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Preparation method and application of gamma-alumina supported aluminum trichloride catalyst

A technology for loading aluminum trichloride and alumina carriers, applied in physical/chemical process catalysts, chemical instruments and methods, organic chemistry, etc., can solve the problems of increasing the difficulty of post-processing, difficulty in recycling, and affecting the service life of devices, etc. Achieve the effects of reducing pollution and corrosion of equipment, facilitating industrial production, and high efficiency of immobilized reaction

Inactive Publication Date: 2014-07-09
EAST CHINA UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, AlCl 3 While the catalyst has extremely high activity, it also has obvious shortcomings: ①It is highly corrosive, and it is easy to damage the reactor and other devices, which affects the service life of the device; ②The use of AlCl 3 Catalysts will produce a large amount of sewage during polymerization production, which will seriously pollute the environment if they cannot be treated in time; ③It is difficult to recycle after the reaction, and post-treatment is required, otherwise a large amount of corrosive waste will be generated
The gas-phase method needs to be reacted at high temperature, which requires high equipment and high energy consumption; after the immobilization is completed, it is necessary to blow off unreacted AlCl with carrier gas at high temperature 3 , which can easily cause environmental pollution
The solution method is relatively simple, but the often used CCl 4 、CH 3 C1 or CH 2 Cl 2 Solvent vs. AlCl 3 low solubility and low loading efficiency; need to increase AlCl appropriately 3 Ratio to improve the efficiency of loading, in this way, after the loading is completed, it is necessary to support the catalyst and solid AlCl 3 Separation; requires extensive solvent wash-out of AlCl after immobilization 3 And distill unreacted AlCl under high vacuum under high temperature conditions (>180°C) 3
This not only causes AlCl 3 The waste of raw materials pollutes the environment, and increases the difficulty of post-processing, which will seriously corrode equipment, so it is difficult to industrialize production

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The preparation of gamma-alumina supported aluminum trichloride catalyst comprises the following steps:

[0037] (1) Impregnating the γ-alumina carrier

[0038] The spherical gamma-alumina carrier is immersed in 0.5M sodium carbonate solution for 6 hours, dried in vacuum and then calcined at 600°C for 6 hours; the operation in this step should be carried out under the protection of argon.

[0039] (2) Immobilize aluminum trichloride in solution

[0040] Under argon protection, 7.5g of anhydrous aluminum trichloride was made into a solution in 150ml of toluene, then added to 15g of activated alumina carrier, kept at reflux temperature for 12 hours, filtered, and the organic solvent was removed. The catalyst was washed with toluene and dried in vacuum to obtain an aluminum trichloride supported catalyst.

[0041] The aluminum trichloride supported catalyst prepared in embodiment 1 is carried out the mensuration of chlorine content with Volhard titration method, and the ...

Embodiment 2

[0045] The preparation of gamma-alumina supported aluminum trichloride catalyst comprises the following steps:

[0046] (1) Impregnating the γ-alumina carrier

[0047] The spherical gamma-alumina carrier is soaked in 1.0M sodium carbonate solution for 6 hours, vacuum-dried and then calcined at 200°C for 12 hours; the operation in this step should be carried out under the protection of argon.

[0048] (2) Immobilize aluminum trichloride in solution

[0049] Under the protection of argon, make a solution of 2g of anhydrous aluminum trichloride in 150ml of toluene, then add it to 15g of activated alumina carrier, keep it at reflux temperature for 36 hours, filter, remove the organic solvent, and the catalyst Wash with toluene and dry in vacuum to obtain aluminum trichloride supported catalyst.

[0050] The aluminum trichloride supported catalyst prepared in embodiment 2 is carried out the mensuration of chlorine content with Volhard titration method, and the chlorine content th...

Embodiment 3

[0054] The preparation of gamma-alumina supported aluminum trichloride catalyst comprises the following steps:

[0055] (1) The immersion treatment of the gamma-alumina carrier is the same as in Example 1, the difference is that the treatment condition of the carrier is carried out at room temperature, and the spherical gamma-alumina carrier is immersed in a 2.0M sodium carbonate solution for 2 hours, After vacuum drying, high-temperature calcination was carried out at 600° C. for 10 hours.

[0056] (2) Immobilize aluminum trichloride in solution

[0057] Under argon protection, 7.5g of anhydrous aluminum trichloride was made into a solution in 150ml of toluene, then added to 15g of activated alumina carrier, maintained at reflux temperature for 12 hours, removed solvent, washed with toluene, Vacuum drying to obtain aluminum trichloride supported catalyst.

[0058] Carry out the mensuration of chlorine content to the aluminum trichloride supported catalyst prepared in embodi...

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Abstract

The invention discloses a preparation method and a new application of a gamma-alumina-supported aluminum trichloride catalyst. The preparation method includes: (1) impregnating the gamma-alumina carrier: placing the gamma-alumina carrier in a weak alkaline solution impregnation, then vacuum drying, and then high-temperature roasting; (2) Immobilize aluminum trichloride in solution: make a solution of anhydrous aluminum trichloride in toluene, then add activated alumina carrier, and keep at reflux temperature After a certain period of time, the organic solvent is removed by filtration, washed with toluene, and vacuum-dried to obtain the target product with a chlorine content of 6.04-17.9ω%. The prepared gamma-alumina supported aluminum trichloride catalyst can be used to catalyze 1-decene oligomerization to prepare 1-decene oligomer. The conversion rate of 1-decene is ≥60ω%. The invention adopts toluene as a solvent, improves the solubility of aluminum trichloride, has high immobilization reaction efficiency, realizes clean loading, reduces the treatment of three wastes, and is convenient for industrialized production.

Description

technical field [0001] The present invention relates to a kind of gamma-alumina (Al 2 o 3 ) supported aluminum trichloride (AlCl 3 ) clean preparation method of the catalyst, and the application of the supported aluminum trichloride catalyst in catalyzing the oligomerization of 1-decene. Background technique [0002] Aluminum trichloride (AlCl 3 ) catalyst is one of the important catalysts widely used in chemical industry, petroleum refining and pharmaceutical industry. Due to its good catalytic effect, it has the characteristics of high polymer yield, narrow molecular weight distribution and good selectivity in catalyzing α-olefin oligomerization. However, AlCl 3 While the catalyst has extremely high activity, it also has obvious shortcomings: ①It is highly corrosive, and it is easy to damage the reactor and other devices, which affects the service life of the device; ②The use of AlCl 3 A large amount of sewage will be generated during the polymerization of the cataly...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J27/125C07C2/22C07C11/02C10G50/02
CPCY02P20/52
Inventor 米普科许胜邢秋菊张志高熊玉洁米怡璇何阳许鹄飞吴志祥陈建任迎春
Owner EAST CHINA UNIV OF SCI & TECH