Preparation method of catalyst for methane oxyhalogenation

A methane halogen oxidation and catalyst technology, which is applied in the field of preparation of methane halogen oxidation catalysts, can solve problems such as 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

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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 catalyst for methane oxyhalogenation

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] Preparation of modified silicon oxide: use equal volume impregnation method on silicon oxide (commercially available commodity, properties are as follows: specific surface 335m 2 / g, pore volume is 0.86ml / g) impregnated with lanthanum nitrate and nickel nitrate aqueous solution, the molar concentration of lanthanum and nickel metal ions in the solution is 0.5mol / L, after impregnation, dry and roast, the drying time is 1h, dry The temperature is 100°C; the calcination time is 2h, and the temperature is 900°C;

[0029] Preparation of zinc-loaded silicon oxide: impregnating zinc nitrate solution on the modified silicon oxide by equal-volume impregnation method, 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 silicon oxide loaded with zinc is spherical, and the equivalent diameter of silicon oxide loaded with zinc is 2 mm;

[0030] Prepare aluminum hydroxide ...

Embodiment 2

[0035] Preparation of modified silicon oxide: use equal volume impregnation method on silicon oxide (commercially available commodity, properties are as follows: specific surface 335m 2 / g, pore volume is 0.86ml / g) impregnated with lanthanum nitrate and nickel nitrate aqueous solution, the molar concentration of lanthanum and nickel metal ions in the solution is 1.5mol / L, after impregnation, dry and roast, the drying time is 2h, dry The temperature is 100°C; the calcination time is 8h, and the temperature is 700°C;

[0036] Preparation of zinc-loaded silicon oxide: impregnating zinc sulfate solution on the modified silicon oxide by equal-volume impregnation method, drying and roasting after impregnation, the drying time is 3 hours, and the drying temperature is 120 ° C; the roasting time is 5 hours, the temperature 450°C, the zinc-loaded silicon oxide is spherical, and the equivalent diameter of the zinc-loaded silicon oxide is 2mm;

[0037] Prepare aluminum hydroxide slurry ...

Embodiment 3

[0042] Preparation of modified silicon oxide: use equal volume impregnation method on silicon oxide (commercially available commodity, properties are as follows: specific surface 335m 2 / g, pore volume is 0.86ml / g) impregnated with lanthanum nitrate and nickel nitrate aqueous solution, the molar concentration of lanthanum and nickel metal ions in the solution is 1mol / L, after impregnation, dry and roast, the drying time is 0.5h, dry The temperature is 130°C; the calcination time is 5h, and the temperature is 800°C;

[0043]Preparation of zinc-loaded silicon oxide: impregnating zinc bromide solution on the modified silicon oxide by 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 silicon oxide is spherical, and the equivalent diameter of the zinc-loaded silicon oxide is 3mm;

[0044] Prepare aluminum hydroxide slurry ...

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Abstract

The invention discloses a preparation method of a catalyst for methane oxyhalogenation. The method comprises the following steps: (1) silica is impregnated with a lanthanum and nickel mixed liquid, dried and then roasted at a high temperature, and modified silica is prepared; (2) zinc is supported on modified silicon oxide prepared in step (1), drying and roasting are performed, and zinc supportedsilicon oxide is prepared; (3) zirconium sulfate solid acid and aluminium hydroxide slurry are mixed, and aluminium hydroxide slurry containing zirconium sulfate solid acid is obtained; (4) the aluminium hydroxide slurry containing zirconium sulfate solid acid performs spray soaking on zinc supported silicon oxide, and the catalyst for methane oxyhalogenation is prepared after drying and roasting. The catalyst prepared with the method has the advantages that methane conversion rate and selectivity of halomethane as a target product are increased simultaneously, deep oxidation of halomethane is inhibited, and yield of halomethane is increased obviously.

Description

technical field [0001] The invention relates to a preparation method of a methane halogen oxidation catalyst, in particular to a preparation method of a low-temperature, high-activity, selective 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 prepar...

Claims

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Application Information

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Patent Type & Authority Applications(China)
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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