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Application of a carbon-based catalyst in the catalytic hydrogenation of p-nitrophenol

A technology of nitrophenol catalysis and carbon-based catalysts, which is applied in the direction of catalyst activation/preparation, physical/chemical process catalysts, metal/metal oxide/metal hydroxide catalysts, etc., and can solve problems involving organic reagents or acid-base conditions, The reaction process is complicated and lengthy, and the recycling performance is poor, so as to achieve the effect of abundant raw materials, cheap and easy-to-obtain raw materials, and good catalytic activity

Active Publication Date: 2020-10-23
QINGDAO UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0009] In summary, the preparation method of the catalyst for the catalytic hydrogenation reaction of p-nitrophenol that is widely used at present is mainly to directly load the active components on molecular sieves, activated carbon, diatomaceous earth and other carriers, and the active components are mostly noble metals. The prepared catalysts have high catalytic activity, but they are often easy to agglomerate and have poor recycling performance. The reaction involves organic reagents or acid-base conditions, which put forward higher requirements for the subsequent treatment of the product.
Some studies gradually use non-precious metals instead of precious metals as active components, which reduces the cost, but the reaction process is complicated and lengthy, and a step of activation treatment is often required before use, which increases the reaction process.

Method used

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  • Application of a carbon-based catalyst in the catalytic hydrogenation of p-nitrophenol
  • Application of a carbon-based catalyst in the catalytic hydrogenation of p-nitrophenol
  • Application of a carbon-based catalyst in the catalytic hydrogenation of p-nitrophenol

Examples

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Effect test

Embodiment 1

[0024] Take commercially purchased microcrystalline cellulose (MCC) as raw material, weigh 8g, put it into a polytetrafluoroethylene-lined reaction kettle with a volume of 100ml, and put a certain volume of deionized water as a solvent to ensure that the volume of the solution is compared with the volume of the kettle. 8:10, choose nickel acetate as the nickel source for doping, the mass ratio of nickel acetate to microcrystalline cellulose is 2:10, mix well and put the reaction kettle into a box-type incubator, and raise the temperature to the target temperature of 230°C. After constant temperature for 12 hours, cool down to room temperature, filter to obtain a dark brown solid, wash with deionized water, absolute ethanol, and acetone three times respectively, dry and grind. The nickel-doped carbon-based catalyst precursor obtained above was put into a tubular calciner, and under the protection of nitrogen atmosphere, the temperature was raised to 900°C at 5°C / min and kept at ...

Embodiment 2

[0027] Take commercially purchased microcrystalline cellulose (MCC) as raw material, weigh 5g, put it into a polytetrafluoroethylene-lined reactor with a volume of 100ml, and put a certain volume of deionized water as a solvent to ensure that the volume of the solution is proportional to the volume of the kettle. It is 6:10, choose ferroferric oxide as the iron source of doping, the mass ratio of ferroferric oxide and microcrystalline cellulose is 1:4, after mixing evenly, put the reaction kettle into a box-type incubator, and heat up to the target The temperature is 220°C, keep the temperature for 14 hours, cool down to room temperature, filter to obtain a dark brown solid, wash with deionized water, absolute ethanol, and acetone three times respectively, dry and grind. The iron-doped carbon-based catalyst precursor obtained above was put into a tubular calciner, and under the protection of nitrogen atmosphere, the temperature was raised to 950°C at 5°C / min and kept at a const...

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Abstract

The invention discloses a hydrothermal preparation method of a carbon-based catalyst used for the catalytic hydrogenation of paranitrophenol. The hydrothermal preparation method is characterized in that: taking microcrystalline cellulose as a raw material and different non-noble metal compounds as a doping source, conducting high-temperature high-pressure hydrothermal treatment, filtering to obtain a deep brown solid product, respectively washing with deionized water and absolute ethyl alcohol for a plurality of times to remove an organic matter on the surface of the product, drying, and grinding. An obtained catalyst precursor is put into a tubular calcinatory, and is calcined under the nitrogen atmosphere at the high temperature for a certain period of time to obtain the metal doped carbon-based catalyst with excellent stability. The catalytic efficiency of the carbon-based catalyst on generation of aminophenol through catalytic hydrogenation of the paranitrophenol is explored in a normal-temperature normal-pressure reaction system. The operation process has the main characteristics that: the cellulose, a biomass resource, is utilized, the operation process is environment-friendly and cheap and is easy to get, the catalytic activity of the non-noble metals is neutral, the reaction conditions are mild, an active center and a carbon material are synchronously generated, so that the structure is more stable, the catalytic reaction is conducted under the conditions of normal pressure and normal temperature, and the reaction process is simple to operate.

Description

[0001] Technical field: [0002] The invention relates to the field of preparation of nano catalyst materials, in particular to the application of a carbon-based catalyst in the catalytic hydrogenation reaction of p-nitrophenol. Background technique: [0003] Aminophenol (PAP) is an important fine organic chemical intermediate, commonly used in the preparation of anesthetics, analgesics, antipyretics, and is widely used in the dye industry, preparation of developers, antioxidants and food additives. Generally, three methods are used to prepare PAP: p-nitrophenol (PNP) is prepared by multi-step iron-acid reduction; nitrobenzene is prepared by catalytic hydrogenation in a strong acid system and electrochemical reduction. But these methods usually take a long time, operate under strict conditions, and involve expensive raw materials. The study also pointed out that various nitrophenol mixtures are the most common organic pollutants in industrial and agricultural wastewater. If v...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/745B01J23/75B01J23/755B01J37/08C07C213/02C07C215/76
CPCB01J23/745B01J23/75B01J23/755B01J37/088C07C213/02C07C215/76
Inventor 吴琼于世涛刘仕伟解从霞于海龙
Owner QINGDAO UNIV OF SCI & TECH
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