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Method for preparing cyclohexene by selectively hydrogenising benzene in magnetic stabilization bed

A technology of selective hydrogenation and magnetically stabilized bed, applied in the fields of hydrogenation to hydrocarbons, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc. Hexene cannot be separated out in time, so as to improve the selectivity and yield, reduce the loss and reduce the production cost.

Inactive Publication Date: 2012-06-27
CHINA UNIV OF PETROLEUM (EAST CHINA)
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

At present, the most widely used method of selective hydrogenation of benzene to prepare cyclohexene is carried out in a high-pressure reactor, but it has the biggest disadvantage that cyclohexene cannot be separated in time and will be further hydrogenated to form cyclohexane, thereby The selectivity and yield of cyclohexene are reduced. In order to solve this problem, we have used a new method of selective hydrogenation of benzene to prepare cyclohexene——selective hydrogenation of benzene in a magnetically stabilized bed to prepare cyclohexene. In this preparation method, cyclohexene will be separated in time as the reaction proceeds, so that cyclohexene will not be further hydrogenated to generate cyclohexane, thereby improving the selectivity and yield of cyclohexene

Method used

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  • Method for preparing cyclohexene by selectively hydrogenising benzene in magnetic stabilization bed

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Embodiment 1

[0015] 1) The coercive force of the magnetic catalyst carrier is 2kA / m, and the specific saturation magnetization is 10Am 2 / kg, the magnetic core is Fe 3 o 4 , the magnetic core size is 1 μm, and the cladding layer is γ-Al 2 o 3 The thickness of the cladding layer is 20μm, the mass fraction of the magnetic core is 20%, and 0.01mol / L RuCl is configured 3 Aqueous solution, and add additive ZnCl 2 aqueous solution, the molar ratio of Ru to metal ions in the auxiliary agent is 5:1, the magnetic catalyst carrier is immersed in the above mixed solution for 3 hours, and then 0.5mol / L NaBH is added dropwise 4 Aqueous solution, control NaBH 4 mixed with solution metal ions Ru 3+ , Zn 2+ The molar ratio is 10:1 to ensure that the metal cations are completely reduced, so that the loading of Ru is 2wt%, and then the magnetic catalyst is washed with deionized water to neutrality, and then washed three times with absolute ethanol, and finally the catalyst sample is stored in Preven...

Embodiment 2

[0019] 1) The coercive force of the magnetic catalyst carrier is 20kA / m, and the specific saturation magnetization is 15Am 2 / kg, the magnetic core is γ-Fe 2 o 3 , the magnetic core size is 5 μm, and the cladding layer is γ-Al 2 o 3 The thickness of the cladding layer is 50 μm, the mass fraction of the magnetic core is 10%, and 0.05mol / L RuCl is configured 3 Aqueous solution, and add additive ZnCl 2 aqueous solution, the molar ratio of Ru to metal ions in the additive is 8:1, the magnetic catalyst carrier is immersed in the above mixed solution for 2 hours, and then 0.5mol / L NaBH is added dropwise 4 Aqueous solution, control NaBH 4 mixed with solution metal ions Ru 3+ , Zn 2+ The molar ratio is 20:1 to ensure that the metal cations are completely reduced, so that the loading of Ru is 5wt%, then the magnetic catalyst is washed with deionized water to neutrality, and then washed three times with absolute ethanol, and finally the catalyst sample is stored in Prevent oxida...

Embodiment 3

[0023] 1) The coercive force of the magnetic catalyst carrier is 10kA / m, and the specific saturation magnetization is 12Am 2 / kg, the magnetic core is Fe 3 o 4 , the magnetic core size is 3 μm, and the cladding layer is γ-Al 2 o 3 The thickness of the cladding layer is 100 μm, the mass fraction of the magnetic core is 40%, and 0.01mol / L RuCl is configured 3 Aqueous solution, and add additive ZnSO 4 aqueous solution, the molar ratio of Ru to metal ions in the auxiliary agent is 10:1, the magnetic catalyst carrier is immersed in the above mixed solution for 3 hours, and then 1mol / L NaBH is added dropwise 4 Aqueous solution, control NaBH 4 mixed with solution metal ions Ru 3+ , Zn 2+ The molar ratio is 15:1 to ensure that the metal cations are completely reduced, so that the loading of Ru is 3wt%, then the magnetic catalyst is washed with deionized water to neutrality, and then washed three times with absolute ethanol, and finally the catalyst sample is stored in Prevent ...

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Abstract

The invention discloses a method for preparing cyclohexene by selectively hydrogenising benzene in a magnetic stabilization bed. The method comprises the following steps: filling a magnetic catalyst into a reaction tube; placing the reaction tube into a uniform magnetic field; utilizing a micro reactor device to control the reaction conditions and the magnetic field intensity; injecting a heated reaction fluid into the reaction tube, thereby forming a magnetic stable state; and preparing the cyclohexene by selectively hydrogenising benzene. According to the method provided by the invention, the high-pressure micro reaction is combined with the magnetic stabilization bed, so that the hydrogenising time is controlled and the continuous operation is realized; the magnetic stabilization bed is utilized to prepare the cyclohexene by selectively hydrogenising benzene, so that the benzene conversion rate can be increased and the selectivity and yield of the cyclohexene can be increased; and the magnetic field is utilized to separate and recover the catalyst, so that the production cost is lowered.

Description

technical field [0001] The invention relates to a method for preparing cyclohexene through selective hydrogenation of benzene in a magnetically stable bed. Background technique [0002] Cyclohexene is an important intermediate in organic synthesis, widely used in the production of medicine, pesticide, polyester and other fine chemicals. There are many ways to obtain cyclohexene in industry. Traditionally, cyclohexene is mainly obtained by dehydration of cyclohexanol, dehalogenation of halogenated cyclohexane, dehydrogenation of cyclohexane, etc., which has the disadvantages of complex production process and high cost. , cannot meet the needs of industrialized large-scale production, so that the application of cyclohexene is limited to the production of high value-added products such as lysine and cyclohexene oxide. One-step selective hydrogenation of benzene to synthesize cyclohexene can shorten the process flow and save equipment investment, and the raw material benzene ha...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C13/20C07C5/11B01J23/89
CPCY02P20/52Y02P20/584
Inventor 于濂清董开拓智倩倩钟晓亮刘晨光
Owner CHINA UNIV OF PETROLEUM (EAST CHINA)
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