Preparation method of siliceous mesocellular foams (MCFs) loaded nano Ni2P hydrogenation catalyst

A technology of mesoporous silica and hydrogenation catalyst, which is applied in the direction of physical/chemical process catalysts, catalyst carriers, chemical instruments and methods, etc. It can solve the problems of complex preparation methods, easy particle agglomeration, and blocked pores, and achieve simple preparation process , Accelerate the diffusion and avoid the effect of clogging

Inactive Publication Date: 2015-03-04
CHANGZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The technical problem to be solved in the present invention is aimed at current Ni 2 P particles are easy to agglomerate, the traditional preparation method is complicated, the conditions are harsh, and the cost is high. Loaded Ni 2 P blocking the pores and other problems, providing a simple method and mild conditions for the preparation of loaded high-dispersion Ni 2 P hydrogenation catalyst method

Method used

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  • Preparation method of siliceous mesocellular foams (MCFs) loaded nano Ni2P hydrogenation catalyst

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] Weigh 3mmol of nickel chloride and add it to 10mL of deionized water. After the nickel chloride is dissolved, add 3mmol of succinic acid and stir for 0.5h to obtain a stable and dispersed aqueous solution of complexed nickel ions; add 0.5g of MCFs to the above solution and stir at room temperature 1h, then heated to 70°C, evaporated to dryness, baked in an oven at 100°C overnight, then roasted in a muffle furnace at 500°C for 3h to obtain supported nickel oxide powder; then added 4.5mmol of dihydrogen hypophosphite to the powder Sodium, mixed mechanically and placed in a tube furnace, in N 2 300°C for 3 hours, then fully washed with deionized water, and dried at 100°C to obtain the catalyst A.

Embodiment 2

[0026] Weigh 3mmol nickel chloride and add it to 10mL deionized water, add 3mmol EDTA after the nickel chloride dissolves, stir for 0.5h to obtain a stable and dispersed complex nickel ion aqueous solution; add 0.5g MCFs to the above solution, stir at room temperature for 1h, Then heated to 70°C, evaporated to dryness, baked in an oven at 100°C overnight, and then roasted in a muffle furnace at 500°C for 3h to obtain supported nickel oxide powder; then added 4.5mmol sodium dihydrogen hypophosphite to the powder, Mixed mechanically and placed in a tube furnace under N 2 300°C for 3 hours, then fully washed with deionized water, and dried at 100°C to obtain the catalyst B.

Embodiment 3

[0028] Weigh 3mmol of nickel chloride and add it to 10mL of deionized water. After the nickel chloride is dissolved, add 3mmol of citric acid and stir for 0.5h to obtain a stable and dispersed aqueous solution of complexed nickel ions; add 0.5g of MCFs to the above solution and stir for 1h at room temperature , then heated to 70°C, evaporated to dryness, and then baked in an oven at 100°C overnight, and then roasted in a muffle furnace at 500°C for 3 hours to obtain a supported nickel oxide powder; then add 4.5mmol sodium dihydrogen hypophosphite to the powder , mixed mechanically and placed in a tube furnace, under N 2 at 300°C for 3 hours, then fully washed with deionized water, and dried at 100°C to obtain the catalyst C.

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Abstract

The invention relates to a preparation method of a siliceous mesocellular foams (MCFs) loaded nano Ni2P hydrogenation catalyst. The catalyst is prepared by a complexation dipping mode and a hypophosphite low-temperature thermal decomposition method by selecting siliceous mesocellular foams with a three-dimensional oversized mesocellular structure and relatively high thermal stability as carriers. According to the preparation method, a complexing agent is introduced for highly dispersing nickel ions, and the complexed nickel ions can enter relatively large ducts of the MCFs, thereby preparing Ni2P nano particles with high dispersity. The catalyst is used for hydrogenation reaction of nitrobenzene, and shows very high catalytic activity and favorable reusability; the catalyst adopts a simple preparation process and mild conditions, and can achieve industrial production easily.

Description

technical field [0001] The invention relates to the technical field of non-noble metal hydrogenation catalysts and their preparation, in particular to a mesoporous silica foam material loaded with nano-Ni 2 Preparation method of P hydrogenation catalyst. Background technique [0002] Transition metal phosphides are another new type of catalytic material after nitrides and carbides. Their approximate spherical structure exposes more coordination unsaturated surface atoms than layered sulfides, thus showing higher Surface active site density. Studies have found that transition metal phosphides have excellent hydrotreating activity, hydrodesulfurization, denitrification selectivity, and low hydrogen consumption, which has attracted great attention. In the currently studied transition metal phosphides (MoP, WP, Ni 2 P. Co. 2 P, FeP, etc.), Ni 2 P shows superior hydrogenation activity, even higher than that of bimetallic nitrides and carbides, and is expected to replace the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185B01J32/00B01J35/10
Inventor 刘平常婉亭李永昕薛冰
Owner CHANGZHOU UNIV
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