thickness of the spherical shell is 2nm; using QuantaChrome The Nova 4000e automatic physical adsorption instrument measures the specific surface area and pore structure of the metal catalyst. It can be known that the active specific surface area of ​​the metal nanoparticles with mesoporous structure is 50m 2 / g, the pore diameter is 2nm, and the pore volume is 0.8cm 3 / g.

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Abstract

The invention discloses a hollow metal ball with a meso-pore structure and a preparation method and an application thereof. A ball shell of the hollow metal ball is composed of metal nanoparticles with 2-5nm particle diameter and the meso-pore structure, the outside diameter of the ball shell is 10-500nm and the wall thickness is 2-5nm. The hollow metal ball with the meso-pore structure can be used as a hydrogenation catalyst for alkene, acetylene hydrocarbon, aromatic hydrocarbon, phenols, nitriles, and compounds containing unsaturated groups such as nitro compounds or carbonyl compounds, etc., which particularly has catalytic effect on hydrogenation reactions such as preparing cyclohexanone with liquid phenol, preparing maltitol with liquid maltose and preparing cinnamyl alcohol with liquid cinnamic aldehyde. The hollow metal ball with the meso-pore structure prepared by the invention has better catalytic performance than common solid nano-particles and long service life, which can be repeatedly used and still keep hardly changed catalytic efficiency; in addition, the method of the invention has simple preparation process, easily controlling conditions and low cost.

Description

technical field [0001] The invention relates to a hollow metal sphere with a mesoporous structure, a preparation method and application thereof, and belongs to the technical field of metal catalysts. Background technique [0002] In recent years, studies have found that nanomaterials with hollow structures have a variety of different applications due to their low density, easy recycling, cost savings and excellent surface permeability, such as optical crystallization, drug delivery, filling and catalysts, especially in catalytic On the one hand, nanomaterials with hollow structures exhibit better catalytic performance than those with ordinary solid structures. In addition, metal materials with mesoporous structures also have excellent physical and chemical properties due to the combination of one-dimensional nanomaterials and the characteristics of metals themselves, especially mesoporous metals due to their special pore structure, quantum effects and interface coupling effe...

Claims

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Application Information

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IPC IPC(8): B01J23/44B01J23/63B01J23/755B01J23/75B01J23/52B01J23/46B01J23/50B01J35/10C07B35/02C07C45/00C07C49/403C07D309/40C07C29/141C07C33/32
Inventor 李辉刘俊李和兴
Owner SHANGHAI NORMAL UNIVERSITY
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