Nanocrystalline metal-loaded titanium carbide catalyst and method for preparing chloro aniline with nanocrystalline metal-loaded titanium carbide catalyst in reduction mode

A nano metal, titanium carbide technology, applied in physical/chemical process catalysts, catalyst carriers, preparation of amino compounds, etc., can solve the problems of long reaction time and high reaction temperature, achieve simple preparation method, reduce catalytic reaction conditions, and wide source. Effect

Inactive Publication Date: 2014-09-10
CHINA WEST NORMAL UNIVERSITY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The reaction temperature is highe

Method used

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preparation example Construction

[0033] The preparation method of titanium carbide supported nanometer metal catalyst comprises the steps:

[0034] a. Preparation of catalyst carrier

[0035]adding titanium aluminum carbon into the hydrofluoric acid aqueous solution, so that the aluminum in the titanium aluminum carbon is completely dissolved in the hydrofluoric acid aqueous solution, filtering to obtain a black precipitate, washing the black precipitate, and drying in vacuum to obtain a catalyst carrier;

[0036] b. Preparation of catalyst

[0037] Put the catalyst carrier into water, and then add the active metal elements that need to be loaded. The active metal elements are added in the form of metal compounds, and then reduced until the loaded metal is zero-valent. After the reduction is completed, continue to stir to disperse the metal elements evenly. Filter out, wash the precipitate, and vacuum-dry to obtain a titanium carbide-supported nano-metal catalyst;

[0038] The active metal element is one or...

Embodiment 1

[0062] The preparation of embodiment 1 catalyst and adopt this catalyst reduction to obtain chloroaniline

[0063] Add 25g of titanium aluminum carbon to 1000mL concentrated hydrofluoric acid aqueous solution, the concentration of hydrofluoric acid aqueous solution is 40wt%, stir at room temperature for 12h, the stirring speed is 600rpm, the reaction solution is centrifuged to obtain a black precipitate, and the black precipitate is mixed with water and Washed three times with ethanol, and dried in vacuum at 60oC for 12h to obtain the carrier titanium carbide.

[0064] Weigh 5 g of the dried carrier titanium carbide and add it to 200 mL of water, add 50 mL of chloroplatinic acid aqueous solution containing 150 mg of platinum, and then dropwise add 450 mg of NaBH 4 50mL of the aqueous solution was reduced until no bubbles were generated. After the reduction was completed, the mixture was stirred for 24 hours, filtered out, washed three times with water and ethanol, and vacuum-d...

Embodiment 2

[0067] The preparation of embodiment 2 catalyst and adopting this catalyst reduction obtains chlorinated aniline

[0068] Add 0.5 g of the carrier titanium carbide prepared in Example 1 into 20 mL of water, add 5 mL of chloroplatinic acid aqueous solution containing 15 mg of platinum, then add 30 mL of isopropanol for reflux reduction for 8 h, continue stirring for 24 h after the reduction, and filter out. Wash with water and ethanol three times respectively, and dry in vacuum at 60°C for 12 hours to obtain a platinum catalyst supported on titanium carbide;

[0069] Transfer 50mg of catalyst, 1.57g of 4-chloronitrobenzene, 70mL of mixed solvent of water and methanol (volume ratio of water and methanol: 2:5) into a 250mL two-neck bottle, and feed hydrogen at a reaction temperature of 25oC and a hydrogen pressure of 1atm React for 1h, stir during the reaction, and the stirring speed is 1200rpm, and the chloroaniline is obtained after the reaction is completed;

[0070] The reac...

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Abstract

The invention relates to a nanocrystalline metal-loaded titanium carbide catalyst and a method for preparing chloro aniline with the nanocrystalline metal-loaded titanium carbide catalyst in a reduction mode, and belongs to the field of organic synthesis and catalytic reactions. The nanocrystalline metal-loaded titanium carbide catalyst is prepared in the modes that lamellar titanium carbide serves as a catalyst carrier, and then reactive metal elements are loaded on the titanium carbide. The reactive metal elements comprise one or two of ruthenium, rhodium, platinum, palladium and iridium. The nanocrystalline metal-loaded titanium carbide catalyst prepared with the method is used for reduction of chloronitrobenzene, and the chloro aniline is obtained. The titanium carbide used as the carrier in the catalyst is prepared from titanium aluminum carbons, sources are wide, the cost is low, and the preparation method is easy and convenient. The nanocrystalline metal-loaded titanium carbide catalyst has the high activity and the high selection for chloronitrobenzene hydrogenation, and reaction conditions for preparing the chloro aniline in the reduction mode are mild.

Description

technical field [0001] The invention relates to a titanium carbide-loaded nanometer metal catalyst and a method for preparing chloroaniline through reduction thereof, belonging to the field of organic synthesis and catalytic reaction. Background technique [0002] Chloroaniline, the reduction product of chloronitrobenzene, has high application value and is an important raw material for the preparation of dyes, medicines, pesticides, insecticides, and herbicides. The industrial production methods of chloroaniline mainly include Fe-HCl reduction system with iron powder as reducing agent and metal catalyst catalytic hydrogenation system. Among them, the Fe-HCl reduction system produces a large amount of waste such as iron sludge (Fe 3 o 4 ) and other by-products, the follow-up treatment is complicated and the environmental pollution is serious. Therefore, this production process has been eliminated by many countries. The catalytic hydrogenation preparation method has the ch...

Claims

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Application Information

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IPC IPC(8): B01J27/22B01J32/00C07C209/36C07C211/52
Inventor 樊光银
Owner CHINA WEST NORMAL UNIVERSITY
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