Catalyst, preparation method and application for hydrogenation synthesis of p-aminophenol

A technology of p-aminophenol and its synthesis method, which is applied in the field of catalysts and its preparation, can solve the problems of no magnetism, lower utilization rate of ferric oxide, and no further improvement of catalytic activity, so as to improve conversion rate and selectivity and facilitate popularization And industrial application, easy to collect and recycle effect

Active Publication Date: 2022-04-19
NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the silica shell does not completely wrap the magnetic core, so after high temperature treatment, the particles become very large, which greatly reduces the utilization rate of ferroferric oxide.
Moreover, there is no strong interaction interface between noble metals and oxides, which does not further improve the catalytic activity
[0004] The patent with the publication number CN107952466A discloses a gold-supported h-BN catalyst, the synthesis method is simple, and the catalytic process is easy to operate, but it is not magnetic, and recovery is somewhat difficult

Method used

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  • Catalyst, preparation method and application for hydrogenation synthesis of p-aminophenol
  • Catalyst, preparation method and application for hydrogenation synthesis of p-aminophenol
  • Catalyst, preparation method and application for hydrogenation synthesis of p-aminophenol

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preparation example Construction

[0030] One aspect of an embodiment of the present invention further provides a method for preparing a catalyst for hydrogenation to synthesize p-aminophenol reactions, comprising:

[0031] (1) The precursor of the precious metal is added to the first oil phase containing the first surfactant, the reaction is carried out, and then the alcohol solvent is added, the precipitate is obtained and centrifuged, and then the mixture of alcohol solvent and alkane is used to wash at least once to obtain the precious metal particles, and the obtained precious metal particles are dispersed in the alkane solution to form a first mixing system;

[0032] (2) The first mixed system is added to the second oil phase containing a first surfactant and a magnetic oxide precursor, into an inert gas, and then reacts, and then add an alcohol solvent and chloroform for washing, centrifugation, to obtain precious metals - magnetic oxide particles, the obtained precious metals - magnetic oxide particles disp...

Embodiment 1

[0072] The steps of the preparation process of a catalyst involved in the present embodiment are as follows:

[0073] (1) Preparation of precious metal particles:

[0074] 40mg of chloroauric acid was added to 10g octadecyne containing 12mg of oleic acid, 12mg of oleamine two surfactants, magnetically stirred, reacted at 110 °C for 0.5h, and then added 10g of hexanol to obtain a precipitate and centrifuged, and then washed several times with a mixture of 10g hexanol and 10g hexane. Finally, disperse the pellet in 10 g of hexane (denoted as: solution A) for later use.

[0075] (2) Preparation of dumbbell-shaped nuclei of "precious metals -magnetic oxides":

[0076] The above (1) of the "solution A" is added containing 12mg of oleic acid, 12mg of oleamine two surfactants and 1.5g of iron oleate of 10g octadecyne, first through the inert gas, for a period of time hexane and other impurities are blown out. It is then heated to 230 °C. Keep the reaction time 1h, reduce to room temperat...

Embodiment 2

[0086] (1) Preparation of precious metal particles:

[0087] 200mg of chloroauric acid was added to 10g of octadecylene containing 100mg of oleic acid, 100mg of oleamine surfactants, magnetically stirred, reacted at 130 °C for 2.5h, and then added 40g of hexanol to obtain a precipitate and centrifuged, and then washed multiple times with a mixture of 20g hexanol and 10g hexane. Finally, disperse the pellet in 10 g of hexane (denoted as: solution A) for later use.

[0088] (2) Preparation of dumbbell-shaped nuclei of "precious metals -magnetic oxides":

[0089] The above (1) of the "solution A" is added to contain 100mg of oleic acid, 100mg of oleamine two surfactants and 5g of iron oleate of 10g octadecyne, first pass the inert gas, for a period of time hexane and other impurities are blown out. It is then heated to 300 °C. Keep the reaction time 3h, reduce to room temperature, add 20g ethanol and 10g chloroform wash, centrifuge to obtain the precipitate, and finally disperse the ...

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Abstract

The invention discloses a catalyst for hydrogenation synthesis of p-aminophenol, which comprises: a core, and a mesoporous silica shell covering the core, and the material of the core includes noble metal-magnetic oxide. The core of the catalyst in the present invention is composed of "noble metal-magnetic oxide". Because it is wrapped by the outer shell, the strong interaction between the contact interface of "noble metal and magnetic oxide" can be enhanced under the condition of avoiding agglomeration, which can greatly improve the catalyst performance. At the same time, due to the existence of magnetic oxides, they can be separated by magnets, which is convenient for recycling and improves the utilization rate. At the same time, the present invention also provides a preparation method of the catalyst, the preparation method is simple and easy to operate, the size and size of the product can be adjusted according to the needs, and it is applied to the hydrogenation reaction of p-nitrophenol, which can improve the conversion rate and selectivity of the reaction. sex.

Description

Technical field [0001] The present invention relates to a catalyst for hydrogenation to synthesize p-aminophenol reaction and a preparation method thereof, particularly to a catalyst may be applied to the hydrogenation of p-nitrophenol to synthesize p-aminophenol reaction and a preparation method thereof. Background [0002] P-nitrophenol is a common intermediate in organics, widely used in medicine, dye rubber and other fields. At present, the production methods of p-aminophenol include the reduction method of p-nitro iron powder, the catalytic hydrogenation method of nitrobenzene and so on. Nitrobenzene catalytic hydrogenation method uses nitrobenzene as a raw material to catalytically reduce hydrogenation in an acidic medium, and the precious metal reuse rate of such methods is low and the selectivity is not high. [0003] The patent under publication number CN106311274A discloses a catalyst that loads Ru on silica, a magnetic core that can be easily recycled. However, the si...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J23/89B01J35/00C07C213/02C07C215/76
Inventor 王義传尹宏峰黄伟新余小龙
Owner NINGBO INST OF MATERIALS TECH & ENG CHINESE ACADEMY OF SCI
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