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Sintering-resisting loading type nanometer palladium catalyst and preparing method and application thereof

A supported catalyst technology, which is applied in the field of anti-sintering nano-Pd catalysts, can solve the problems of industrial application limitations, long preparation cycle, cumbersome preparation process, etc., and achieve improved anti-sintering performance, excellent CO ignition performance, and improved dispersion. Effect

Inactive Publication Date: 2013-01-16
XIAMEN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although the catalyst prepared by this method can effectively inhibit the agglomeration of metal particles in a certain temperature range, its high temperature (>700°C) stability) still needs to be improved, and due to the special structure of the encapsulated catalyst, the reactants must first Diffusion passes through the cladding layer to reach the metal active center, and there is a contact problem between the metal active phase and the substrate in the reaction, while PdSiO 2 The preparation process is relatively cumbersome, the preparation cycle is long, and it needs to go through processes such as precipitation, suction filtration, washing, drying, and roasting, so that its industrial application is subject to certain restrictions.
Therefore, it is very difficult and challenging to explore a simple method to prepare highly dispersed, sintering-resistant Pd-supported catalysts.

Method used

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  • Sintering-resisting loading type nanometer palladium catalyst and preparing method and application thereof
  • Sintering-resisting loading type nanometer palladium catalyst and preparing method and application thereof
  • Sintering-resisting loading type nanometer palladium catalyst and preparing method and application thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Weigh 10g SiO 2 Carrier (Aldrich Chemical Company, 35~60 mesh), soaked in 20% dilute nitric acid solution for 24h, stirred 3~5 times during the period, then washed with distilled water to pH=7.0, dried at 110°C for 12h, and set aside. 2g of processed SiO 2 Immerse in 6ml of Pd with a mass concentration of 1.04mg / ml for 24h, then dry at 110°C for 12h, roast at 800°C in air for 2h, the heating rate is 10°C / min, and 600°C in high-purity hydrogen C reduced for 0.5h to get 3wt%Pd / SiO 2 -800-Air catalyst, denoted as Cat 1, the particle size of Pd particles is 3.1nm, see figure 1 and 2 .

[0027] Take by weighing 10mg above-mentioned catalyst Cat 1 and pack in the micro-fixed-bed flow reactor, catalyst first in high-purity H 2 Heat up to 600°C at a rate of 20°C / min in the gas stream, reduce for 30 minutes, cool down to room temperature, switch to high-purity He for about 20 minutes, and then switch to CO / O 2 / He (1 / 1 / 98, volume ratio) reaction gas for heating reaction, t...

Embodiment 2

[0035] Implementation steps and conditions are the same as embodiment 1, but catalyst roasting atmosphere is changed into N by air 2 , to get 3wt%Pd / SiO 2 -800-N 2 Catalyst, denoted as Cat 2, the particle size of Pd particles is 3.8nm, see Figure 5 and 6 , and its CO oxidation reaction performance results are shown in Table 1.

Embodiment 3

[0039] Implementation steps and conditions are the same as in Example 1, except that the solvent acetylacetone used as palladium acetylacetonate is changed to toluene to obtain 3wt%Pd / SiO 2 -800-Air-2 catalyst, denoted as Cat 3, the particle size of Pd particles is 3.1nm, and its CO oxidation reaction performance results are shown in Table 1.

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Abstract

A sintering-resisting loading type nanometer palladium catalyst and a preparing method and application thereof relate to a nanometer metal catalyst. The sintering-resisting loading type nanometer palladium catalyst contains active component acetylacetone palladium and carrier SiO2, and metal Pd occupies 0.5-5.0% of the sintering-resisting loading type nanometer palladium catalyst according to mass percent. The preparing method of the sintering-resisting loading type nanometer palladium catalyst includes steps: (1) SiO2 is selected to serve as the carrier, immersed into nitric acid solution and washed until the pH of SiO2 is 6.5-7.0, and then is dried; (2) Pd (acac) 2 compound is dissolved in acetylacetone or toluene solvents to prepare Pd (acac) 2 solution with mass concentration of Pd to be 0.26-1.04 mg / ml; (3) SiO2 obtained in the step (1) is immersed into the metal salt solution obtained in the step (2), and an initial catalyst is obtained after drying and roasting; and (4) the initial catalyst obtained in the step (3) is subjected to hydrogen gas reduction, and the sintering-resisting loading type nanometer palladium catalyst is finally obtained.

Description

technical field [0001] The invention relates to a nanometer metal catalyst, in particular to a sintering-resistant nanometer Pd catalyst, which is prepared by a simple impregnation method and its application in CO oxidation reaction. Background technique [0002] Supported Pd catalyst is one of the most important metal catalysts, which can be widely used in reactions such as olefin hydrogenation, alcohol oxidation, coupling reaction, automobile exhaust elimination, CO oxidation treatment, etc. The size is closely related, usually the Pd catalyst with smaller particles has better catalytic performance. Okada et al. (Catalysis Today, 2011, doi:10.1016 / j.cattod.2011.08.014) compared the preparation of nano-Pd / SiO by deposition and impregnation methods 2 It was found that the particle size of Pd on the catalyst prepared by the deposition method (3.9nm) was significantly smaller than that of the catalyst prepared by the impregnation method (6~12nm), and the former was more condu...

Claims

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Application Information

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IPC IPC(8): B01J23/44C01B31/20C01B32/50
Inventor 翁维正李兵章青万惠霖
Owner XIAMEN UNIV
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