Carbon self-supported metal phosphide catalyst, and preparation method and application thereof

A metal phosphide and catalyst technology, applied in the direction of physical/chemical process catalysts, hydrocarbons, hydrocarbons, etc., can solve the problems of high cost, reduced metal bond strength, unfavorable large-scale production, etc., to prevent oxidation, strong Absorbing performance, effect of low reduction temperature

Active Publication Date: 2019-05-21
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The triangular prism structure is the smallest structural unit, P atoms intercalate with metal atoms, reducing the strength of metal bonds
The reduction of metal phosphate is a traditional method for preparing phosphides, but the process involves high temperature, high cost, and produces flammable and explosive phosphine gas, which is not conducive to large-scale industrial production. Improve the reduction process of phosphides and reduce energy consumption , has become a research hotspot

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] According to the stoichiometric ratio Ni:P=1:1 (molar ratio), weigh nickel nitrate hexahydrate Ni(NO 3 ) 2 ·6H 2 O 23.264g, add 50mL distilled water, stir 0.5h, fully dissolve, obtain nickel nitrate solution; Weigh phytic acid (C 6 h 18 o 24 P 6 , content 50wt%), 17.6g was added to the nickel nitrate solution, mixed and stirred for 2 hours, and the resulting mixed solution was placed in an oven at 120°C and baked until gelatinous, and then put in a microwave oven with high heat (power 1200W ) and calcined for 3 min to obtain a catalyst precursor.

[0025] The catalyst precursor obtained above was placed in a tube furnace, and the temperature was raised from room temperature to 650°C at a rate of 5°C / min in a hydrogen atmosphere for calcination and reduction, and the calcination and reduction was carried out at 650°C for 3 hours to obtain a metal nickel phosphide catalyst. In order to prevent the metal nickel phosphide from being oxidized, the catalyst needs to be ...

Embodiment 2

[0028] According to the stoichiometric ratio Ni:P=1:2 (molar ratio), weigh nickel nitrate hexahydrate Ni(NO 3 ) 2 ·6H 2 O 23.264g, add 50mL distilled water, stir 0.5h, fully dissolve, obtain nickel nitrate solution; Weigh phytic acid (C 6 h 18 o 24 P 6 , content 50wt%) 35.2g, added to the nickel nitrate solution, mixed and stirred for 2 hours, the formed mixed solution was placed in a 120°C oven and baked until gelatinous, and then put in a microwave oven with high heat (power 1200W ) was calcined for 3 minutes to obtain a catalyst precursor;

[0029] The catalyst precursor obtained above was placed in a tube furnace, and the temperature was raised from room temperature to 650°C at a rate of 5°C / min in a hydrogen atmosphere for calcination and reduction, and the calcination and reduction was carried out at 650°C for 3 hours to obtain a metal nickel phosphide catalyst. In order to prevent the metal nickel phosphide from being oxidized, the catalyst needs to be passivated....

Embodiment 3

[0032]According to the stoichiometric ratio Ni:P=1:3 (molar ratio), weigh nickel nitrate hexahydrate Ni(NO 3 ) 2 ·6H 2 O 14.535g, add 50mL distilled water, stir 0.5h, fully dissolve, obtain nickel nitrate solution; Weigh phytic acid (C 6 h 18 o 24 P 6 , content 50wt%) 33g, added to the nickel nitrate solution, mixed and stirred for 2 hours, put the formed mixed solution in an oven at 120°C and bake until gelatinous, and then put it in a microwave oven with high heat (power 1200W) Calcining for 3min to obtain a catalyst precursor;

[0033] The catalyst precursor obtained above was placed in a tube furnace, and the temperature was raised from room temperature to 650°C at a rate of 5°C / min in a hydrogen atmosphere for calcination and reduction, and the calcination and reduction was carried out at 650°C for 3 hours to obtain a metal nickel phosphide catalyst. In order to prevent the metal nickel phosphide from being oxidized, the catalyst needs to be passivated. At the passi...

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PUM

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Abstract

The invention discloses a preparation method of a carbon self-supported metal phosphide catalyst. The preparation method comprises the following steps: dispersing a transition metal element or a transition metal compound in distilled water to form a transition metal dispersion; uniformly mixing the transition metal dispersion with phytic acid, placing the obtained mixture in an oven, drying the mixture to form a colloidal material, and calcining the colloidal material in a microwave oven to obtain a catalyst precursor; and placing the catalyst precursor in a tubular furnace, carrying out calcining reduction in a H2 atmosphere, cooling the obtained material to a passivation temperature, introducing an inert gas containing low-concentration oxygen, and carrying out calcining passivation to obtain the carbon self-supported metal phosphide catalyst. In the present invention, the phytic acid can rapidly absorb microwaves, the transition metal phosphate precursor can be quickly obtained during microwave calcining, the phytic acid is carbonized when absorbing the microwaves and being rapidly heated in order to coat the transition metal phosphate precursor, and carbon wraps the carbon self-supported metal phosphide catalyst which is obtained by the reduction to form a slight carbon film in order to prevent the catalyst from being oxidized.

Description

technical field [0001] The invention relates to a carbon self-supporting metal phosphide catalyst, a preparation method and application thereof. Background technique [0002] The hydrogenation process usually uses platinum, palladium, ruthenium and other noble metals as catalysts, which have high catalytic activity. However, due to the scarcity and high cost of noble metal resources, it is necessary to find suitable catalysts to replace noble metal catalysts in order to reduce costs. In recent years, transition metal phosphides have become a research hotspot in the field of hydrogenation due to their excellent hydrodesulfurization and hydrodenitrogenation activities and stability, and may partially replace noble metals as a new generation of hydroprocessing catalysts. The reduction of metal phosphate is a traditional method for preparing phosphides, but the process involves high temperature and high cost, which is not conducive to large-scale industrial production. Improvi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/185B01J27/19C07C17/23C07C19/08C07C5/09C07C11/04C07C1/20C07C1/32C07C9/10C07C13/567
CPCY02P20/52Y02P30/20Y02P30/40
Inventor 韩文锋李西良刘兵唐浩东李瑛刘化章
Owner ZHEJIANG UNIV OF TECH
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