Preparation method of hydrogenation catalyst for nitrobenzene and derivatives thereof

A hydrogenation catalyst and nitrobenzene technology, which is applied in the direction of amino compound preparation, physical/chemical process catalyst, metal/metal oxide/metal hydroxide catalyst, etc., can solve the complicated preparation process, large particle size, and easy agglomeration Problems such as growth, to achieve the effect of low equipment requirements, improved load capacity, and excellent performance

Inactive Publication Date: 2019-04-19
DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Publication number [CN201210366356.8] discloses a method for highly selective hydrogenation of halogenated anilines using supported noble metals treated with sulfides at 30-70°C as catalysts and halogenated nitrobenzenes as raw materials. The prepared catalyst can effectively inhibit the side reaction of hydrodehalogenation, and the selectivity of the product is high; however, the limited and high cost of precious metal resources and the high specific surface energy of metal nanoparticles are easy to agglomerate and grow when heated, res

Method used

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  • Preparation method of hydrogenation catalyst for nitrobenzene and derivatives thereof
  • Preparation method of hydrogenation catalyst for nitrobenzene and derivatives thereof
  • Preparation method of hydrogenation catalyst for nitrobenzene and derivatives thereof

Examples

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Effect test

Embodiment 1

[0029] 1) Preparation of functional carbon materials

[0030] Disperse 100 mg of sodium polystyrene sulfonate in a sodium chloride solution with a volume of 500 ml and a mass fraction of 1 wt%, and sonicate for 10 minutes; disperse 100 mg of carbon nanotubes in the above solution and sonicate for 2 hours at 30 ℃; filter and dry Obtain functionalized carbon materials;

[0031] 2) Preparation of precious metal nanoparticles

[0032] Add 10ml of an aqueous solution containing 20.60mg of chloroauric acid to 41.2mg of polyvinylpyrrolidone with a molecular weight of 8000, mix and stir for 1 hour at a stirring speed of 1000rpm, then add 103.0mg of sodium borohydride to reduce for 2 hours to obtain nano-Au particle catalyst;

[0033] 3) Support precious metal nanoparticles

[0034] Disperse 49mg of functionalized carbon material in 10ml of ethanol solution, sonicate for 0.5h, then drop 5ml of ethanol solution containing 1mg of nano Au particles, mix and stir for 6h, functionalized carbon mater...

Embodiment 2

[0037] 1) Preparation of functional carbon materials

[0038] Disperse 50 mg of polydiallyl dimethyl ammonium chloride in a sodium chloride solution with a volume of 500 ml and a mass fraction of 5 wt%, and sonicate for 10 minutes; disperse 100 mg of carbon nanotubes in the above solution and perform ultrasonic treatment at 30°C 2h; suction filtration and drying to obtain functionalized carbon material;

[0039] 2) Preparation of precious metal nanoparticles

[0040] Add 10ml of an aqueous solution containing 20.60mg of chloroauric acid to 20.6mg of polyvinylpyrrolidone with a molecular weight of 10000, mix and stir for 1 hour at a stirring speed of 1000rpm, and then add 164.8mg of sodium borohydride to reduce for 4 hours to obtain nano-Au particle catalyst;

[0041] 3) Support precious metal nanoparticles

[0042] Disperse 95mg of functionalized carbon material in 20ml of ethanol solution, sonicate for 0.5h, drop 10ml of ethanol solution containing 5mg nano Au particles, mix and stir ...

Embodiment 3

[0045] 1) Preparation of functional carbon materials

[0046] Disperse 100 mg of sodium polystyrene sulfonate in a sodium chloride solution with a volume of 500 ml and a mass fraction of 2 wt%, and sonicate for 10 minutes; disperse 50 mg of carbon nanotubes in the above solution and sonicate for 2 hours at 50°C; filter and dry Obtain functionalized carbon materials;

[0047] 2) Preparation of precious metal nanoparticles

[0048] Add 10ml of an aqueous solution containing 20.60mg of chloroauric acid to 41.2mg of polyvinylpyrrolidone with a molecular weight of 8000 and mix and stir for 1h at a stirring speed of 1000rpm, then add 103.0mg of ascorbic acid to reduce for 2h to obtain nano-Au particle catalyst;

[0049] 3) Support precious metal nanoparticles

[0050] Disperse 92mg functionalized carbon material in 10ml ethanol solution, sonicate for 0.5h, drop 10ml ethanol solution containing 8mg nano Au particles, mix and stir for 10h, functionalized carbon material supports precious metal...

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Abstract

The invention relates to a preparation method of a hydrogenation catalyst for nitrobenzene and its derivatives. A carbon material is functionally modified with a high-molecular polymer and then loadedwith noble metal. The preparation method of the catalyst comprises the following steps: (1) the carbon material and the high-molecular polymer undergo ultrasonic treatment on in a certain concentration of a salt solution at a certain temperature for 0.5 to 6 hour to obtain a functionalized carbon material; (2) noble metal particles with a certain size distribution are prepared from the salt solution of the noble metal under the action of a protective agent and a reducing agent; (3) the aqueous solution or the organic solution of the obtained noble metal particles undergoes ultrasonic treatment for 10 min and is stirred for 2-12 h and then loaded on the functional group modified carbon material so as to obtain a noble metal-loaded catalyst. The preparation method of the catalyst is simple,effective and green and environmentally-friendly. After reduction by the reducing agent, the uniformly-dispersed noble metal-loaded catalyst with a certain size distribution is obtained. In addition,the catalyst has a broad application prospect in the field of catalysis of nitrobenzene and its derivatives.

Description

technical field [0001] The invention belongs to the technical field of organic synthesis, and relates to a preparation method of a hydrogenation catalyst for nitrobenzene and its derivatives. Background technique [0002] As an organic intermediate, nitroaniline compounds are widely used in the production of dyes, medicines, pesticides, rubber additives and fine chemical intermediates. For example, o-nitroaniline is mainly used as a dye intermediate, the determination of trace iodide, the production of the pesticide carbendazim, etc.; 2-amino-5-nitrophenol is used for the production of neutral pink BL, the manufacture of metal complex dyes, Reactive black, leather spray red GL, leather spray black RL, solvent red BL, solvent red KL, etc. At present, nitroaniline compounds are mainly obtained by selective reduction of nitro compounds, including iron powder reduction method, alkali sulfide reduction method and catalytic hydrogenation method. The first two synthetic methods h...

Claims

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Application Information

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IPC IPC(8): B01J31/10B01J31/08B01J23/44B01J23/52C07C209/36C07C211/46
CPCB01J23/44B01J23/52B01J31/08B01J31/10B01J2231/641C07C209/36C07C211/46
Inventor 黄家辉金新新谢妍
Owner DALIAN INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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