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Preparation method of ZrO2 nanosheet supported ruthenium catalyst

A ruthenium catalyst and nanosheet technology, which is applied in the field of preparation of ZrO2 nanosheet-supported ruthenium catalysts, can solve the problems of large amount of non-supported precious metal Ru, agglomeration and deactivation, etc., and achieve the promotion of gas-solid-water-oil four-phase reaction , promote desorption, and enhance the effect of force

Active Publication Date: 2016-07-06
FUZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Simplify the preparation process, optimize the texture of the catalyst, promote the mass transfer process of the reaction, and solve the problem that the unsupported noble metal Ru of the catalyst is large in amount and easy to agglomerate and deactivate

Method used

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  • Preparation method of ZrO2 nanosheet supported ruthenium catalyst
  • Preparation method of ZrO2 nanosheet supported ruthenium catalyst
  • Preparation method of ZrO2 nanosheet supported ruthenium catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Weigh 1.3gRuNO (NO 3 ) 3 , 17.1gZrO(NO 3 ) 2 2H 2 O was dissolved in 156mL deionized water, transferred to a hydrothermal kettle with a volume of 200mL, heated at 170°C for 6h, and naturally cooled to room temperature to obtain a khaki-yellow slurry; the slurry was taken out, and 10wt.% NaOH solution was used as a precipitating agent. Precipitate at 60°C, control the pH at the end of the precipitation to be 9, and let it stand for 4 hours; centrifuge and wash the obtained precipitate with deionized water until it is neutral; vacuum dry the precipitate at 80°C for 12 hours, and then store it in a hydrogen atmosphere at 200°C Roasting 6h.

Embodiment 2

[0030] Weigh 0.48gKRuO 4 , 17.1gZrO(NO 3 ) 2 2H 2 O was dissolved in 156mL of 10vol.% alcohol solution, transferred to a 200mL hydrothermal kettle, heated in water at 130°C for 18 hours, and naturally cooled to room temperature to obtain a khaki-yellow slurry; take out the slurry, and use 10wt.% KOH solution as Precipitant, precipitate at 70°C, control the pH of the end of the precipitation to be 13, and let it stand for 12 hours; centrifuge and wash the obtained precipitate with deionized water until neutral; dry the precipitate at 80°C for 12 hours in a hydrogen atmosphere Calcined at 450°C for 4h.

Embodiment 3

[0032] Weigh 2.14gRuCl 3 ·3H 2 O, 20.6gZrOCl 2 ·8H 2 O was dissolved in 150mL deionized water, transferred to a hydrothermal kettle with a volume of 200mL, heated at 150°C for 12h, and naturally cooled to room temperature to obtain a khaki slurry; the slurry was taken out, and 10wt.% NaOH solution was used as a precipitating agent. Precipitate at 80°C, control the pH at the end of the precipitation to 10, let it stand for 12 hours, add 1mL of 30wt.%H 2 o 2 solution; the resulting precipitate was centrifuged and washed with a mixture of acetone and deionized water (volume ratio 1:5) until AgNO 3 The solution was detected to be free of chloride ions; the precipitate was vacuum-dried at 80° C. for 12 hours, and then calcined at 300° C. for 4 hours under a hydrogen atmosphere.

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Abstract

The invention discloses a preparation method of a ZrO2 nanosheet supported ruthenium catalyst. The catalyst is characterized in that metal Ru is supported on a ZrO2 nanosheet and the loading volume of Ru is 1wt%-10wt% (subjected to ZrO2). The preparation method comprises the following steps: with a hydrothermal-precipitation method, anchoring the active component Ru on the ZrO2 nanosheet (ZrO2-NS) for preparing a nanometer compound catalyst; mixing Ru and Zr soluble salt solutions and conducting hydrothermal reaction, thereby acquiring a catalyst precursor crystal nucleus; and introducing a precipitator, drying and reducing, thereby acquiring the ZrO2 nanosheet supported ruthenium catalyst (Ru / ZrO2-NS). Compared with other supported type benzene hydrogenation catalyst, the catalyst prepared according to the method provided by the invention has the advantages that Ru is uniformly distributed on the ZrO2 nanosheet, the dispersity is high and the preparation process is simple, when applied to reaction for local benzene hydrogenation for preparing cyclohexene, the catalyst has the advantages of high conversion rate, excellent selectivity and high stability.

Description

technical field [0001] The present invention relates to a kind of ZrO 2 The invention discloses a method for preparing a ruthenium catalyst supported by nanosheets, belonging to the technical field of catalyst preparation. Background technique [0002] Cyclohexene is an extremely important chemical intermediate widely used in the production of pharmaceuticals, agricultural chemicals, feed, polyester materials and other fine chemical products. Cyclohexene is usually prepared by dehydration of cyclohexanol. Traditional preparation methods include halocyclohexane dehalogenation method and Brich reduction method, but both have disadvantages such as complex process, many by-products, large energy consumption and serious environmental pollution. In comparison, the partial hydrogenation of benzene to cyclohexene is atom-economical, which can reduce energy consumption and improve economic benefits. However, from a thermodynamic point of view, the standard Gibbs free energy of the ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/46C07C5/05C07C13/20
CPCC07C5/05C07C13/20B01J23/462C07C2523/46B01J35/396Y02P20/52
Inventor 詹瑛瑛钟世腾董森陈崇启郭学华辜冬梅彭胜江莉龙王亚涛
Owner FUZHOU UNIV
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