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Bimetal catalyst for preparing m-nitroaniline through hydrogenation of m-dinitrobenzene

A technology of bimetallic catalyst and m-dinitrobenzene, which is applied in the direction of metal/metal oxide/metal hydroxide catalyst, physical/chemical process catalyst, amino compound preparation, etc., can solve the problem of high cost of electrode materials and electrolysis equipment, It is unfavorable for industrialized production, a large amount of iron sludge and other problems, and the method is green and efficient, the method is simple, and the effect of improving catalytic performance is achieved.

Active Publication Date: 2019-11-19
JIANGXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In industry, m-nitroaniline is usually prepared by chemical reduction, that is, reducing agents such as alkali sulfide and iron powder reduce m-dinitrobenzene to m-nitroaniline in acidic medium, but a large amount of iron sludge will be produced during the experiment. cause environmental pollution
The electrode materials and electrolytic equipment used in the electrolytic reduction method in the current research are high in cost, which is not conducive to industrial production

Method used

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  • Bimetal catalyst for preparing m-nitroaniline through hydrogenation of m-dinitrobenzene
  • Bimetal catalyst for preparing m-nitroaniline through hydrogenation of m-dinitrobenzene
  • Bimetal catalyst for preparing m-nitroaniline through hydrogenation of m-dinitrobenzene

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0022] (1) Preparation of Ni / C, Au / C, AuNi / C catalysts

[0023] The preparation method of Ni / C: weigh 0.9000-1.8000g of NiCl 2 ·6H 2 O in a 250ml Erlenmeyer flask, then add 60-100ml of ethylene glycol and 10-40ml of deionized water, and ultrasonically disperse for 10-40 minutes; add the prepared 5-10ml of NaOH solution (or Na 2 CO 3 ), magnetically stirred for 10-20 minutes; weighed 1.2500g of carbon carrier and added it to the Erlenmeyer flask, aged for 4-10h; pipetted 10-40ml of hydrazine hydrate (or sodium borohydride ethylene glycol solution) into the above solution, and magnetically stirred 10 minutes; transfer the solution in the Erlenmeyer flask to the lining of the autoclave, and magnetically stir for 15-24 hours; filter and wash, wash with ethanol and deionized water several times, vacuum dry, grind, and weigh to obtain Ni / C ;

[0024] The preparation method of Au / C: pipette a certain amount of HAuCl 4 Put the solution in a beaker, add 0.3g of carbon carrier, hea...

Embodiment 3

[0031] The 2.5%Au-2%Ni / C catalyst prepared in Example 1 was used to carry out the experiment of preparing m-nitroaniline by selective hydrogenation of m-dinitrobenzene. Weigh 0.05g of 2.5%Au-2%Ni / C catalyst in an autoclave, pipette 10ml of m-dinitrobenzyl alcohol solution, and stir at a reaction temperature of 150°C, a hydrogen pressure of 3MPa, and a rotating speed of 870r / min After reacting under the same conditions for 1 hour, the separated clear liquid was analyzed by gas chromatography. The conversion rate of m-dinitrobenzene was 100%, and the selectivity of m-nitroaniline was 68.16%. The reaction results are shown in attached table 1.

Embodiment 4

[0033] The 0.5%Au-4%Ni / C catalyst prepared in Example 1 was used to carry out the experiment of preparing m-nitroaniline by selective hydrogenation of m-dinitrobenzene. Weigh 0.05g of 0.5%Au-4%Ni / C catalyst in an autoclave, pipette 10ml of m-dinitrobenzyl alcohol solution, and stir at a reaction temperature of 150°C, a hydrogen pressure of 3MPa, and a rotating speed of 870r / min After reacting under the conditions for 1 h, the separated clear liquid was analyzed by gas chromatography. The conversion rate of m-dinitrobenzene was 100%, and the selectivity of m-nitroaniline was 92.00%. The reaction results are shown in attached table 1.

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Abstract

The invention discloses a bimetal catalyst for preparing m-nitroaniline through hydrogenation of m-dinitrobenzene, wherein a carbon-based material is used as a carrier, and supports Au-transition metal to prepare the catalyst, the catalyst is recorded as Au-M / C, M is one selected from Ni, Cu, Co and Fe, the Au loading amount is 0.1-8%, and the M content is 0.1-15%. According to the present invention, the synergistic effect between the Au and the transition metal in the bimetal catalyst is provided so as to improve the catalytic performance of the catalyst and the selectivity of the product, the catalyst can be recycled so as to reduce the cost, and the preparation method is simple, environmentally friendly and efficient.

Description

technical field [0001] The invention relates to the technical field of preparing m-nitroaniline, in particular to a bimetallic catalyst for preparing m-nitroaniline by hydrogenating m-dinitrobenzene. Background technique [0002] m-Nitroaniline is also an important organic raw material, which is widely used in the organic synthesis industry. Its main uses are: for organic synthesis and pine color inspection. It can be used in detection techniques such as ICP-AES, AAS, AFS, ICP-MS, and ion chromatography, and can also be used as a standard sample in titration analysis. It can be used as a dye intermediate, such as used to synthesize ice dyes, and can be used as an intermediate in organic synthesis such as pesticides, medicines, and color developing agents. [0003] In industry, m-nitroaniline is usually prepared by chemical reduction, that is, reducing agents such as alkali sulfide and iron powder reduce m-dinitrobenzene to m-nitroaniline in acidic medium, but a large amount...

Claims

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Application Information

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IPC IPC(8): B01J23/89B01J23/755B01J23/52C07C211/52C07C209/36
CPCB01J23/892B01J23/755B01J23/52C07C209/365C07C211/52Y02P20/584
Inventor 朱丽华阮露娜张欢裴安荣梦珂
Owner JIANGXI UNIV OF SCI & TECH
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