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Preparation method of high-selectivity methane halogenation oxidation catalyst

A methane halide oxidation, high selectivity technology, applied in the direction of physical/chemical process catalysts, preparation of halogenated hydrocarbons, chemical instruments and methods, etc., can solve the problems of low yield of methyl halides, reduction of selectivity of methyl halides, etc.

Active Publication Date: 2018-05-25
FUSHUN RES INST OF PETROLEUM & PETROCHEMICALS SINOPEC CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] The methane halogen oxidation reaction in the prior art has the following technical problems. High temperature is beneficial to improve the conversion rate of methane, but it will cause deep oxidation of the generated methyl halides, especially monohalomethanes, to generate CO or CO 2 , which significantly reduces the selectivity of methyl halides, resulting in low yields of methyl halides. Therefore, it is of great significance to develop a catalyst for the methane halooxidation reaction with high methane conversion and selectivity of methyl halides.

Method used

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  • Preparation method of high-selectivity methane halogenation oxidation catalyst

Examples

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Effect test

Embodiment 1

[0028] Preparation of modified alumina: using equal volume impregnation method on alumina (commercially available, the properties are as follows: specific surface 335m 2 / g, pore volume is 0.86ml / g) impregnated with sucrose aqueous solution, the mass concentration of sucrose aqueous solution is 5%, the pH value is 2, the aging temperature is 80℃, the aging time is 2h, the drying temperature after aging is 150℃, the drying time 24h, roasting at 300°C for 3 hours;

[0029] Preparation of zinc-loaded alumina: impregnating zinc nitrate solution on the modified alumina by equal volume impregnation, drying and roasting after impregnation, the drying time is 2 hours, and the drying temperature is 130°C; the roasting time is 4 hours, the temperature 400°C, the zinc-loaded alumina is spherical, and the equivalent diameter of the zinc-loaded alumina is 2 mm;

[0030] Prepare aluminum hydroxide slurry by hydrolysis of aluminum isopropoxide: mix water and aluminum isopropoxide at a molar...

Embodiment 2

[0035] Preparation of modified alumina: using equal volume impregnation method on alumina (commercially available, the properties are as follows: specific surface 335m 2 / g, pore volume is 0.86ml / g), dipped in glucose aqueous solution, the weight concentration of glucose aqueous solution is 20%, the preferred pH value is 3, the aging temperature is 60°C, the aging time is 5h, and the drying temperature after aging is 100°C for 8h. , roasting at 450°C for 3 hours;

[0036] Preparation of zinc-loaded alumina: impregnate the modified alumina with a zinc sulfate solution using an equal-volume impregnation method, dry and roast after impregnation, the drying time is 3 hours, and the drying temperature is 120 ° C; the roasting time is 5 hours, the temperature is 450°C, the zinc-loaded alumina is spherical, and the equivalent diameter of the zinc-loaded alumina is 2mm;

[0037] Prepare aluminum hydroxide slurry by hydrolysis of aluminum isopropoxide: mix water and aluminum isopropox...

Embodiment 3

[0042] Preparation of modified alumina: using equal volume impregnation method on alumina (commercially available, the properties are as follows: specific surface 335m 2 / g, the pore volume is 0.86ml / g), the fructose aqueous solution is impregnated, the weight concentration of the fructose aqueous solution is 10%, the pH value is 1, the aging temperature is 70°C, the aging time is 3.5h, and the drying temperature after aging is 110°C Dry for 15h. Roasting at 380°C for 4 hours;

[0043]Preparation of zinc-loaded alumina: impregnating zinc bromide solution on the modified alumina by an equal volume impregnation method, drying and roasting after impregnation, the drying time is 4 hours, and the drying temperature is 100 ° C; the roasting time is 4 hours, The temperature is 500°C, the zinc-loaded alumina is spherical, and the equivalent diameter of the zinc-loaded alumina is 3mm;

[0044] Prepare aluminum hydroxide slurry by hydrolysis of aluminum isopropoxide: mix water and alu...

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Abstract

The invention discloses a preparation method of a high-selectivity methane halogenation oxidation catalyst. The preparation method comprises following steps: (1), aluminum oxide is impregnated by an acid solution of sugar and then subjected to aging, drying and roasting treatment, and modified aluminum oxide is obtained; (2), zinc is supported to modified aluminum oxide prepared in the step (1), and after drying and roasting, zinc supported aluminum oxide is prepared; (3), zirconium sulfate solid acid and aluminum hydroxide slurry are mixed, and aluminum hydroxide slurry containing zirconium sulfate solid acid is obtained; (4), zinc supported aluminum oxide is subjected to spray soaking by the aluminum hydroxide slurry containing zirconium sulfate solid acid and prepared in the step (3), and after drying and roasting, the methane halogenation oxidation catalyst is prepared. According to the catalyst prepared with the method, conversion rate of methane and selectivity of a target product methyl halide can be increased simultaneously, deep oxidation of methyl halide is inhibited, and yield of methyl halide is obviously increased.

Description

technical field [0001] The invention relates to a preparation method of a high-selectivity methane halogen oxidation catalyst, in particular to a preparation method of a low-temperature high-selectivity methane halogen oxidation catalyst. Background technique [0002] Methane does not directly react with halogen, but uses HCl, HBr or metal halide as a halogen source, and the process of reacting with the participation of oxygen to form halide is called halogen oxidation reaction. This method was first applied to the industrial production of chlorine by catalytic oxidation of HCl, known as the Deacon process. [0003] The early methane halogen oxidation reaction mainly used HCl as the halogen source, and the catalyst mainly used CuCl 2 As the active component, Bromhead et al. (Bromhead J, Font-Freide J J, Westlake D J. Process for the production of methyl or ethyl mono-chloride or bromide. EP. Patent, 0117731.1984-09-05) loaded CuCl on alumina 2 An oxychlorination catalyst i...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/053B01J35/02C07C17/154C07C19/075B01J35/00
CPCC07C17/154B01J27/053B01J35/396B01J35/50C07C19/075
Inventor 李杰张信伟尹泽群刘全杰倪向前
Owner FUSHUN RES INST OF PETROLEUM & PETROCHEMICALS SINOPEC CORP
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