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Preparation method of high-activity methane halogen oxidation catalyst

A methane halogen oxidation and catalyst technology, which is applied in the field of preparation of highly active methane halogen oxidation catalysts, can solve problems such as low yield of methyl halides and reduced selectivity of methyl halides

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

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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-activity methane halogen 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, the pore volume is 0.86ml / g) impregnated with gallium nitrate and nickel nitrate aqueous solution, the molar concentration of gallium ions in the solution is 1 mol / L, and the molar concentration of nickel metal ions is 0.5 mol / L, after impregnation, it is dried and roasted. The drying time is 1h, and the drying temperature is 100°C; the calcination time is 2h, and the temperature is 900°C;

[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 2mm;

[0030] Prepare aluminum hydr...

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) impregnated with gallium nitrate and nickel nitrate aqueous solution, the molar concentration of gallium ions in the solution is 3mol / L, and the molar concentration of nickel metal ions is 1.5mol / L, after impregnation, it is dried and roasted. The drying time is 2h, and the drying temperature is 100°C; the roasting time is 8h, and the temperature is 700°C;

[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...

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, pore volume is 0.86ml / g) impregnated gallium nitrate, nickel nitrate aqueous solution, the molar concentration of gallium ion in the solution is 2mol / L, the molar concentration of nickel metal ion is 1mol / L, after impregnating, carry out drying, roasting, described The drying time is 0.5h, and the drying temperature is 130°C; the calcination time is 5h, and the temperature is 800°C;

[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 aluminu...

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Abstract

The invention discloses a preparation method of a high-activity methane halogen oxidation catalyst. The preparation method comprises following steps: (1), aluminum oxide is subjected to co-impregnation by a mixed solution containing gallium and nickel and then is dried and subjected to high-temperature roasting treatment, and modified aluminum oxide is obtained; (2), zinc is supported to modifiedaluminum 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 sulfatesolid acid and prepared in the step (3), and after drying and roasting, the methane halogen 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-activity methane halogen oxidation catalyst, in particular to a preparation method of a low-temperature high-activity 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 is prep...

Claims

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Application Information

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IPC IPC(8): B01J27/053C07C17/154C07C19/03
CPCB01J27/053C07C17/154C07C19/03
Inventor 张信伟李杰尹泽群刘全杰倪向前
Owner FUSHUN RES INST OF PETROLEUM & PETROCHEMICALS SINOPEC CORP
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