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Integral catalyst for producing cyclohexene with benzene hydrogenation and method for producing the same

A monolithic catalyst and cyclohexene technology, applied in chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, physical/chemical process catalysts, etc., can solve selectivity decline, catalyst wear, particle catalyst and The problem of separation of reaction liquid has not been solved, and the effect of reducing dosage, overcoming loss and simple preparation method is achieved.

Inactive Publication Date: 2008-09-24
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Regardless of whether it is a non-supported or supported catalyst, the mass transfer efficiency can only be improved by reducing the particle size and adding strong stirring, which makes the problem of rapid decline in conversion and selectivity caused by catalyst wear and sticking to the wall more prominent; The problem of separation of catalyst and reaction solution remains unresolved, making most of the inventions difficult to use in practical industries

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0036] The present invention also provides the preparation method of above-mentioned catalyst, its step comprises:

[0037] 1) Prepare a slurry, which includes one or more nitrates, hydroxides or oxides of main group metals or semimetals, add an appropriate amount of dilute nitric acid, the concentration of dilute nitric acid is 1%-10%, control The pH value is 1-3, and the ball milling time is 6-18 hours. Or use known methods to make nitrates, hydroxides or oxides of one or more of the above-mentioned main group metals or semimetals into a sol

[0038] 2) The above-mentioned ball mill slurry or sol is loaded on the whole honeycomb in a known way, and after being dried by microwave for 1-10 minutes, the firing temperature in a muffle furnace is 500-1500°C, preferably 800-1100°C

[0039] 3) The above-mentioned monolithic honeycomb loaded with auxiliary coatings supports noble metal active components or noble metals and transition metals to form a mixed solution. After microwave...

Embodiment 1

[0045] Preparation of Auxiliary Coating Precursor Slurry

[0046] Weigh 4.3gAl 2 o 3 ·3H 2 O, 5.5gAl(OH) 3 , 6.4g γ-Al 2 o 3 , 3.0gAl(NO 3 ) 3 and 60ml HNO 3 , After ball milling for 18 hours, a slurry suspension was obtained for use.

[0047] Catalyst preparation

[0048] 400cpsi overall honeycomb catalyst ( 1.02×2.2cm) with dilute HNO 3 Treatment, washing with deionized water, drying, high temperature treatment at 900°C, impregnating the above slurry suspension by conventional dipping method, microwave drying, heating to 1000°C in a muffle furnace and roasting for 2 hours. Subsequent impregnation of RuCl 3 Aqueous solution, heated to 300°C in a muffle furnace for 2 hours to obtain 0.3% Ru / Al 2 o 3 / Monolith Catalyst.

[0049] Catalyst evaluation

[0050] The whole reaction will be carried out in a fixed bed reactor. The prepared 2 monolithic honeycomb catalysts (every piece of catalyst volume is about 1.8ml) are put into the integration reactor, using 20% ​...

Embodiment 2

[0052] Auxiliary Coating Preparation

[0053] Weigh 12.0g of metatitanic acid, add HCl 15ml and HNO 3 5ml, ball milled for 18 hours to obtain a slurry suspension for use.

[0054] Catalyst preparation is identical with embodiment 1, obtains 0.3%Ru / TiO 2 / Monolith Catalyst. Evaluation conditions are the same as in Example 1. The results are shown in Table 1.

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Abstract

The invention relates to an integral catalyst used in making cyclohexene from benzene hydrogenation, taking a cordierite ceramic honeycomb or a metal honeycomb as a carrier, being coated with an additive accounting for 1-50wt percent of a honeycomb carrier in weight and an active component accounting for 0.05-10wt percent of a cellular carrier in weight; an accessory ingredient is one or more than one among Al2O3, SiO2, TiO2, ZrO2, La2O3, Fe2O3, ZnO, Cr2O3, GaO, CuO, BaO, CaO; the active component is precious metal such as Ru, Pt, Pd, or Rh, or the mixture of the precious metal and the additive. The integral honeycomb catalyst of the invention has a simple preparation method and the raw material is wide and easy to get. The active component of the integral catalyst of the invention is not so easy to lose, thereby reducing the amount of the precious metal, besides, the higher yield of cyclohexene and the selectivity can be obtained.

Description

technical field [0001] The invention relates to a catalyst used for hydrogenation of benzene to cyclohexene. [0002] The present invention also relates to a method for preparing the above-mentioned catalyst. Background technique [0003] Due to the presence of active double bonds, cyclohexene has become an important intermediate in organic synthesis, and can be widely used in the production of medicines, pesticides, feed additives, polyesters and other fine chemicals, especially in the synthesis of polyamides such as nylon 66. Ammonium is widely used in the industry. [0004] Traditional methods for producing cyclohexene include dehydration of cyclohexanol, dehydrohalogenation of halocyclohexane, dehydrogenation of cyclohexane, etc. These methods have disadvantages such as complex production process, high energy consumption, low yield and high cost, which make the production of cyclohexene unable to meet the development needs of modern synthetic industry. The selective h...

Claims

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Application Information

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IPC IPC(8): B01J23/46B01J23/40B01J21/16C07C5/11C07C13/20
CPCY02P20/52
Inventor 王树东赵玉军周瑾
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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