Method for using parachloronitrobenzene to prepare parachloroaniline through selective hydrogenation

A technology of p-chloronitrobenzene and p-chloroaniline, which is applied in the field of selective hydrogenation of p-chloronitrobenzene to prepare p-chloroaniline, which can solve the problems affecting the overall performance of the catalyst, easy aggregation of platinum nanoparticles, and harsh preparation conditions. Achieve the effects of good selective catalytic hydrogenation effect, superior catalytic activity, and simple preparation method

Active Publication Date: 2018-05-15
XIANGTAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are always some problems in the above-mentioned prior art: as some preparation conditions are harsh in the preparation method, the reagents used are not friendly to the environment, the dispersibility of platinum is not good, and the particle size is relatively large
At present, the common m

Method used

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  • Method for using parachloronitrobenzene to prepare parachloroaniline through selective hydrogenation
  • Method for using parachloronitrobenzene to prepare parachloroaniline through selective hydrogenation
  • Method for using parachloronitrobenzene to prepare parachloroaniline through selective hydrogenation

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Experimental program
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Effect test

Embodiment 1

[0039] The mesoporous silicon material SBA-15 was added to 15 mL of absolute ethanol, and ultrasonically oscillated for 2 hours to obtain a mixture of treated SBA-15 and absolute ethanol. Under the condition of stirring, drop 0.5mL butyl titanate into the above mixture drop by drop, stir for 1h; slowly add 1mL water to the mixture to hydrolyze the butyl titanate, and continue stirring for 1h to completely hydrolyze the butyl titanate . Heat and stir at 40°C to make the above mixture into a gel. Vacuum drying overnight at 80°C to get 10% TiO 2 / SBA-15 composite carrier (TiO in the composite carrier 2 Content is 10wt%). Take 0.702gTiO 2 / SBA-15 composite carrier dispersed in 100mL deionized water, add 10mL anhydrous methanol, ultrasonically disperse for 10min, then add 0.1mL chloroplatinic acid solution, ultrasonically disperse for 20min, and then place the solution under ultraviolet light under stirring conditions After 12 hours, the resulting solution was filtered and was...

Embodiment 2

[0041] With embodiment 1, the difference is that Pt / TiO 2 The mass fraction of Pt in / SBA-15 is 0.08%, that is, 0.08%Pt / 10%TiO 2 / SBA-15.

Embodiment 3

[0043] With embodiment 1, the difference is that Pt / TiO 2 / TiO in SBA-15 2 The mass fraction in the composite support is 15%, that is, 0.1%Pt / 15%TiO 2 / SBA-15.

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Abstract

The invention provides a method for using parachloronitrobenzene to prepare parachloroaniline through selective hydrogenation. The method comprises the steps that a catalyst containing platinum and titanium dioxide to catalyze parachloronitrobenzene to prepare parachloroaniline through selective hydrogenation under a hydrogen environment and a heating condition, and a dechlorinating side reactionsin the hydrogenation process are sharply decreased, wherein the catalyst is Pt/TiO2/SBA-15 catalyst. The catalyst is used for presenting superior catalytic activity in the process of catalyzing parachloronitrobenzene to prepare parachloroaniline through selective hydrogenation, the conversion rate and the selectivity are very high, both can reach 99% or more, and the dechlorinating side reactionsare sharply decreased. The composite nanostructure catalyst Pt/TiO2/SBA-15 used in the method is simple to prepare, short in production cycle, and low in platinum loading capacity, accordingly the catalyst cost is low, high temperature treatment is not needed, and a reduction agent does not need to be added in the preparation process. The platinum dispersity is good, and the catalytic activity ishigh.

Description

technical field [0001] The invention belongs to the field of catalytic hydrogenation, in particular to a method for preparing p-chloroaniline by selective hydrogenation of p-chloronitrobenzene. Background technique [0002] p-Chloroaniline is an important organic intermediate widely used in the synthesis of dyes, medicines and pesticides. At present, most p-chloroanilines are produced by reducing p-chloronitrobenzene. The reduction methods mainly include metal reduction method, electrochemical reduction method, non-hydrogen reducing agent reduction method, catalytic hydrogenation reduction method, etc., among which catalytic hydrogenation The reduction method has advanced technology and high yield, which is more in line with the requirements of modern chemical industry for atom economy; among them, the catalytic hydrogenation method of precious metals occupies the main position. In the past, the heterogeneous catalytic reduction method under high temperature and pressure was...

Claims

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Application Information

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IPC IPC(8): B01J29/03C07C209/36C07C211/52
CPCB01J29/0325B01J2229/186C07C209/365C07C211/52
Inventor 周继承王非张燕吉
Owner XIANGTAN UNIV
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