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Catalyst for synthesizing parachloroaniline by parachloronitrobenzene through hydrogenation and preparation method thereof

A technology of p-chloronitrobenzene and p-chloroaniline, applied in the preparation of amino compounds, chemical instruments and methods, metal/metal oxide/metal hydroxide catalysts, etc., can solve the problem of low catalytic activity and achieve high activity , to achieve selectivity, to inhibit the effect of dechlorination reaction

Inactive Publication Date: 2010-06-23
LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Ruthenium catalysts exhibit high selectivity but low catalytic activity

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0012] (1) Acidification treatment of attapulgite

[0013] Put the attapulgite into a round bottom flask, add 2-10wt% sulfuric acid solution, reflux at 25-110°C for 1-10 hours, filter, wash with water until the pH is neutral, and then dry at 80-120°C for 8-12 hours .

[0014] (2) Preparation of attapulgite-supported platinum catalyst

[0015] Weigh 0.5g of acid-treated attapulgite and 0.086g of polyvinylpyrrolidone into a 25ml round bottom flask, then add 10ml of 0.008M H 2 PtCl 6 ·6H 2 The aqueous solution of O was stirred evenly at room temperature, and then dried to obtain the catalyst precursor. The obtained catalyst precursor was placed in a tubular heating furnace, reduced under hydrogen at 300° C. for 4 hours, filtered, washed with water, and dried to obtain the catalyst. XRF indicated that the platinum content in the catalyst was 2.8 wt%.

[0016] The prepared catalyst is used in the selective hydrogenation reaction of p-chloronitrobenzene in a 100ml electromagne...

Embodiment 2

[0019] (1) Acidification treatment of attapulgite

[0020] Put the attapulgite into a round bottom flask, add 2-10wt% hydrochloric acid solution, reflux at 25-110°C for 1-10 hours, filter, wash with water until the pH is neutral, and then dry at 80-120°C for 8-12 hours .

[0021] (2) The preparation process of attapulgite supported platinum catalyst is the same as in Example 1

[0022] Under the reaction conditions of 40°C, hydrogen pressure 2.0MPa, 5mg catalyst, 0.5g p-chloronitrobenzene, and 8ml methanol, after 10 minutes of reaction, the conversion rate of p-chloronitrobenzene was 70%, and the selectivity of p-chloroaniline was 94.8%. .

Embodiment 3

[0024] The preparation process of the catalyst is the same as in Example 1, except for the content of platinum. XRF shows that the content of platinum in the catalyst is 1.1%.

[0025] Under the reaction conditions of 40°C, hydrogen pressure 2.0MPa, 5mg catalyst, 0.5g p-chloronitrobenzene, and 8ml methanol, after 10 minutes of reaction, the conversion rate of p-chloronitrobenzene is 50%, and the selectivity of p-chloroaniline is 89%. .

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PUM

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Abstract

The invention discloses a catalyst for synthesizing parachloroaniline by parachloronitrobenzene through hydrogenation and a preparation method thereof. The active component of the catalyst is Pt, the carrier is attapulgite, and the content of the Pt is 0.1-5wt%. The catalyst not only has high activity, but also effectively inhibits the generation of a dechlorination reaction. Under the condition that the parachloronitrobenzene is completely transformed, the selectivity of 100% for the parachloroaniline is realized.

Description

technical field [0001] The invention relates to a catalyst for synthesizing p-chloroaniline by hydrogenation of p-chloronitrobenzene and a preparation method thereof. Background technique [0002] 4-Chloroaniline is an important industrial intermediate, widely used in the synthesis of fine chemicals such as dyes, pesticides, and pharmaceuticals. It is generally produced by reduction of p-chloronitrobenzene. Traditional preparation methods such as reduction of iron powder, alkali sulfide and hydrazine hydrate have problems such as impact on the environment and high production costs. At present, the catalytic hydrogenation reduction method has attracted more and more attention due to its advantages of atom economy and environmental friendliness. However, in the process of catalytic hydrogenation of p-chloronitrobenzene, there is a competitive reaction between nitro hydrogenation and C-Cl bond hydrogenolysis, so how to effectively inhibit the occurrence of dechlorination react...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/42C07C211/52C07C209/36
Inventor 徐贤伦王芳刘俊华
Owner LANZHOU INST OF CHEM PHYSICS CHINESE ACAD OF SCI
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