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B-containing nano crystalline Ru-based catalyst, preparation method and applications thereof

A catalyst and nanocrystalline technology, which is applied in the field of selective hydrogenation of benzene to cyclohexene containing B nanocrystalline Ru-based catalysts, can solve the problems of low cyclohexene selectivity, high material requirements, equipment corrosion, etc., and achieve Effect of high activity and cyclohexene selectivity, reduced requirements, good thermal stability

Active Publication Date: 2014-04-30
ZHENGZHOU NORMAL UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The slurry is acidic under hydrogenation conditions, causing severe corrosion to equipment and requiring high material requirements, but the selectivity of cyclohexene is still low

Method used

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  • B-containing nano crystalline Ru-based catalyst, preparation method and applications thereof
  • B-containing nano crystalline Ru-based catalyst, preparation method and applications thereof
  • B-containing nano crystalline Ru-based catalyst, preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] Mix 1.71g of ruthenium trichloride (containing 0.65g of metal Ru), 0.0242g of boric acid and 0.0024g of zinc oxide into 400ml of distilled water to prepare a slurry, and adjust its pH value to 6-7 with ammonia water. The above solution was poured into a 1L Hastelloy-lined reactor, and the temperature was raised to 100° C. for 5 hours, and the stirring rate was controlled at 200 r / min during the process. The slurry was cooled and taken out, and suction filtered until the pH of the filtrate=7. Mix the obtained solid and 400ml of distilled water into the reaction kettle, and reduce for 3h under the reducing conditions of hydrogen pressure of 2MPa, temperature controlled at 140°C and stirring speed of 1200r / min. The obtained solid is nano RuZnB crystalline alloy. The XRD spectrum of the catalyst is shown in figure 1 , the diffraction peaks at 38.3°, 43.8°, 58.2°, 69.4° and 78.1° in the figure all belong to the characteristic peaks of crystalline metal Ru. It can be seen ...

Embodiment 2

[0034] 0.0024g zinc oxide is changed into 0.0029g zinc hydroxide of equivalent substance amount, and other conditions are with embodiment 1. The XRD spectrum of the catalyst is shown in figure 2 , it can be seen that it is similar to the XRD spectrum of the catalyst in Example 1, and the diffraction peaks at 38.3°, 43.8°, 58.2°, 69.4° and 78.1° in the figure all belong to the characteristic peaks of crystalline metal Ru. It can be seen that the catalyst is in a crystalline state, and the Ru crystallite size is 4.4nh as measured by the FWHM method. Inductively coupled plasma atomic emission spectrometry measured that the mass percentage of Zn in the catalyst was 0.31%, and the mass percentage of B was 0.57%.

Embodiment 3

[0036]Change 0.0242g boric acid and 0.0024g zinc oxide into 0.0197g borax and 0.0085g zinc sulfate heptahydrate, and other conditions are with embodiment 1. The XRD spectrum of the catalyst is shown in image 3 , it can be seen that it is similar to the XRD spectrum of the catalyst in Example 1, and the diffraction peaks at 38.3°, 43.8°, 58.2°, 69.4° and 78.1° in the figure all belong to the characteristic peaks of crystalline metal Ru. The Ru crystallite size was measured to be 4.2nh by FWHM method. The mass percentage of Zn in the catalyst was measured by inductively coupled plasma atomic emission spectrometry to be 0.32%, and the mass percentage of B was 0.58%.

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Abstract

The invention discloses a B-containing nano crystalline Ru-based catalyst and the application thereof in preparation of cyclohexene by selective hydrogenation. The catalyst contains B, Ru and Zn, and the catalyst is characterized in that the crystallite size of Ru is 3-7nm, and a 2-theta angle of an XRD spectrum diagram is 38.2-38.4 DEG, 43.7-43.9 DEG, 58.1-58.3 DEG, 69.3-69.5 DEG, and / or 78.0-78.2 DEG, and has a characteristic peak. The catalyst disclosed by the invention makes up for a thermodynamic instability characteristic of an amorphous Ru-B catalyst, and has good thermal stability, and in the presence of zinc sulfate, the activity, selectivity and stability of the catalyst are higher than those of a traditional industrial catalyst; and in the absence of zinc sulfate, the catalyst also has high cyclohexene selectivity. The catalyst disclosed by the invention has a good industrial application prospect.

Description

technical field [0001] The invention belongs to the field of chemical industry, and in particular relates to a B-containing nanocrystalline Ru-based catalyst for preparing cyclohexene through selective hydrogenation of benzene, a preparation method and application thereof. Background technique [0002] With the rapid development of construction, decoration, automobile, and national defense industries, the demand for chemical products such as cyclohexanone, adipic acid, nylon-6, and nylon-66 is increasing day by day. Most of the above-mentioned products are currently produced by the traditional benzene complete hydrogenation route in my country, which has potential safety hazards, waste of resources and environmental pollution. In contrast, the hydrogenation route of benzene consumes less than one-third of the hydrogen, the utilization rate of carbon atoms is 100%, and it is environmentally friendly. So far, only Japan has realized the industrialization of benzene selective ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/60C07C13/20C07C5/11
Inventor 孙海杰陈凌霞秦会安李永宇陈秀丽黄振旭穆兵赵文伯王鑫
Owner ZHENGZHOU NORMAL UNIV
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