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Catalyst for hydrogenation production of aniline or derivatives thereof by nitrobenzene or derivatives thereof, and preparation method and application thereof

A technology of derivatives and catalysts, which is applied in the field of catalysts, preparation methods and applications for the hydrogenation of nitrobenzene or its derivatives to produce aniline or its derivatives, can solve the problems of complicated separation process and poor selectivity of target products, and achieve Low equipment investment, good application prospects and practical value, high activity and selectivity

Inactive Publication Date: 2017-07-04
SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the selectivity of the target product is poor, and the subsequent separation process is complicated

Method used

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  • Catalyst for hydrogenation production of aniline or derivatives thereof by nitrobenzene or derivatives thereof, and preparation method and application thereof
  • Catalyst for hydrogenation production of aniline or derivatives thereof by nitrobenzene or derivatives thereof, and preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0037]Take 0.086g of nickel nitrate, 0.522g of ammonium heptamolybdate, add 5g of ammonia water, heat the mixed solution to 80°C, add ionic water to make the solution volume 16.271ml, and obtain a mixed solution with a total solution concentration of 0.2mol / L, and use 0.5mol / L nitric acid to adjust the pH to 8.0. Add 9.5g of alumina for impregnation for 2 hours, and stir continuously at a rate of 30 rpm during the impregnation process to make the impregnation uniform. After 2 hours, the sample was filtered out and dried. During drying, the temperature was slowly raised from room temperature to 100°C at a rate of 10°C / min, and dried at this temperature for 24h. The resulting dried samples were calcined at 400 °C for 12 h. The obtained roasted sample was put into a fixed-bed reactor for vulcanization, the hydrogen pressure was 0.5 MPa, the vulcanizing agent was dimethyl disulfide, the dosage was 0.293 g, the carrier oil was cyclohexane, and the sulfur content was 1000 ppm. Ra...

Embodiment 2

[0040] Get 6.522g ferric nitrate nonahydrate, 2.850g ammonium heptamolybdate, add 20g ammoniacal liquor, the mixed solution is heated to 50 ℃, add ionized water to make the solution volume be 9.224ml, obtain the total solution concentration and be 3.5mol / L mixed solution, use 0.5mol / L hydrochloric acid to adjust the pH value to 13.0. Add 6.0g of alumina for impregnation for 24 hours, and stir continuously at a rate of 300 rpm during the impregnation process to make the impregnation uniform. After 24 hours, the sample was filtered out and dried. During drying, the temperature was slowly raised from room temperature to 100°C at a rate of 10°C / min, and dried at this temperature for 6 hours. The obtained samples were calcined at 600°C for 3h. The obtained sample was put into a fixed bed reactor for vulcanization, the hydrogen pressure was 3.0MPa, the vulcanizing agent was dimethyl disulfide, the dosage was about 2.281g, the carrier oil was n-hexane, and the sulfur content was abo...

Embodiment 3

[0043] Take 1.354g of copper nitrate, 2.550g of ammonium heptamolybdate, add 9g of ammonia water, heat the mixed solution to 60°C, add ionic water to make the solution volume 12.036ml, and obtain a mixed solution with a total solution concentration of 1.8mmol / L, and use 0.5mol / L ethylenediamine to adjust the pH to 12.0. Add 7.0g of alumina for impregnation for 16 hours, and stir continuously at a rate of 150 rpm during the impregnation process to make the impregnation uniform. After 18 hours, the sample was filtered out and dried. During drying, the temperature was slowly raised from room temperature to 120°C at a rate of 15°C / min, and dried at this temperature for 10h. The obtained samples were calcined at 500°C for 8h. The obtained sample was put into a fixed-bed reactor for vulcanization, the hydrogen pressure was 2.0 MPa, the vulcanizing agent was dimethyl disulfide, the dosage was about 1.700 g, the carrier oil was cyclohexane, and the sulfur content was about 3000 ppm....

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Abstract

A catalyst for hydrogenation production of aniline or derivatives thereof by nitrobenzene or derivatives thereof is in a sulfide state and has the composition represented by Mx-Mo-Sy / Al2O3, wherein M is Fe, Ni, Cu, Co, W or a combination thereof, x is 0.1-1, and y is 1-4. The mass percentage content of the Mx-Mo-Sy in the catalyst is 5%-40%. The catalyst has the advantages of high conversion rate, good selectivity, low cost and mild reaction conditions.

Description

technical field [0001] The invention belongs to a catalyst for producing aniline or its derivatives by hydrogenation of nitrobenzene or its derivatives, a preparation method and application. Background technique [0002] Aromatic amine compounds are intermediates in the production of important chemical products such as medicines, dyes, stabilizers, fungicides, insecticides, herbicides, developers, antioxidants and petroleum additives. At present, the main production methods include electrolytic reduction of nitrobenzene derivatives, catalytic hydrogenation, reduction of iron powder, and biological fermentation. Due to the high technical difficulty, strict production control requirements and high power consumption, the electrolytic reduction method of nitrobenzene derivatives has not yet achieved industrialization in my country; the biological fermentation process is relatively green and environmentally friendly, but the production time is long, the efficiency needs to be imp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/051C07B43/04C07C209/36C07C211/45C07C211/46C07C211/52C07C227/06C07C229/56C07C221/00C07C223/06C07C303/22C07C309/46C07C213/02C07C215/76C07C217/84C07C253/30C07C255/58C07C319/12C07C323/34
CPCB01J27/0515B01J27/051C07B43/04C07C209/36C07C213/02C07C221/00C07C227/06C07C253/30C07C303/22C07C319/12C07C211/45C07C211/46C07C211/52C07C229/56C07C223/06C07C309/46C07C215/76C07C217/84C07C255/58C07C323/34
Inventor 李学宽韩文鹏葛晖唐明兴杜明仙周立公杨英
Owner SHANXI INST OF COAL CHEM CHINESE ACAD OF SCI
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