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Rhenium catalyst and method for catalyzed synthesis of 2-methyl-1,4-naphthoquinone by rhenium catalyst

A catalyst and methyl technology, applied in the field of rhenium catalyst and its catalytic synthesis of 2-methyl-1,4-naphthoquinone, can solve the problems of environmental pollution, large amount of catalyst, low reaction efficiency, etc., and achieve high activity and preparation Simple method and good stability

Active Publication Date: 2017-05-10
NANJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Aiming at the existing problems of large catalyst consumption, low reaction efficiency and serious environmental pollution, the invention provides a kind of environment-friendly oxidation preparation of 2-methylnaphthalene with mild reaction conditions, high reaction yield, low catalyst consumption, and A New Method of -1,4-Naphthoquinone

Method used

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  • Rhenium catalyst and method for catalyzed synthesis of 2-methyl-1,4-naphthoquinone by rhenium catalyst
  • Rhenium catalyst and method for catalyzed synthesis of 2-methyl-1,4-naphthoquinone by rhenium catalyst
  • Rhenium catalyst and method for catalyzed synthesis of 2-methyl-1,4-naphthoquinone by rhenium catalyst

Examples

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Effect test

Embodiment example 1

[0019] Measure the perrhenic acid solution containing 0.0100g metal rhenium in a round bottom flask, dilute it with 20ml methanol as a solvent, then add 1.0000g activated carbon to the solution, and stir at room temperature for 4h. Move the round bottom flask to an oil bath at 50°C, and add 0.1576mg of 1-methyl-3-cyanomethylimidazolium chloride into the round bottom flask, and continue stirring at this temperature for 12h. 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 600°C. The heating rate was 5°C / min, and the temperature was maintained for 2h. Catalyst A1 (rhenium loading 1%) was obtained after natural cooling to room temperature.

Embodiment example 2

[0021] Measure the perrhenic acid solution containing 0.0100g metal rhenium in a round bottom flask, dilute it with 20ml methanol as a solvent, then add 1.0000g activated carbon to the solution, and stir at room temperature for 4h. Move the round bottom flask to an oil bath at 50°C, and add 0.1576mg of 1-methyl-3-cyanomethylimidazolium chloride into the round bottom flask, and continue stirring at this temperature for 12h. After the stirring, the round-bottomed flask was placed on a rotary evaporator to dry the solvent, 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 700°C. The heating rate was 5°C / min, and the temperature was maintained for 2h. Catalyst A2 (rhenium loading 1%) was obtained after natural cooling to room temperature.

Embodiment example 3

[0023] Measure the perrhenic acid solution containing 0.0100g metal rhenium in a round bottom flask, dilute it with 20ml methanol as a solvent, then add 1.0000g activated carbon to the solution, and stir at room temperature for 4h. Move the round bottom flask to an oil bath at 50°C, and add 0.1576mg of 1-methyl-3-cyanomethylimidazolium chloride into the round bottom flask, and continue stirring at this temperature for 12h. 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 800°C. The heating rate was 5°C / min, and the temperature was maintained for 2h. After naturally cooling down to room temperature, catalyst A3 (rhenium loading was 1%) was obtained.

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Abstract

The invention relates to a rhenium catalyst and a method for catalyzed synthesis of 2-methyl-1,4-naphthoquinone by the rhenium catalyst. The rhenium catalyst is characterized in that a rhenium compound is supported on activated carbon and is coated with a carbon-nitride material; then the rhenium compound is calcined in the atmosphere of inert gas to obtain a coated supported rhenium catalyst, wherein the supporting mass of rhenium accounts for 1 to 3 percent of total mass of the catalyst. The method for the catalyzed synthesis of the 2-methyl-1,4-naphthoquinone by the rhenium catalyst comprises the following specific steps: adding 2-methylnaphthalene, an oxidizing agent and a catalyst into an organic solvent; controlling the reaction temperature and the time to obtain a product, namely the 2-methyl-1,4-naphthoquinone. The catalyst is simple in preparation method, good in stability and suitable for industrial production; in addition, the rhenium catalyst shows good activity and selectivity for the reaction and is easy to recycle and reutilize.

Description

technical field [0001] The invention relates to a rhenium catalyst and a method for catalytically synthesizing 2-methyl-1,4-naphthoquinone, in particular to an activated carbon-supported rhenium metal nanocatalyst coated with a carbon-nitrogen material and catalytic oxidation synthesis of 2-methyl-1,4-naphthoquinone. 1,4-Naphthoquinone. Background technique [0002] 2-methyl-1,4-naphthoquinone (2-MNQ for short) is the earliest used vitamin K3, and it is also an important intermediate for the synthesis of various vitamin K. The compound has anticoagulant effect and can effectively activate anticoagulant factors in organisms; it can also be used as an additive to promote the growth and development of livestock; it is also the most important fat-soluble antioxidant in biological systems, which can promote high-energy compounds in the human body Metabolism, at the same time has the effect of diuresis, enhance liver detoxification function. [0003] There are many preparation m...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J23/36C07C46/02C07C50/10
CPCC07C46/02B01J23/36B01J27/24C07C50/10Y02P20/584
Inventor 黄军祁正亮
Owner NANJING UNIV OF TECH
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