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Rh3Ni1 catalyst and method for preparing arylamine by carrying out catalytic reduction on nitro aromatic hydrocarbon through Rh3Ni1 catalyst

A technology of nitroaromatics and catalysts, applied in the field of heterogeneous catalysis, can solve problems such as complex structures, and achieve the effects of simple preparation procedures, high catalyst activity and selectivity, and mild reaction conditions

Inactive Publication Date: 2013-03-13
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Although bimetallic Rh 32 Fe 28 Nanoparticles exhibit higher activity than monometallic Rh, however, in order to stabilize bimetallic nanoparticles, complex dendrimer carriers need to be added

Method used

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  • Rh3Ni1 catalyst and method for preparing arylamine by carrying out catalytic reduction on nitro aromatic hydrocarbon through Rh3Ni1 catalyst
  • Rh3Ni1 catalyst and method for preparing arylamine by carrying out catalytic reduction on nitro aromatic hydrocarbon through Rh3Ni1 catalyst
  • Rh3Ni1 catalyst and method for preparing arylamine by carrying out catalytic reduction on nitro aromatic hydrocarbon through Rh3Ni1 catalyst

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Experimental program
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Effect test

Embodiment 2

[0041]Implementation method: heat octadecylamine to form a clear solution as solvent, surfactant and reducing agent. Continue heating to 140 DEG C, then add trihydrate rhodium trichloride and nickel acetylacetonate, wherein the mass molar concentration of trihydrate rhodium trichloride is 0.045mmol / g, and the mass molar concentration of nickel acetylacetonate is 0.015mmol / g, A clear liquid was obtained. In the state of vigorous stirring, inject the above-mentioned clear liquid into octadecylamine that has been warmed up to 240°C in advance for dilution, and the mass molar concentration of rhodium trichloride trihydrate is 0.012mmol / g, and the mass molar concentration of nickel acetylacetonate is 0.012mmol / g. A solution with a molar concentration of 0.004mmol / g. Aging the above solution for 3 minutes at 240°C, cooling to 70°C, adding ethanol to precipitate a precipitate, washing with ethanol after centrifugation to obtain bimetallic Rh 3 Ni 1 , wherein the particle size of t...

Embodiment 3

[0043] Implementation method: heat octadecylamine to form a clear solution as solvent, surfactant and reducing agent. Continue heating to 150 DEG C, then add trihydrate rhodium trichloride and nickel acetylacetonate, wherein the mass molar concentration of trihydrate rhodium trichloride is 0.075mmol / g, and the mass molar concentration of nickel acetylacetonate is 0.025mmol / g, A clear liquid was obtained. In the state of vigorous stirring, inject the above-mentioned clear liquid into octadecylamine that has been warmed up to 250°C in advance for dilution, and the mass molar concentration of rhodium trichloride trihydrate is 0.015mmol / g, and the mass molar concentration of nickel acetylacetonate is 0.015mmol / g. A solution with a molar concentration of 0.005mmol / g. Aging the above solution at 250°C for 5 minutes, cooling to 80°C, adding ethanol, precipitated precipitate, washing with ethanol after centrifugation to obtain bimetallic Rh 3 Ni 1 , where the particle size of the s...

Embodiment 4

[0045] Implementation method: at room temperature, mix nitrobenzene and Rh 3 Ni 1 Place in ethyl acetate, wherein the molar concentration of the substrate is 0.05mol / L, and the molar concentration of the catalyst is 0.00015mol / L. After sealing the reactor, add a balloon filled with hydrogen, and continuously change the air for 3 times. Under the state of stirring, react the mixture at room temperature for 8 hours, recover the catalyst by centrifugation, and distill the supernatant to remove the solvent under reduced pressure to obtain aniline. The yield 99%.

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Abstract

The invention relates to a Rh3Ni1 catalyst and a method for preparing arylamine by carrying out catalytic reduction on nitro aromatic hydrocarbon through the Rh3Ni1 catalyst, and belongs to the technical field of heterogeneous catalysis. The method for preparing the arylamine by carrying out the catalytic reduction on the nitro aromatic hydrocarbon through the Rh3Ni1 catalyst comprises the following steps of putting the nitro aromatic hydrocarbon as a substrate and bimetal Rh3Ni1 as a catalyst in an organic solvent to react in the atmosphere of room-temperature constant-pressure hydrogen to selectively reduce the nitro aromatic hydrocarbon so as to prepare the arylamine, wherein the utilized bimetal Rh3Ni1 is bimetal Rh3Ni1 nano alloy prepared in octadecylamine by taking rhodium chloride trihydrate and nickel acetylacetonate as precursors. The method disclosed by the invention has the advantages that a preparation process of the catalyst is simple, the reaction condition is mild (room temperature and constant pressure), the activity and selectivity of the catalyst are high and the like.

Description

technical field [0001] The present invention relates to bimetallic Rh 3 Ni 1 The preparation and the method for preparing aromatic amines by catalytically reducing nitroaromatics belong to the technical field of heterogeneous catalysis. Background technique [0002] Functionalized aniline is an important intermediate in the synthesis of chemicals such as drugs, polymer materials and dyes. At present, people mainly prepare aniline by reducing nitroaromatics, such as using a stoichiometric reducing agent, using metal complex catalysis or hydrogen transfer hydrogenation or catalytic hydrogenation. Among them, the catalytic hydrogenation method has outstanding advantages in terms of environmental friendliness and atomic utilization. However, industrial catalytic hydrogenation processes are usually carried out under high temperature and pressure. In addition to high energy consumption, for the reduction of polysubstituted nitroaromatics with other reducible groups (such as hal...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07B43/04C07C209/36C07C211/46C07C211/58C07C211/47C07C221/00C07C223/06C07C211/51C07C213/02C07C215/68C07C225/22C07C211/52C07C211/50C07C217/84C07C227/04C07C229/60B01J23/89
CPCY02P20/584
Inventor 蔡双飞何伟李亚栋段昊泓戎宏盼王定胜李林森
Owner TSINGHUA UNIV
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