Supported nickel catalyst for synthesizing chlora aniline by hydrogenation of chloronitrobenzene and its preparation method thereof

A technology for chlorinated nitrobenzene and chlorinated aniline is applied in the field of catalysts for synthesizing chlorinated aniline by liquid-phase hydrogenation of chlorinated nitrobenzene, and can solve the problems of high catalytic activity of noble metal catalysts, serious side reactions, and high cost, and achieves Excellent reaction performance, low dechlorination performance, low cost effect

Inactive Publication Date: 2006-04-26
TIANJIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Noble metal catalysts have high catalytic activity, good selectivity, and mild reaction conditions, but their disadvantages are high cost
Although the Raney nickel catalyst has the advantage of lower price, its side reaction of hydrodechlorination is relatively serious, and it is necessary to use a toxic co-catalyst to improve the selectivity of the product; meanwhile, the Raney nickel catalyst is in the process of preparation and use. Contamination and safety concerns remain

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0013] The titanium dioxide was dried at 110°C for 4 hours, immersed in an aqueous nickel nitrate solution at 30°C for 4 hours using an equal volume immersion method, then dried at 110°C for 4 hours, and then calcined in an air atmosphere at 400°C for 2 hours. Then, the catalyst precursor was reduced with hydrogen at 400° C. for 2 hours to obtain a catalyst with a nickel content of 10%, which was added to the ethanol solution in which o-chloronitrobenzene was dissolved under the protection of nitrogen. Under the conditions of 80℃, hydrogen pressure 1.0MPa, catalyst dosage 500mg, 5g m-dinitrobenzene dissolved in 100ml ethanol, after 60 minutes of reaction, the conversion rate of o-chloronitrobenzene is 99.9%, and the selectivity of o-chloroaniline is 99.1%.

Embodiment 2

[0015] The catalyst preparation process and catalytic hydrogenation reaction conditions are the same as in Example 1, except that zirconia is used as the catalyst carrier. After 200 minutes of reaction, the conversion of o-chloronitrobenzene was 99.5%, and the selectivity of o-chloroaniline was 98.1%.

Embodiment 3

[0017] The catalyst preparation process and catalytic hydrogenation reaction conditions are the same as in Example 1, except that silica is used as the catalyst carrier. After 600 minutes of reaction, the conversion of o-chloronitrobenzene was 80.5%, and the selectivity of o-chloroaniline was 96.6%.

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PUM

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Abstract

The invention relates to a carrier nickel-base catalyst used to hydrogenate the chloronitrobenzene to synthesize chloroaniline, which comprises silicon dioxide, titania or zirconia as carrier, wherein 10~40% nickel. The preparation process comprises: drying, dipping, calcining, reducing, and activating. The advantages of this invention include: low cost, simple process, little pollution, and well reaction performance.

Description

Technical field [0001] The invention relates to a supported nickel catalyst for liquid phase hydrogenation of chloronitrobenzene to synthesize chloroaniline and a preparation method thereof, belonging to the catalyst technology for liquid phase hydrogenation of chloronitrobenzene to synthesize chloroaniline. Background technique [0002] Chloroaniline is an important organic intermediate, which is widely used in the synthesis of fine chemical products such as pharmaceuticals, dyes, and pigments. For example, o-chloroaniline can be applied to dye bases, as the diazo component of azo dyes and as intermediates for the manufacture of pharmaceuticals and pesticides. [0003] At present, the industry mainly uses iron powder reduction, alkali sulfide or hydrazine hydrate reduction, sulfonated ammonolysis and liquid phase catalytic hydrogenation to synthesize chloroaniline from nitrochlorobenzene. Among them, the reduction reaction route using iron powder, alkali sulfide or hydrazine hyd...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J32/00C07C209/36C07C211/52
Inventor 陈吉祥熊峻张继炎
Owner TIANJIN UNIV
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