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Catalyst for preparing o-toluidine by hydrogenating o-nitrotoluene and preparation method of catalyst

A technology for o-nitrotoluene and o-toluidine is applied in the field of catalytic hydrogenation of o-nitrotoluene to prepare o-toluidine catalyst and the field of preparation thereof, and can solve the problems of easy crushing selectivity, poor thermal stability, low temperature and the like

Active Publication Date: 2021-03-23
CHINA PETROLEUM & CHEM CORP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0012] The purpose of the present invention is to overcome the disadvantages of poor thermal stability, easy carbon deposition, easy crushing and low selectivity of traditional copper-silica gel catalysts, and provide a kind of o-nitrate catalyst with good thermal stability, difficult carbon deposition, high strength and high selectivity. Catalyst for Preparation of o-Toluidine by Catalytic Hydrogenation of Methyltoluene

Method used

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  • Catalyst for preparing o-toluidine by hydrogenating o-nitrotoluene and preparation method of catalyst
  • Catalyst for preparing o-toluidine by hydrogenating o-nitrotoluene and preparation method of catalyst

Examples

Experimental program
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Effect test

Embodiment 1

[0035] (1) Weigh 100g of raw silica gel and wash it with deionized water, put it into a reactor equipped with 200ml of deionized water, control the temperature of the reactor at 130°C, and the reaction pressure at 0.35MPa, and add concentrated nitric acid to adjust the solution under stirring conditions The acidity, adjust the concentration of nitric acid solution to 3%, the treatment time is 2h, and then wash with deionized water until the pH value of the washing solution is 7.0; (2) Weigh 100g copper nitrate and dissolve it in 180ml deionized water, the pH value of the solution is 5 , adding ammonia water with a specific gravity of 0.985 to the copper nitrate solution, controlling the pH value of the solution to be 10, forming a molecular formula of [Cu(NH 3 ) 4 ] 2+ copper ammonia complex, the copper content in the complex is 30g / l; (3) Add the copper ammonia complex obtained in step (2) into the dipping kettle, and add the modified silica gel obtained in step (1) Among t...

Embodiment 2

[0037](1) Weigh 100g of raw silica gel and wash it with deionized water, put it into a reactor equipped with 200ml of deionized water, control the temperature of the reactor at 140°C, and the reaction pressure at 0.25MPa, and add concentrated nitric acid to adjust the solution under stirring conditions The acidity, adjust the concentration of nitric acid solution to 4%, the treatment time is 2.5h, and then wash with deionized water until the pH value of the washing solution is 7.0; (2) Weigh 100g of copper nitrate and dissolve it in 180ml of deionized water, the pH of the solution is 4. Add ammonia water with a specific gravity of 0.985 to the copper nitrate solution, control the pH value of the solution to 9, and form a molecular formula of [Cu(NH 3 ) 4 ] 2+ copper ammonia complex, the copper content in the complex is 32g / l; (3) Add the copper ammonia complex obtained in step (2) into the dipping kettle, and add the modified silica gel obtained in step (1) Among them, at a ...

Embodiment 3

[0039] (1) Weigh 100g of raw silica gel and wash it with deionized water, put it into a reactor equipped with 200ml of deionized water, control the temperature of the reactor at 135°C, and the reaction pressure at 0.3MPa, and add concentrated nitric acid to adjust the solution under stirring conditions The acidity, adjust the concentration of nitric acid solution to 4%, the treatment time is 3h, and then wash with deionized water until the pH value of the washing solution is 7.0; (2) Weigh 100g copper nitrate and dissolve it in 180ml deionized water, the pH value of the solution is 6 , adding ammonia water with a specific gravity of 0.984 to the copper nitrate solution, controlling the pH of the solution to be 11, forming a molecular formula of [Cu(NH 3 ) 4 ] 2+ copper ammonia complex, the copper content in the complex is 35g / l; (3) Add the copper ammonia complex obtained in step (2) into the dipping kettle, and add the modified silica gel obtained in step (1) Among them, at...

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Abstract

The invention relates to a catalyst for preparing o-toluidine through catalytic hydrogenation of o-nitrotoluene and a preparation method of the catalyst. The catalyst takes metal Cu as an active component and takes modified SiO2 as a carrier. The active component Cu accounts for 15%-25% of the weight of the catalyst. In the preparation process of the catalyst, silica gel is pretreated, so that theprepared catalyst is regular in appearance, high in strength and not easy to crush. The active component copper is impregnated on silica gel in the form of a copper-ammonia complex in an alkaline atmosphere to form a Cu-Si coalition structure, thereby enhancing the thermal stability and carbon deposition resistance of the catalyst, and increasing the one-way service cycle of the catalyst to 8 hours or above. According to the method disclosed by the invention, the pore structure of the catalyst is improved, the proportion of the pore size of 2-15nm reaches more than 80%, the active component is highly dispersed on the carrier, and the conversion rate and selectivity of the catalyst reach more than 99.9%.

Description

technical field [0001] The invention belongs to the technical field of catalysts, and in particular relates to a catalyst for preparing o-toluidine by catalytic hydrogenation of o-nitrotoluene and a preparation method thereof. Background technique [0002] O-toluidine is mainly used as an intermediate in dyes, pesticides, medicines and organic synthesis. One of the preparation methods is the aniline methylation method: in the presence of ferric oxide-germanium dioxide catalyst, toluene and methanol react to form a toluidine mixture. Wherein the selectivity of o-toluidine is more than 40%, and o-toluidine is obtained by separation. The other is the reduction of o-nitrotoluene: iron powder can be used as a reducing agent, and o-toluidine can be obtained by hydrogenation reaction at 260-280°C in the presence of a copper catalyst. Nickel catalysts can also be used. According to different manufacturing methods, the product contains m-toluidine, p-toluidine, nitrotoluene and oth...

Claims

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Application Information

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IPC IPC(8): B01J23/72C07C209/36C07C211/47
CPCB01J23/72C07C209/36B01J35/647C07C211/47Y02P20/584
Inventor 李兴田王金利刘超李忠于黄伟冯明黄霞
Owner CHINA PETROLEUM & CHEM CORP
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