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Vanadium catalyst and method utilizing vanadium catalyst to synthesize 2,3,5-trimethylbenzoquinone

A technology of trimethylphenol and catalyst, which is applied in the field of catalyst and its catalytic synthesis of 2,3,5-trimethylbenzoquinone, can solve the problems of low reaction efficiency and large amount of catalyst, and achieve high activity, high activity and Selective, easy to recycle effect

Inactive Publication Date: 2015-03-11
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0004] The purpose of the present invention is to provide a vanadium catalyst for the problems of large catalyst consumption and low reaction efficiency in the prior art; another purpose of the present invention is to provide the preparation method of the above-mentioned catalyst; another purpose of the present invention is to provide Catalyzed method for synthesizing 2,3,5-trimethylbenzoquinone, the reaction conditions are mild, the reaction yield is high, and the amount of catalyst is low, and 2,3,6-trimethylphenol is oxidized to prepare 2,3,5- Trimethylbenzoquinone

Method used

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  • Vanadium catalyst and method utilizing vanadium catalyst to synthesize 2,3,5-trimethylbenzoquinone
  • Vanadium catalyst and method utilizing vanadium catalyst to synthesize 2,3,5-trimethylbenzoquinone
  • Vanadium catalyst and method utilizing vanadium catalyst to synthesize 2,3,5-trimethylbenzoquinone

Examples

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Embodiment example 1

[0015] Weigh 0.1756g of vanadium trichloride in a round bottom flask, dissolve it in 20ml of ethanol as a solvent, add 1.0000g of activated carbon to the solution after dissolution, and stir at room temperature for 4h. Move the round bottom flask to an oil bath at 50°C, add 0.1500g of dicyandiamide to the round bottom flask, and continue stirring at this temperature for 4h. After the stirring, the round-bottomed flask was placed on a rotary evaporator to dry the solvent, and then dried overnight at 40°C in a vacuum oven, and the obtained precatalyst was calcined in a tube furnace under a nitrogen atmosphere until the temperature was 500°C. The heating rate was 4°C / min, and the temperature was maintained for 4h. Catalyst A1 (4.3% vanadium loading) was obtained after natural cooling to room temperature.

Embodiment example 2

[0017] Weigh 0.1287g of ammonium metavanadate in a round-bottomed flask, and dissolve it in an oil bath at 60°C with 20ml of water as a solvent. Add 0.1500g of dicyandiamide to the bottom flask, and continue to stir at this temperature for 3h. After the stirring, the round-bottomed flask was placed on a rotary evaporator to dry the solvent, and then dried overnight at 30°C in a vacuum oven, and the obtained precatalyst was calcined in a nitrogen atmosphere tube furnace until the temperature was 300°C. The heating rate was 4°C / min, and the temperature was maintained for 3h. Catalyst A2 (4.38% vanadium loading) was obtained after natural cooling to room temperature.

Embodiment example 3

[0019] Weigh 0.2947g of vanadyl acetylacetonate into a round bottom flask, dissolve it in 20ml of ethanol as a solvent, add 1.0000g of activated carbon to the solution after dissolution, and stir at room temperature for 5h. Move the round bottom flask to an oil bath at 40°C, add 0.1500g of dicyandiamide to the round bottom flask, and continue stirring at this temperature for 5h. After stirring, the round-bottomed flask was placed on a rotary evaporator to dry the solvent, and then dried overnight at 50°C in a vacuum oven, and the obtained precatalyst was calcined in a tube furnace under a nitrogen atmosphere until the temperature was 400°C. The heating rate was 4°C / min, and the temperature was maintained for 5h. Catalyst A3 (3.9% vanadium loading) was obtained after natural cooling to room temperature.

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Abstract

The invention relates to a vanadium catalyst and a method utilizing the vanadium catalyst to synthesize 2,3,5-trimethylbenzoquionone. The carrier of the catalyst is active carbon, and the active component is metal vanadium, which is coated by a carbon-nitrogen material. The carbon-nitrogen material is formed by calcining a raw material namely dicyandiamide in an inert atmosphere. The preparation method of the catalyst comprises the following steps: dissolving a vanadium compound into a soluble solvent, then impregnating active carbon into the solvent, adding raw materials, drying, and then calcining in an inert atmosphere so as to obtain the catalyst coated by a carbon-nitrogen material. The catalytic synthesis of 2,3,5-trimethylbenzoquinone comprises the following steps: taking 2,3,6-trimethylphoenl as the raw material, adding an organic solvent, the vanadium catalyst, and hydrogen peroxide, and then carrying out reactions at a specific temperature so as to obtain the 2,3,5-trimethylbenzoquinone. The catalyst preparation method has the advantages of simpleness, cheap raw material, and suitability for industrial production. Moreover, the prepared catalyst has a very good activity and selectivity in the catalytic synthesis of 2,3,5-trimethylbenzoquinone, and can be easily recycled.

Description

technical field [0001] The invention relates to a catalyst and a method for catalytically synthesizing 2,3,5-trimethylbenzoquinone; in particular, to a carbon-nitrogen material-coated activated carbon-supported vanadium metal nano-vanadium catalyst and its catalytic synthesis of 2,3, 5-trimethylbenzoquinone method. Background technique [0002] Known catalysts include metal-containing molecular sieves (Ind.Eng.Chem.Res.2014,53,11276-11283), in which copper-containing molecular sieves are used as catalysts to oxidize 2,3,6-trimethylphenol, and the conversion rate is only 70 % and the selectivity of 2,3,5-trimethylbenzoquinone is only about 80%, the oxidation effect of chromium-containing molecular sieve and iron-containing molecular sieve can only reach a conversion rate of about 10%, and this catalyst is not suitable for industrial application. Although multi-metallic catalysts (Catal. Sci. Technol., 2014, 4, 200-207) have a better effect in oxidizing 2,3,6-trimethylphenol,...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J35/00C07C50/02C07C46/06
Inventor 黄军李冰
Owner NANJING UNIV OF TECH
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