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Preparation method of cyclohexene catalyst, as well as preparation method and device of cyclohexene

A cyclohexene and catalyst technology, which is applied in the field of chemical raw material preparation, can solve the problems of separation of granular catalyst and reaction solution, difficult application of catalyst, loss of catalyst, etc., and achieve uniform distribution of active components, easy industrial production, and high utilization rate Effect

Inactive Publication Date: 2014-02-12
张天来 +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0004] In the fluidized bed reactor, the catalyst is in the form of particles, and the activity of the catalyst is mainly increased by adding stirring power, which will cause the catalyst to wear and stick to the wall, resulting in a rapid decline in conversion and selectivity; in addition, there are particle catalysts and reaction liquids. Separation problems, leading to severe loss of catalyst, which makes most of these catalysts and their processes difficult to apply in actual industry

Method used

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  • Preparation method of cyclohexene catalyst, as well as preparation method and device of cyclohexene

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preparation example Construction

[0017] The preparation method of cyclohexene catalyst, catalyst is made up of active component A, auxiliary agent M and carrier, and preparation method is: with ACl 3 ·nH 2 O is the precursor of the active component A, the soluble salt is used as the precursor of the auxiliary agent M, and then the carrier is added. The mass percentage of each component is: based on the carrier, the active component A is 3 to 10% of the carrier, and the auxiliary agent M is 10-20% of the active component A; add an organic solvent and stir evenly to obtain a solution, then stir and evaporate to dryness to remove organic matter to obtain a solid powder, which is compressed into a tablet to obtain a solid catalyst.

[0018] The additive M is one or two compounds of Zn, Fe, Ni, La. ZnSO is preferred 4 , FeSO 4 .

[0019] The carrier is one or a mixture of Si, Al, Co, Cr, Ti, Zr oxides. ZrO is preferred 2 , SiO 2 、Al 2 o 3 .

[0020] The organic solvent is one of hexanediol, formaldehyde ...

Embodiment approach 1

[0031] First add 9.5g of carrier (SiO 2 / ZrO 2 =1:4) into about 50ml of hexanediol solution, heated to 160°C in an oil bath, stirred the carrier solution for 1 hour, and then added 1.295 ACl 3 ·nH 2 O, after stirring for 3 h, the temperature was raised to 250° C., stirred and evaporated to dryness, and the organic solution was removed to obtain a gray powdery substance.

[0032] The powder was compressed into 30-mesh granules and loaded into a fixed-bed reactor with a volume of 20 ml.

[0033] Before the reaction, first raise the temperature to 350°C, and pass H under the pressure of 0.2MPa 2 , the flow rate is 20ml / min, and the reduction operation is carried out for 8h.

[0034] After confirming that the restoration is complete, H 2 The flow rate is increased to 1000mi / min, the system pressure is increased to 4.0MPa, when the temperature reaches 150°C, 2.0wt% ZnSO is introduced into the reactor 4 The aqueous solution (pH=5.5) was pretreated for 4 hours, and then benzene...

Embodiment approach 2

[0036] First add 9.5g of carrier (SiO 2 / ZrO 2 =1:4) into about 50ml of hexanediol solution, heated to 160°C in an oil bath, and after the carrier solution was stirred for 1h, 1.295g of ACl was added 3 ·nH 2 O, 0.129g ZnCl 2 After stirring for 3 h, the temperature was raised to 250° C., stirred and evaporated to dryness, and the organic solution was removed to obtain a gray powdery substance.

[0037] The powder was compressed into 30-mesh granules and loaded into a fixed-bed reactor with a volume of 20 ml.

[0038] Before the reaction, first raise the temperature to 350°C, and pass H under the pressure of 0.2MPa 2 , the flow rate is 20ml / min, and the reduction operation is carried out for 8h.

[0039] After reduction, H 2The flow rate is raised to 1000ml / min, the system pressure is raised to 4.0MPa, and when the temperature reaches 150°C, 2.0wt% ZnSO is introduced into the reactor 4 The aqueous solution (pH=5.5) was pretreated for 4 hours, and then benzene was introduc...

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Abstract

The invention discloses a preparation method of a cyclohexene catalyst, as well as a preparation method and device of cyclohexene, and belongs to the technical field of preparation of chemical raw materials. The preparation method of the cyclohexene catalyst comprises the following steps: taking ACl3. nH2O as a precursor of an active component A, taking a soluble salt as the precursor of an additive M and further adding a carrier, wherein the percentage by weight of each component is as shown in the specification: taking the carrier as the reference, ensuring that the active component A accounts for 3-10% of the carrier, and the additive M accounts for 10-20% of the active component A; and further adding an organic solvent, uniformly stirring, preparing a solution, further stirring, evaporating, removing organic matters, obtaining solid powder, and compressing to form a tablet so as to prepare the solid catalyst. According to the preparation method of the cyclohexene catalyst, a reactor filled with the solid catalyst is taken as the core, and the preparation method comprises reduction of the catalyst and catalytic reaction. The device comprises a mixer, a pressure stabilizer, the reactor, an oil-water separator and a solvent pump. The cyclohexene catalyst prepared by the preparation method disclosed by the invention has the advantages of relatively high activity, selectivity and thermal-mechanical stability, simple preparation process and easiness in industrial production; and the preparation of the cyclohexene adopts the fixed bed reactor, so that the distribution of active components of the catalyst is relatively uniform, and the utilization rate of precious metals is relatively high.

Description

Technical field [0001] The invention relates to the preparation of chemical raw materials, especially the preparation of cyclohexene, and belongs to the technical field of chemical raw material preparation. Background technique [0002] Due to its active double bond, cyclohexene has become an important organic intermediate, which can be widely used in the production of medicine, pesticide, feed additive, polyester and other fine chemicals. Cyclohexene has no natural products and must be chemically synthesized, and hydrogenation of benzene is the best route. In particular, cyclohexene is produced by partial hydrogenation of benzene, and then cyclohexanol and cyclohexanone are produced, which is safer and more reliable than the traditional route of complete hydrogenation of benzene to produce alcohols and ketones. It consumes one-third less hydrogen and has a carbon yield of 100. %; energy-saving and high-efficiency, and conducive to environmental protection. [0003] At pre...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/38B01J23/60B01J23/66B01J23/89C07C13/20C07C5/11
Inventor 张天来李建修
Owner 张天来
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