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Preparation method of Pd elementary substance coated ZnO nanorod array

A nanorod array and elemental technology, which is applied in the field of preparation of ZnO nanorod arrays, can solve the problems of many by-products, low catalytic efficiency, difficult separation and recovery of catalysts, etc., and achieves the effects of simple process, increased specific surface area, and avoidance of agglomeration.

Inactive Publication Date: 2014-08-13
DONGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, due to the limitations of its own reaction vessel and catalyst carrier, the traditional noble metal catalytic reaction has many inevitable disadvantages, such as low catalytic efficiency, many by-products, and the catalyst is not easy to separate and recycle.

Method used

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  • Preparation method of Pd elementary substance coated ZnO nanorod array
  • Preparation method of Pd elementary substance coated ZnO nanorod array
  • Preparation method of Pd elementary substance coated ZnO nanorod array

Examples

Experimental program
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Effect test

Embodiment 1

[0034] Prepare lotion I (the volume ratio of concentrated sulfuric acid, hydrogen peroxide and distilled water is 4:1:20) and lotion II (the volume ratio of ammonia, hydrogen peroxide and distilled water is 1:4:20). At room temperature, soak the microchannel in lotion I for 30 minutes, rinse with deionized water, then soak the microchannel in lotion II for 30 minutes, rinse with deionized water, and dry for later use. Simultaneously transport zinc acetate dihydrate ethanol solution (0.01M) and sodium hydroxide ethanol solution (0.04M) at a speed of 25 μL / min into the microchannel pre-placed in a 60°C oven, and stop the delivery after the microchannel is filled. , after reacting for 2 hours, the temperature was raised to 70°C, reacted for another 2h, and then heated to 150°C for 2h annealing, the microchannel was cleaned with deionized water, and dried at 150°C to obtain a ZnO seed layer film on the inner surface of the microchannel. At 90°C, the zinc nitrate hexahydrate soluti...

Embodiment 2

[0039]Prepare lotion I (the volume ratio of concentrated sulfuric acid, hydrogen peroxide and distilled water is 4:1:20) and lotion II (the volume ratio of ammonia, hydrogen peroxide and distilled water is 1:4:20). At room temperature, soak the microchannel in lotion I for 20 minutes, rinse with deionized water, then soak the microchannel in lotion II for 20 minutes, rinse with deionized water, and dry for later use; dihydrate zinc acetate ethanol The solution (0.01M) and the sodium hydroxide ethanol solution (0.04M) were delivered to the microchannel pre-placed in a 60°C oven at the same time at a speed of 25μL / min. After the microchannel was filled, the delivery was stopped, and the temperature was raised to 70°C, react for another 2h, heat up to 150°C and anneal for 2h, wash the microchannel with deionized water, and dry at 150°C to obtain a ZnO seed layer film on the inner surface of the microchannel; Zinc solution (0.05M) and hexamethylenetetramine solution (0.05M) were s...

Embodiment 3

[0044] Prepare lotion I (the volume ratio of concentrated sulfuric acid, hydrogen peroxide and distilled water is 4:1:20) and lotion II (the volume ratio of ammonia, hydrogen peroxide and distilled water is 1:4:20). At room temperature, soak the microchannel in lotion I for 40 minutes, rinse with deionized water, then soak the microchannel in lotion II for 40 minutes, rinse with deionized water, and dry for later use. Simultaneously transport zinc acetate dihydrate ethanol solution (0.01M) and sodium hydroxide ethanol solution (0.04M) at a speed of 25 μL / min into the microchannel pre-placed in a 60°C oven, and stop the delivery after the microchannel is filled. , After reacting for 2 hours, the temperature was raised to 70°C, and then reacted for 2 hours, and then the temperature was raised to 150°C for 2 hours of annealing. The microchannel was cleaned with deionized water and dried at 150° C. to obtain a ZnO seed layer film on the inner surface of the microchannel. At 90°C,...

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Abstract

The invention relates to a preparation method of a Pd elementary substance coated ZnO nanorod array. The preparation method comprises the following steps of: (1) cleaning a glass capillary micro-channel; simultaneously filling the cleaned micro-channel with zinc acetate dihydrate ethanol solution and sodium hydroxide ethanol solution to obtain a ZnO crystal seed layer thin film on the inner surface of the micro-channel, and simultaneously introducing zinc nitrate aqueous solution and hexamethylene tetramine aqueous solution into the micro-channel with the ZnO crystal seed thin film grown on the inner surface to obtain a ZnO nanorod array vertically grown on the inner surface of the micro-channel; (2) diluting acid solution of palladium salt by using de-ionized water, adding PVP (Polyvinyl Pyrrolidone) and then dropwise adding mixed solution of alcohol and water at a uniform speed to obtain Pd elementary substance sol; and (3) conveying the Pd elementary substance sol into the micro-channel with the ZnO nanorod array vertically grown on the inner surface obtained by the step (1) for coating, and finally drying. The method has the advantages of simple process and low cost; and the obtained Pd / ZnO nanorod array has a large specific area.

Description

technical field [0001] The invention belongs to the field of preparation of ZnO nano-rod arrays, in particular to a preparation method of Pd simple substance-coated ZnO nano-rod arrays. Background technique [0002] Due to their irreplaceable catalytic activity and selectivity, noble metal catalysts play an extremely important role in pharmaceutical preparation, petrochemical industry and organic synthesis. As an excellent noble metal catalyst, palladium has excellent catalytic performance. It is widely used in various organic chemical reactions such as hydrogenation, oxidative dehydrogenation, hydrocracking, coupling, and automobile exhaust purification. It is widely used in the petrochemical industry The application in the catalyst even surpasses the platinum catalyst. However, due to the limitations of the reaction vessel and the catalyst carrier, the traditional noble metal catalyzed reaction has many inevitable disadvantages, such as low catalytic efficiency, many by-p...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/60B01J19/00
Inventor 王宏志张权李耀刚张青红
Owner DONGHUA UNIV
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