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A kind of highly dispersed and loaded noble metal catalytic material and its preparation method

A catalytic material and precious metal technology, applied in the field of highly dispersed supported precious metal catalytic materials and preparation, can solve the problems of reducing the size of active components, large size, particle agglomeration, etc., achieve good conversion rate and selectivity, and mild reaction process conditions , the effect of easy recycling

Active Publication Date: 2020-06-05
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the influence of solvation and cluster effects in the preparation of supported noble metal catalysts by the impregnation method, there is still the problem of particle agglomeration, and at the same time, a reducing agent needs to be added during the preparation process.
In the literature Qi Hetong, YuPing, Wang Yuexiang, Han Guangchao, Liu Huibiao, Yi Yuanping, Li Yuliang, MaoLanqun, JACS, 2015, 137, 5260, the graphyne oxide material is used as a carrier, and the carrier itself is used to directly reduce the noble metal active precursor to prepare The Pd / graphyne oxide catalyst was used, and the step of adding a reducing agent was omitted, but the catalyst active component Pd nanoparticles prepared by this method were relatively large in size, with an average particle diameter of 4.5nm, and further improvement of the test program was needed to reduce the active group. Dimensions

Method used

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  • A kind of highly dispersed and loaded noble metal catalytic material and its preparation method
  • A kind of highly dispersed and loaded noble metal catalytic material and its preparation method
  • A kind of highly dispersed and loaded noble metal catalytic material and its preparation method

Examples

Experimental program
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Effect test

Embodiment 1

[0042] A. FeSO 4 ·7H 2 O 1.3901g, Al 2 (SO 4 ) 3 18H 2 O 1.6650g was dissolved in 150mL deionized water to prepare mixed salt solution; NaOH 0.6400g and NaOH 2 CO 3 1. Dissolve 0600g in 150mL deionized water to make a mixed alkali solution. The two were dropped into the flask at a constant speed, the volume ratio of the two was controlled to be 10:13, the pH was adjusted to 8.5-9.5, and the flask was kept tightly closed, and the reaction was stirred at a constant temperature of 60°C for 4 hours. Naturally cool to room temperature, filter, wash the precipitate until neutral, and dry at 60°C for 8 hours to obtain the reduced hydrotalcite carrier FeAl-LDH.

[0043] B. Weigh 0.5000 g of FeAl-LDH powder in step A and disperse it in 100 mL of surfactant CTAC solution with a concentration of 6.25 mmol / L, and stir at room temperature for 10-20 min to form a uniformly dispersed suspension;

[0044] C. Stir the suspension obtained in step B at a constant temperature at 0°C, and...

Embodiment 2

[0046] A. Mn(NO 3 ) 2 4H 2 O 1.6065g, Al(NO 3 ) 3 9H 2 O 1.2006g was dissolved in 150mL deionized water to prepare salt solution; NaOH 0.6144g and NaOH 2 CO 3 Dissolve 0.6783g in 150mL deionized water to prepare a mixed alkali solution. Drop the two into the flask at the same time and at a constant speed by the double drop method, control the volume ratio of the two to 5:7, adjust the pH to 8-9, stir and react at a constant temperature of 80°C for 10 hours, cool to room temperature naturally, filter and wash the precipitate To neutrality, dry at 60°C for 8 hours to obtain the reducing hydrotalcite carrier MnAl-LDH.

[0047] B. Weigh 0.5000 g of the MnAl-LDH powder in step A and disperse it in 100 mL of surfactant CTAB solution with a concentration of 10.85 mmol / L, and stir at room temperature for 15 min to form a uniformly dispersed suspension;

[0048] C. Stir the suspension obtained in step B at a constant temperature at 25°C, and at the same time add 785 microliter...

Embodiment 3

[0050] A. will Co(NO 3 ) 2 ·6H 2 O 2.9105g, Al(NO 3 ) 3 9H 2 O 1.8757g was dissolved in 150mL deionized water to prepare mixed salt solution; NaOH 0.9600g and NaOH 2 CO 3 1. Dissolve 0600g in 150mL deionized water to make a mixed alkali solution. The two were dropped into the flask at the same time at a constant speed by the double drop method, the volume ratio of the two was controlled to be 1:1, and the reaction was stirred at a constant temperature of 90°C for 2h. Cool naturally to room temperature, filter and wash the precipitate to neutrality, and dry at 60°C for 10 h to obtain CoAl-LDH, a reduced hydrotalcite carrier.

[0051] B. Weigh 0.5000 g of CoAl-LDH powder in step A and disperse it in 100 mL of CTAC solution with a concentration of 6.25 mmol / L, and stir at room temperature for 15 min to obtain a uniformly dispersed suspension;

[0052] C. Stir the suspension obtained in step B at a constant temperature at a temperature of 50°C, and add 470 microliters of ...

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Abstract

The invention discloses a highly dispersed supported precious metal catalytic material and a preparation method. The preparation method adopted is to mix a reducing LDH carrier, a precious metal salt and a surfactant solution, and prepare a highly dispersed supported precious metal catalyst M / ZT in one step. -S. Since the variable valence metal is directly introduced into the LDHs layer during the preparation process of LDHs, a highly dispersed LDHs carrier with reducing sites is prepared; the highly dispersed reducing sites can spontaneously induce the reduction of oxidized precious metals and realize the active components of supported precious metal catalysts. The particles are highly dispersed and do not require reduction with reducing agents or high-temperature roasting. By changing the catalyst preparation temperature and surfactant addition conditions, the particle size, distribution and stable loading of the active components can be controlled. This highly dispersed supported catalyst shows good application effects in the selective oxidation reaction of benzyl alcohol and the hydrogenation reaction of anthraquinone.

Description

technical field [0001] The invention belongs to the field of catalyst preparation, and in particular relates to a highly dispersed and loaded noble metal catalytic material and a preparation method. Background technique [0002] Catalytic technology is a common key technology in petrochemical, fine chemical, coal chemical and environmental chemical industries, which has played a huge role in promoting economic development and social progress. Supported noble metal catalysts are a very important type of catalytic material in catalytic technology. It plays an important role in petrochemical, fine chemical, coal chemical and environmental chemical, especially in the fields of selective hydrogenation and selective oxidation. Supported noble metal catalysts rely on the activation of reactant molecules by single-state active noble metal nanoparticles on the surface of the carrier to play a catalytic role. However, the reserves of precious metals in our country are scarce and expe...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89B01J23/68C07C47/54C07C45/38C01B15/023
CPCB01J23/8906B01J23/688B01J23/8913C07C45/38C01B15/023B01J35/394C07C47/54
Inventor 李殿卿李海萍贺宇飞冯俊婷
Owner BEIJING UNIV OF CHEM TECH
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