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A kind of preparation method of zrO2 nano sheet supported ruthenium catalyst

A technology of ruthenium catalysts and nanosheets, 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 , to promote desorption, the effect of high dispersion of Ru

Active Publication Date: 2018-06-15
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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  • A kind of preparation method of zrO2 nano sheet supported ruthenium catalyst
  • A kind of preparation method of zrO2 nano sheet supported ruthenium catalyst
  • A kind of preparation method of zrO2 nano sheet supported ruthenium catalyst

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Experimental program
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Effect test

Embodiment 1

[0028] Weigh 1.3 g RuNO (NO 3 ) 3 , 17.1 g ZrO(NO 3 ) 2 2H 2 O was dissolved in 156 mL deionized water, transferred to a 200 mL hydrothermal kettle, heated at 170 °C for 6 h, and naturally cooled to room temperature to obtain a khaki slurry; the slurry was taken out and washed with 10 wt.% NaOH solution As a precipitating agent, precipitation was carried out at 60 °C, and the pH at the end of the precipitation was controlled to be 9, and it was aged for 4 h; the obtained precipitate was centrifuged and washed with deionized water until it was neutral; after the precipitate was vacuum-dried at 80 °C for 12 h, Calcined at 200 °C for 6 h under hydrogen atmosphere.

Embodiment 2

[0030] Weigh 0.48 g KRuO 4 , 17.1 g ZrO(NO 3 ) 2 2H 2 O was dissolved in 156 mL of 10 vol.% alcohol solution, transferred to a 200 mL hydrothermal kettle, heated at 130 °C for 18 h, and naturally cooled to room temperature to obtain a khaki-yellow slurry; the slurry was taken out and washed with 10 wt.% KOH solution was used as a precipitating agent, and the precipitation was carried out at 70 °C. The pH of the precipitation termination was controlled to be 13, and the precipitation was left to age for 12 h; the obtained precipitate was washed with deionized water to neutrality; After drying for 12 h, they were calcined at 450 °C for 4 h in a hydrogen atmosphere.

Embodiment 3

[0032] Weigh 2.14 g RuCl 3 ·3H 2 O, 20.6 g ZrOCl 2 ·8H 2 O was dissolved in 150 mL of deionized water, transferred to a hydrothermal kettle with a capacity of 200 mL, heated at 150 °C for 12 h, and naturally cooled to room temperature to obtain a khaki-yellow slurry; the slurry was taken out and washed with 10 wt.% NaOH solution As a precipitating agent, precipitate at 80 °C, control the pH of the end of the precipitation to 10, let stand and age for 12 h, add 1 mL of 30 wt.% 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 h, and then calcined at 300 °C for 4 h in a hydrogen atmosphere.

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Abstract

The invention discloses a preparation method of a ZrO2 nanosheet-supported ruthenium catalyst. The catalyst is loaded on a ZrO2 nanosheet by metal Ru, and the Ru loading amount is 1-10 wt.% (based on ZrO2). The preparation method is as follows: Prepared by hydrothermal-precipitation method, the active component Ru is anchored on ZrO2 nanosheets (ZrO2-NS) to prepare nanocomposite catalysts, and the soluble salt solution of Ru and Zr is mixed to obtain the crystal nucleus of the catalyst precursor through hydrothermal reaction; then by A precipitating agent was introduced, followed by drying and reduction to obtain a ZrO2 nanosheet-supported ruthenium catalyst (Ru / ZrO2‑NS) catalyst. Compared with other loaded benzene hydrogenation catalysts, the catalyst Ru prepared by the present invention is uniformly distributed on the ZrO2 nanosheets, has a high degree of dispersion, and its preparation process is simple; it is used for the partial hydrogenation of benzene to prepare cyclohexene, and has a high conversion rate , good 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 for the...

Claims

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Application Information

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Patent Type & Authority Patents(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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