Preparation method of core-shell structured Pd-Co/CN@SiO2 nano-catalyst

A nano-catalyst, core-shell structure technology, applied in the preparation of organic compounds, catalysts for physical/chemical processes, preparation of amino compounds, etc., can solve the problems of easy sintering of metal nanometers, high equipment requirements, and unfavorable industrial production. The effect of improving catalytic activity, easy operation and strong practicability

Inactive Publication Date: 2018-12-18
NANJING UNIV OF SCI & TECH +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

X. Sun et al. (Journal of Catalysis 357 (2018) 20–28) reported a cobalt nano-dispersed material on porous nitrogen-doped graphite, Co@mesoNC, which has good catalytic system for various nitro-containing compounds. Catalytic activity, but it needs to be transformed at 383K, 3MPa
Eckardt M et al. (Scientific Reports, 2018, 8(1)) prepared a nitrogen-doped graphite

Method used

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  • Preparation method of core-shell structured Pd-Co/CN@SiO2 nano-catalyst
  • Preparation method of core-shell structured Pd-Co/CN@SiO2 nano-catalyst
  • Preparation method of core-shell structured Pd-Co/CN@SiO2 nano-catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] 0.45g Co(NO 3 ) 2 ·6H 2 O, 0.05g K 2 PdCl 4 Dissolve in 3ml deionized water, 5.5g 2-MeIM dissolved in 20ml deionized water, mix the two solutions and stir for 24h, filter and dry to obtain palladium-loaded cobalt-based metal organic framework Pd 2+ / ZIF-67. Take 30 mg palladium-loaded cobalt-based metal-organic framework Pd 2+ / ZIF-67 was dispersed in a mixture of 33ml deionized water and 20ml absolute ethanol, 250mg 2-methylimidazole was added, 0.55ml 25% CTAC aqueous solution was added after ultrasonication for 10min, and 0.4ml tetraethyl silicate was added after stirring for 20min. After 2h, filter and dry. The resulting mass was placed in a tube furnace, N 2 Calcined slowly at 800°C for 4 hours under atmosphere to obtain core-shell structure Pd-Co / CN@SiO 2 nanocatalyst.

[0023] figure 1 It is the X-ray photoelectron energy spectrum of the catalyst. Figure b is the 3d spectrum of Pd. It can be seen from the figure that the binding energies of the two main...

Embodiment 2

[0027] It is basically the same as Example 1, except that the calcination temperature is changed to 750°C.

Embodiment 3

[0029] It is basically the same as Example 1, except that the calcination temperature is changed to 850°C.

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Abstract

The invention discloses a preparation method of a core-shell structured Pd-Co/CN@SiO2 nano-catalyst. The method comprises the following steps: mixing and reacting cobalt nitrate hexahydrate, potassiumchloropalladate and 2-methylimidazole to prepare a palladium-supported cobalt-based metal organic framework Pd<2+>/ZIF-67, then reacting the Pd<2+>/ZIF-67 with 2-methylimidazole, cetyltrimethylammonium chloride and tetraethyl orthosilicate to make the surface of the Pd<2+>/ZIF-67 wrapped with silica, and performing calcination to obtain the Pd-Co/CN@SiO2 catalyst. SiO2 shell coating can effectively prevent the agglomeration of Pd-Co nanoparticles and prevent the loss of metal particles in a catalytic reaction, so the catalytic activity is improved, and the hydrogenation reduction of nitro compounds under normal temperature and normal pressure conditions is realized; the method has the advantages of mild conditions, strong practicability, and easiness in operation; and the catalyst has theadvantage of magnetism, easiness in recovery, and realization of cycle use.

Description

technical field [0001] The invention belongs to the technical field of nanometer metal catalysts, and relates to a core-shell structure Pd-Co / CN@SiO 2 Preparation methods of nanocatalysts. Background technique [0002] As important chemical intermediates, substituted amino compounds are widely used in the synthesis of drugs, pesticides, organic pigments, coatings, polymers, etc. They are generally prepared by reducing the corresponding nitro compounds. Currently commonly used reduction methods are: iron powder or alkali sulfide reduction method, sodium borohydride, hydrazine hydrate, formic acid, hydrogenation reduction method, etc. A large amount of three wastes will be produced in the reduction process of iron powder or alkali sulfide, causing serious environmental pollution and serious corrosion to equipment. When sodium borohydride, hydrazine hydrate, and formic acid are used as reducing agents, although these reducing agents have good selectivity, they often have the...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J35/00C07C209/36C07C211/46C07C211/52C07C213/02C07C217/84C07D215/40
CPCB01J27/24B01J35/0033B01J35/0086C07C209/36C07C213/02C07D215/40C07C211/46C07C211/52C07C217/84
Inventor 陆明许登祝洁王鹏程林秋汉
Owner NANJING UNIV OF SCI & TECH
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