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High-dispersion loaded noble metal catalytic material and preparation method thereof

A technology of catalytic materials and precious metals, which is applied in the field of highly dispersed and loaded noble metal catalytic materials and its preparation, can solve the problems of particle agglomeration, reduction of active component size, large size, etc., and achieve mild reaction process conditions, good conversion rate and selectivity , Ease of recycling

Active Publication Date: 2019-08-27
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, LiuH uibiao, 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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  • High-dispersion loaded noble metal catalytic material and preparation method thereof
  • High-dispersion loaded noble metal catalytic material and preparation method thereof
  • High-dispersion loaded noble metal catalytic material and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0044] 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.

[0045] 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;

[0046] C. Stir the suspension obtained in step B at a constant temperature at 0°C, and...

Embodiment 2

[0048] 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.

[0049] 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;

[0050] 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

[0052] 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.

[0053] B. Weigh 0.5000 g of the 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 minutes to obtain a uniformly dispersed suspension;

[0054] C. Stir the suspension obtained in step B at a constant temperature at a temperature of 50°C, and add 470 microli...

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Abstract

The invention discloses a high-dispersion loaded noble metal catalytic material and a preparation method thereof. The preparation method includes the steps that a reductive LDH carrier, noble metal salt and a surfactant solution are mixed, and a high-dispersion loaded noble metal catalyst M / ZT-S is prepared through a one-step method. In the LDHs preparation process, variable-valence metal is directly introduced into an LDHs laminated plate, and the highly dispersed LDHs carrier with reductive sites is prepared. The high-dispersion reductive sites can spontaneously induce the reduction of the oxidation-state noble metal, and high dispersion of active component particles of a loaded noble metal catalyst is realized. Reduction is carried out without using a reducing agent or high-temperatureroasting. By changing the preparation temperature of the catalyst and adding surfactant conditions, the control over the particle size, distribution and stable loading of active components can be realized. The high-dispersion loaded catalyst shows good application effects in a benzene methanol selective oxidation reaction and an anthraquinone hydrogenation reaction.

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 Applications(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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