A preparation method of a porous alumina shell material that can improve the sintering resistance of noble metal nanoparticles

A technology of porous alumina and nanoparticles, applied in the direction of metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, catalyst protection, etc., can solve the problem of low shell porosity, cumbersome operation, and unfavorable active sites Expose the problems of reaction substrate diffusion and achieve the effect of simple operation, mild conditions and rich design ideas

Active Publication Date: 2021-11-19
UNIV OF JINAN
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] al 2 o 3 There are many reports on the preparation methods of shell materials. For example, Siqueros et al. used atomic layer deposition technology and used trimethylaluminum and water as precursors to successfully prepare Al 2 o 3 Shell material (Inorg. Chem. 2014, 53, 4872−4880), but dense Al 2 o 3 Shell layer, which is not conducive to the exposure of active sites and the diffusion of reaction substrates
In addition to atomic layer deposition, Wan et al. successfully coated Al on noble metal @C by hydrolyzing aluminum sulfate 2 o 3 (ACS Appl. Mater. Interfaces2015, 7, 27031−27034), this coating method needs a buffer solution as a reaction medium, the operation is cumbersome, and Al 2 o 3 Shell porosity is very low

Method used

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  • A preparation method of a porous alumina shell material that can improve the sintering resistance of noble metal nanoparticles
  • A preparation method of a porous alumina shell material that can improve the sintering resistance of noble metal nanoparticles

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Effect test

Embodiment 1

[0023] (a) 1.0 g Ce(NO 3 ) 3 . 6H 2 O was dissolved in 1 ml of deionized water, and 1 ml of CH was added with stirring 3 COOH and 30 ml ethylene glycol form a homogeneous solution, which is heated at 180°C for 200 min. Cool to room temperature, centrifuge, wash with water and ethanol, and dry to obtain spherical CeO 2 carrier material;

[0024] (b) 0.3 g spherical CeO 2 Disperse in 100 ml deionized water, sonicate to disperse, then add 1.254ml AuCl 3 ·HCl·4H 2 O solution was stirred for 1 h. Adjust the pH to neutral with NaOH solution (1 M). After standing for 30 min, 2 ml NaBH 4 (0.01 g) in water was added dropwise to the above solution. After stirring for 10 min, the spherical CeO was obtained by centrifugation, washing and drying. 2 - Au material;

[0025] (c) The above 20 mg spherical CeO 2 -Au, 10 mg Al(NO 3 ) 3 9H 2 O and 20 mg terephthalic acid (H 2 BDC) dispersed in 5 ml dimethylformamide (DMF) and 5 ml H 2 The mixed solution of O was heated in a wat...

Embodiment 2

[0028] (a) 1.0 g Ce(NO 3 ) 3 . 6H 2 O was dissolved in 1 ml of deionized water, and 1 ml of CH was added with stirring 3 COOH and 30 ml ethylene glycol form a homogeneous solution, which is heated at 180°C for 200 min. Cool to room temperature, centrifuge, wash with water and ethanol, and dry to obtain spherical CeO 2 carrier material;

[0029] (b) 0.3 g spherical CeO 2 Disperse in 100 ml deionized water, sonicate to disperse, then add 1.254ml AuCl 3 ·HCl·4H 2 O solution was stirred for 1 h. Adjust the pH to neutral with NaOH solution (1 M). After standing for 30 min, 2 ml NaBH 4 (0.01 g) in water was added dropwise to the above solution. After stirring for 10 min, the spherical CeO was obtained by centrifugation, washing and drying. 2 - Au material;

[0030] (c) The above 20 mg spherical CeO 2 -Au, 30 mg Al(NO 3 ) 3 9H 2 O and 20 mg terephthalic acid (H 2 BDC) dispersed in 5 ml dimethylformamide (DMF) and 5 ml H 2 The mixed solution of O was heated in a wat...

Embodiment 3

[0033] (a) Weigh 1.30 g Ce(NO 3 ) 3 . 6H 2 O and 14.4 g NaOH were dissolved in 20 ml and 40 ml high-purity water respectively, and after the cerium nitrate was completely dissolved, they were added to the 100 ml polytetrafluoroethylene liner filled with NaOH under stirring. After continuing to stir for 30 min, the lining was transferred to a stainless steel reactor, sealed and hydrothermally reacted at 100 °C for 24 h, cooled to room temperature, centrifuged, washed with water and ethanol, and dried at 80 °C to obtain rod-shaped CeO 2 carrier material;

[0034] (b) 0.3 g rod-like CeO 2 Disperse in 100 ml deionized water, sonicate to disperse, then add 1.254ml AuCl 3 ·HCl·4H 2 O solution was stirred for 1 h. Adjust the pH to neutral with NaOH solution (1 M). After standing for 30 min, 2 ml NaBH 4 (0.01 g) in water was added dropwise to the above solution. After stirring for 10 min, after centrifugation, washing and drying, the rod-shaped CeO 2 - Au material;

[0035...

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Abstract

The invention provides a preparation method of a porous alumina shell material which can improve the anti-sintering performance of noble metal particles. Firstly, the method of liquid phase reduction is used to load noble metal particles on the carrier, and then the carrier-noble metal, H 2 BDC and Al(NO 3 ) 3 9H 2 O is dispersed in a mixed solvent and reacted in a water bath for a certain period of time to obtain carrier-noble metal particles @MIL-53(Al). Carrier-noble metal particles@Al are obtained after high-temperature calcination 2 o 3 . The present invention relates to a method for preparing oxide-noble metal @MIL-53(Al) material by one-step synthesis on the basis of oxide-noble metal and calcined to obtain a porous alumina shell material that can improve the sintering resistance of noble metal particles .

Description

technical field [0001] The invention belongs to the technical field of functional materials. Specifically, the invention relates to a method for preparing a porous alumina shell material that can improve the sintering resistance of noble metal nanoparticles. Background technique [0002] Due to their high activity and selectivity, noble metal catalysts are widely used in reactions such as oxidation, reduction, and hydrogenation, and play a very important role in the fields of chemical industry, petroleum refining, petrochemical, pharmaceutical, environmental protection, and new energy. In order to improve the utilization rate of noble metals, noble metals are usually loaded on the carrier. Among them, oxide@noble metal is a catalyst combination with excellent performance in thermal catalytic oxidation reaction. However, at high reaction temperature, noble metals are prone to sintering and agglomeration, which affects the reactivity and reduces the utilization rate of noble...

Claims

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Application Information

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Patent Type & AuthorityPatents(China)
IPC IPC(8): B01J23/66B01J23/52B01J33/00
CPCB01J23/66B01J23/52B01J23/002B01J33/00B01J35/398
Inventor许田田陈国柱
OwnerUNIV OF JINAN