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Support catalysts for p-chloronitrobenzene selective hydrogenation and preparation method thereof

A supported catalyst, the technology of p-chloronitrobenzene, which is applied in the preparation of amino compounds, metal/metal oxide/metal hydroxide catalysts, chemical instruments and methods, etc., can solve the problem of high selectivity and high strength and easy recovery of precious metals and other problems, to achieve the effect of suitable for industrial production, simple operation and mild process conditions

Inactive Publication Date: 2009-01-14
NANKAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0033] The technical problem to be solved by the present invention is to provide a supported catalyst for synthesizing p-chloroaniline by catalytic hydrogenation of p-chloronitrobenzene and its preparation method, which overcomes the problem of being composed of p-chloronitrobenzene, ethanol and a hydrogenation catalyst. In the reaction system, the shortcomings of high activity, high selectivity, high strength, high stability, easy separation process and easy recovery of precious metals cannot be taken into account in order to obtain higher p-chloroaniline selectivity and improve p-chloro Yield and cost reduction of p-chloroaniline by catalytic hydrogenation of nitrobenzene

Method used

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  • Support catalysts for p-chloronitrobenzene selective hydrogenation and preparation method thereof
  • Support catalysts for p-chloronitrobenzene selective hydrogenation and preparation method thereof
  • Support catalysts for p-chloronitrobenzene selective hydrogenation and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0053] The preparation of supported catalyst, the steps are as follows:

[0054] 1) Place the nano-flaky pseudo-boehmite AlO(OH) used as a carrier in a muffle furnace for 1-6 hours at 200-750°C, and set aside;

[0055] 2) Weigh 0.5 g of the calcined nano-flaky pseudo-boehmite AlO(OH) carrier, and use deionized water to measure the volume of the impregnation solution required for equal-volume impregnation to be 20 mL;

[0056] 3) Weigh 0.07g of the catalyst matrix main agent RuCl according to the specified weight ratio 3 .3H 2 O, dissolved in 20mL of water, made into impregnation solution;

[0057] 4) Weigh 0.5 g of the roasted nano-flaky pseudo-boehmite AlO(OH) carrier, and impregnate it with 20 mL of the above impregnation solution for 4 to 25 hours in a constant temperature water bath at 20°C;

[0058] 5) Place the impregnated catalyst in a three-necked bottle, using KBH 4 As a reducing agent, it was reduced under the protection of argon at 35°C, and the temperature was ...

Embodiment 2

[0062] Weigh the catalyst precursor main agent RuCl 3 .3H 2 O, dissolved in 20mL of ethanol aqueous solution with a concentration of 20% to 80% by mass to make an impregnating solution. Others are the same as in Example 1, and the supported catalyst Ru / nano-flaky pseudo-boehmite AlO(OH) can be obtained.

Embodiment 3

[0064] Weigh the catalyst precursor main agent RuCl 3 .3H 2 O, dissolved in 20mL ethanol solution, made into impregnation solution. Others are the same as in Example 1, and the supported catalyst Ru / nano-flaky pseudo-boehmite AlO(OH) can be obtained.

[0065] Table 1

[0066]

[0067] The following conclusions can be drawn from Table 1: the Ru / nano-flaky pseudo-boehmite AlO(OH) prepared in aqueous solution and ethanol aqueous solution has a higher yield.

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Abstract

The invention relates to a method to prepare a load catalyst of parachloroaniline used to prepare parachloronitrobenzene hydrogenation and an application method thereof. During preparation of the catalyst, AlO(OH), r-Al<2>O<3>, SiO<2> and SBA-15 are used as carriers respectively to compare the performances of Ru catalyst after loading different carriers. Because the AlO(OH) has excellent dispersing performance in water, Ru nano particles are dispersed evenly, during the reaction for preparing parachloroaniline by using parachloronitrobenzene hydrogenation, excellent catalytic activity is achieved. The temperature and the solvent are changed during the process of catalyst preparation, and ultrasonic assistance is introduced to optimize the method of catalyst preparation. The catalyst has high activity, high selectivity, and has the advantages of that the stability is high, the separation technique is easy and the precious metal is easy to reclaim; the method is applicable to the reaction for preparing parachloroaniline by using parachloronitrobenzene hydrogenation, and excellent hydrogenation activity and selectivity are achieved during the reaction.

Description

technical field [0001] The technical scheme of the present invention designs a metal-containing catalyst, specifically a supported catalyst for selective hydrogenation of p-chloronitrobenzene and a preparation method thereof. Background technique [0002] Introduction to the reaction of p-chloronitrobenzene hydrogenation to p-chloroaniline: [0003] p-Chloroaniline is an important fine chemical product and organic intermediate, widely used in synthetic rubber, chemical reagents, dyes, pigments, medicines, pesticides, etc. The annual constant quantity of our country is measured in hundreds of thousands of tons, and the output value is several billion. p-Chloroaniline is generally produced by reduction of p-Chloroaniline. The oldest method in industry is to use metal to reduce p-chloronitrobenzene to prepare p-chloroaniline in the presence of a small amount of acid. This method was reported as early as 1854 and is still used as a production process: [0004] (1) Iron powder...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/46C07C211/52C07C209/36
Inventor 李伟邓佳张明慧陶克毅
Owner NANKAI UNIV
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