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Catalyst for preparing cyclohexene by benzene hydrogenation, its preparing method and using method

A catalyst, cyclohexene technology, applied to oxide or hydroxide catalysts, including metal fields, can solve problems such as difficult retention, and achieve long life, good selectivity, and high activity.

Inactive Publication Date: 2006-01-04
ZHENGZHOU UNIV +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The difficulty of the benzene partial hydrogenation route is that the hydrogenation of benzene is a continuous reaction, and it is difficult to stay in the stage of the intermediate product cyclohexene

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Put 2.7g of ruthenium chloride and 0.022g of lanthanum chloride in a 1000ml beaker, add 200ml of deionized water and stir to dissolve to obtain solution 1.

[0053] Add 9.0 g of zirconium dioxide into solution 1 and continue stirring for 30 minutes to obtain emulsion 2.

[0054] At 20°C, 2.7g of sodium borohydride was dissolved in 50ml of distilled water, and added dropwise to emulsion 2, and the emulsion changed from milky white to brown, brown, and black in turn. After the dropwise addition was completed, the stirring was stopped to obtain a cloudy solution 3, which was left to stand and separated into layers.

[0055] The supernatant in 3 was decanted, and the black solid in the lower layer was retained. Wash with deionized water several times in small amounts. 0.01mol / L silver nitrate solution was used to test the chlorine ions in the washing solution until no white precipitate was formed to obtain 10 g of supported amorphous alloy catalyst.

[0056] In the catal...

Embodiment 2

[0058] Put 4.1g of ruthenium chloride and 0.18g of lanthanum chloride in a 1000ml beaker, add 300ml of deionized water and stir to dissolve to obtain solution 1.

[0059] Add 8.5 g of zirconium dioxide to solution 1, and continue stirring for 40 minutes to obtain emulsion 2.

[0060] At 25°C, 10.2g of sodium borohydride was dissolved in 150ml of distilled water, and added dropwise to emulsion 2, and the emulsion changed from milky white to brown, brown, and black in turn. After the dropwise addition was completed, the stirring was stopped to obtain a cloudy solution 3, which was left to stand and separated into layers.

[0061] The supernatant in 3 was decanted, and the black solid in the lower layer was retained. Wash with deionized water several times in small amounts. 0.01mol / L silver nitrate solution was used to test the chlorine ions in the washing solution until no white precipitate was formed to obtain 10 g of supported amorphous alloy catalyst.

[0062] In the catal...

Embodiment 3

[0064] Put 5 g of ruthenium chloride and 0.35 g of lanthanum chloride in a 1000 ml beaker, add 300 ml of deionized water and stir to dissolve, to obtain solution 1.

[0065] Add 9g of zirconium dioxide into solution 1, and continue to stir for 40 minutes to obtain emulsion 2.

[0066] At 25°C, 15g of sodium borohydride was dissolved in 180ml of distilled water, and added dropwise to emulsion 2, and the emulsion changed from milky white to brown, brown, and black in turn. After the dropwise addition was completed, the stirring was stopped to obtain a cloudy solution 3, which was left to stand and separated into layers.

[0067] The supernatant in 3 was decanted, and the black solid in the lower layer was retained. Wash with deionized water several times in small amounts. Chloride ions in the washing solution were tested with 0.01mol / L silver nitrate solution until no white precipitate was formed, and 11 g of the supported amorphous alloy catalyst was obtained.

[0068] In th...

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PUM

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Abstract

The catalyst for hydrogenating benzene to prepare cyclohexene is supported non-crystal alloy Ru-M-B / ZrO2, with weight ratio between Ru-M-B and ZrO2 of 10-30 %. The preparation process of the catalyst is one chemical reduction process with micron level ZrO2 as carrier, Rh as active component, RE as assistant and borohydride as reductant. In the process, metal Rh, light RE and metal-like B are supported firmly in the non-crystal alloy Ru-M-B form onto ZrO2. The present invention also provides the usage of the catalyst in producing cyclohexene, and by considering the characteristic of continuous benzene hydrogenating reaction, the reaction slurry comprising water, ZrO2, ZnSO4.7H2O is used in deactivating the catalyst to raise the yield of cyclohexene and reduce the production of side product cyclohexane. The present invention is suitable for industrial cyclohexene production.

Description

Technical field: [0001] The invention belongs to the technical field including metal, oxide or hydroxide catalysts, and in particular relates to a preparation method and use method of a catalyst for hydrogenation of benzene to cyclohexene. Background technique: [0002] As an intermediate in organic synthesis, cyclohexene is widely used in the production of adipic acid, nylon 6, nylon 66, polyamide, polyester and other fine chemicals. Cyclohexene and its downstream products have important industrial uses and broad market prospects, and the hydrogenation of benzene to cyclohexene has huge industrial economic value. [0003] At present, in the production of nylon 6 and nylon 66, the complete hydrogenation of benzene is widely used at home and abroad: that is, the route of completely hydrogenating benzene to generate cyclohexane, and then oxidizing cyclohexane to generate a mixture of cyclohexanone and cyclohexanol. Since cyclohexane oxidation is a free radical reaction, it ca...

Claims

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Application Information

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IPC IPC(8): B01J23/63C07C5/11C07C13/20
CPCY02P20/52
Inventor 刘寿长刘木森李利民戴新民王向宇马源唐明生郑晓广张洪权李识寒陈聚良张结实姜继锁
Owner ZHENGZHOU UNIV
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