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Nitrogen-doped activated carbon supported noble metal catalyst and application thereof

A precious metal catalyst, activated carbon technology, applied in metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, organic chemistry, etc., can solve the problems of high preparation cost, waste gas generation, low yield, etc. The effect of low catalyst dosage, lower use cost and high metal utilization rate

Active Publication Date: 2017-12-01
ZHEJIANG UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

But it is also obvious that this method has high energy consumption, low yield, high preparation cost, and the process is often accompanied by waste gas generation

Method used

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  • Nitrogen-doped activated carbon supported noble metal catalyst and application thereof
  • Nitrogen-doped activated carbon supported noble metal catalyst and application thereof
  • Nitrogen-doped activated carbon supported noble metal catalyst and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0048] Activated carbon physical parameters and treatment: the ash content is 6.0wt%, the specific surface area is 500m 2 / g, 150-1000 mesh activated carbon, made of coconut shell. Each gram of the activated carbon was soaked and boiled in 5ml of 0.1mol / L hydrochloric acid for 1h, then treated with 3.5ml of concentrated nitric acid (10%), stirred at 35°C for 1h, and dried for later use.

[0049] Dissolve 0.08g of dicyandiamide in 40mL of water at 75°C, add 0.56g of activated carbon into the nitrogen source solution under stirring (at this time, the mass ratio of nitrogen to activated carbon is 0.1:1), and ultrasonically treat for 10 minutes, during which the temperature is 75 ℃, keep the temperature and continue mechanical stirring for 1h. Transfer the obtained slurry to a hydrothermal kettle, fill it with air and seal it under normal pressure, heat-treat it at 80°C for 2 hours, and after cooling to room temperature, wash the obtained nitrogen-containing activated carbon slur...

Embodiment 2

[0052] The physical parameters and treatment of the carrier activated carbon: the ash content is 1.0wt%, and the specific surface area is 1500m 2 / g, 200-800 mesh activated carbon, made of coconut shell. Each gram of the activated carbon was soaked and boiled in 10ml of 1.0mol / L hydrochloric acid for 1h, then treated with 15ml of concentrated nitric acid (10%), stirred at 35°C for 1h, and dried for later use.

[0053] Dissolve 0.34g of dicyandiamide in 40mL of water at 95°C, and add 0.238g of activated carbon into the nitrogen source solution under stirring. 75°C, keep the temperature and continue mechanical stirring for 10h. Transfer the obtained slurry to a hydrothermal kettle, fill it with air and seal it under normal pressure, heat-treat it at 120°C for 10 hours, and after cooling to room temperature, wash the obtained nitrogen-containing activated carbon slurry with a 50% volume fraction of ethanol-water mixture until pH=7~ 8. Dry in vacuum (-0.05Mpa) at 80°C for 10h. ...

Embodiment 3

[0056] The physical parameters and treatment of the carrier activated carbon: the ash content is 3.0wt%, and the specific surface area is 1500m 2 / g, 200-800 mesh activated carbon, made of coconut shell. Each gram of the activated carbon was soaked and boiled in 10ml of 3.0mol / L hydrochloric acid for 4h, then treated with 15ml of hydrogen peroxide (15wt%), stirred at 35°C for 15h, and dried for later use.

[0057] Dissolve 0.67g of dicyandiamide in 40mL of water at 95°C, add 0.45g of activated carbon into the nitrogen source solution, at this time, the mass ratio of nitrogen to activated carbon is 1:1, and ultrasonically treat for 20min at a temperature of 75°C, then The temperature was raised to 95°C, and the temperature was maintained to continue mechanical stirring for 24h. Transfer the obtained slurry to a hydrothermal kettle, fill it with nitrogen and seal it under normal pressure, heat-treat at 180°C for 12 hours, and after cooling to room temperature, wash the obtained...

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Abstract

The invention discloses a nitrogen-doped activated carbon supported noble metal catalyst and an application thereof. The catalyst is composed of a carrier and an active component; the carrier is nitrogen-doped activated carbon; the active component is one of palladium, platinum, rhodium, ruthenium and iridium; and the load of the active component is not higher than 15wt% based on the mass of the carrier. The invention provides the application of the nitrogen-doped activated carbon supported noble metal catalyst to reaction for preparing an alkyl-containing halogenated aromatic aminocompound shown as a formula (II) by carrying out catalytic hydrogenation reduction on an alkyl-containing halogenated aromatic nitrocompound shown as a formula (I) to show that the nitrogen-doped activated carbon supported noble metal catalyst has the characteristics of high hydrogenation reaction rate, high catalytic activity, high selectivity and high stability.

Description

(1) Technical field [0001] The invention relates to a nitrogen-doped activated carbon-supported noble metal catalyst and its preparation method and application. This type of catalyst is suitable for the catalytic hydrogenation reduction reaction of halogenated aromatic nitro compounds, especially for halogenated aromatic nitro compounds containing alkyl groups. The compound catalyzes the hydrogenation reduction reaction. (2) Technical background [0002] The process of reducing nitro groups to amino groups is widely used in the fields of medicine, pesticides, dyes, rubber additives and photosensitive materials. The traditional reduction method is the chemical reduction method, which mostly uses sodium sulfide or iron powder to reduce nitro groups in an acidic environment. This type of process is easy to operate, has a small risk factor, and requires low investment in equipment, so it has become the most commonly used nitro reduction method. However, the disadvantages of th...

Claims

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Application Information

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IPC IPC(8): B01J23/42B01J23/44B01J23/46B01J27/24C07C209/36C07C211/52
CPCB01J23/42B01J23/44B01J23/464B01J27/24C07C209/36C07C211/52
Inventor 卢春山齐亚妮冯振龙王梦君马磊张群峰丰枫李小年
Owner ZHEJIANG UNIV OF TECH
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