Preparation method and application of palladium(Pd) catalyst loaded in hollow mesoporous silicon nanocapsules

A technology of nanocapsules and palladium catalysts, which is applied in the field of catalyst preparation of precious metal palladium, can solve the problems of time-consuming and costly organic amine molecules, and achieve the effects of preventing loss and high catalytic activity

Active Publication Date: 2018-03-09
LANZHOU UNIVERSITY
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, covalent modification of organic amine molecule

Method used

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  • Preparation method and application of palladium(Pd) catalyst loaded in hollow mesoporous silicon nanocapsules
  • Preparation method and application of palladium(Pd) catalyst loaded in hollow mesoporous silicon nanocapsules
  • Preparation method and application of palladium(Pd) catalyst loaded in hollow mesoporous silicon nanocapsules

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Embodiment 1

[0026] A method for preparing a palladium catalyst supported in the core of a hollow mesoporous silicon nanocapsule, the specific method is as follows: add palladium acetate, water, carbon nanotubes, and aqueous formaldehyde solution (mass fraction 28wt%) at a mass ratio of 1:500:2:50 In the reactor, stir evenly and react at 40°C for 5 h, filter with suction, and dry at 80°C for 6 h to obtain the Pd / CNTs material.

[0027] The above Pd / CNTs, triethanolamine, distilled water, and cetyltrimethylammonium chloride were added into the reactor at a mass ratio of 1:0.1:200:30, and mechanically stirred at 60°C for 1 h. Then, the ethyl orthosilicate / cyclohexane mixed solution that is 300 times the mass ratio of Pd / CNTs is added to the above-mentioned dispersion system, wherein the ethyl orthosilicate / cyclohexane mixed solution is composed of ethyl orthosilicate and cyclohexane Alkanes are mixed according to the volume ratio of 1:10. then 80 o C under reflux stirring reaction 20h, whe...

Embodiment 2

[0029] A method for preparing a palladium catalyst supported in a hollow mesoporous silicon nanocapsule core, the specific method is as follows: add palladium acetate, water, carbon nanotubes, and aqueous formaldehyde solution (mass fraction 28wt%) at a mass ratio of 1:700:3:80 In the reactor, stir evenly and react at 60°C for 8 h, filter with suction, and dry at 80°C for 8 h to obtain the Pd / CNTs material.

[0030] The above Pd / CNTs, triethanolamine, distilled water, and cetyltrimethylammonium chloride were added into the reactor at a mass ratio of 1:0.2:260:45, and mechanically stirred at 80°C for 3 h. Then, the tetraethyl orthosilicate / cyclohexane mixed solution that is 400 times the mass ratio of Pd / CNTs is added to the above-mentioned dispersion system, wherein the tetraethyl orthosilicate / cyclohexane mixed solution is made of tetraethyl orthosilicate and cyclohexane Alkanes are mixed according to the volume ratio of 1:10. then 60 o C under reflux and slowly stirred for...

Embodiment 3

[0032] A method for preparing a palladium catalyst supported in a hollow mesoporous silicon nanocapsule core, the specific method is as follows: add palladium acetate, water, carbon nanotubes, and aqueous formaldehyde solution (mass fraction 28wt%) at a mass ratio of 1: 1000: 4: 100 In the reactor, stir evenly and react at 70°C for 10 h, filter with suction, and dry at 80°C for 7 h to obtain the Pd / CNTs material.

[0033] Pd / CNTs, triethanolamine, distilled water, and cetyltrimethylammonium chloride were added into the reactor at a mass ratio of 1:0.3:300:50, and mechanically stirred at 60°C for 1 h. Then, the tetraethyl orthosilicate / cyclohexane mixed solution that is 500 times the mass ratio of Pd / CNTs is added to the above-mentioned dispersion system, wherein the tetraethyl orthosilicate / cyclohexane mixed solution is composed of tetraethyl orthosilicate and cyclohexane Alkanes are mixed according to the volume ratio of 1:10. Then slowly stir at 60°C under reflux for 40 h, ...

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Abstract

The invention relates to a preparation method of a palladium(Pd) catalyst loaded in hollow mesoporous silicon nanocapsules, which is a method for loading Pd catalyst active components to the inside ofa hollow mesoporous carrier in a dispersing way to overcome defects of the Pd catalysts of the prior art. According to the method, Pd nano-particle loaded carbon nano tubes (Pd/CNTs) are taken as templates, the surfaces of the Pd/CNTs are coated with mesoporous silicon, the CNTs are removed by means of roasting, and thus the Pd catalyst loaded in hollow mesoporous silicon nanocapsules is obtained. Through the hollow mesoporous structure, gas-phase and liquid-phase reactant molecules enter or exit the shell effectively to contact the Pd active components; thus, correlated chemical reactions, such as hydrodechlorination of chlorinated phenol, hydrogenation reaction of aldehydes, hydrogenation reaction of nitro-compound, Suzuki coupling reaction, hydrogen production by catalyzing formic acidor ammonia borane, are catalyzed under high activity of Pd. But above all, the Pd catalyst loaded in hollow mesoporous silicon nanocapsules is capable of preventing loss of the nano particles of Pd active components effectively.

Description

technical field [0001] The invention belongs to the technical field of catalyst preparation methods for noble metal palladium, and in particular relates to a preparation method for palladium catalysts loaded in hollow mesoporous silicon nanocapsule cores. Background technique [0002] Catalysts based on noble metal palladium are very common in catalytic reactions, including homogeneous palladium catalysts, such as palladium acetate, palladium chloride, palladium organic complexes, etc. These homogeneous catalysts are in a single-atom catalytic state in catalytic reactions, and their catalytic activity However, it is difficult to separate from the reaction system, so the large-scale industrial application of homogeneous palladium catalyst is difficult to realize. The supported palladium catalyst can be widely used in industrial catalysis because it is easier to separate from the reaction system by centrifugation or filtration and further reuse. [0003] At present, supported...

Claims

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Application Information

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IPC IPC(8): B01J23/44C07C209/36C07C211/46
CPCB01J23/44B01J35/006B01J35/0073B01J37/0018C07C209/36C07C211/46
Inventor 董正平田蒙
Owner LANZHOU UNIVERSITY
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