Catalyst for preparing halogeno anilin through catalytic hydrogenation of halogeno nitrobenzene and preparation method

A technology for halogenated nitrobenzene and halogenated aniline, which is applied in the preparation of amino compounds, the preparation of organic compounds, metal/metal oxide/metal hydroxide catalysts, etc. Expensive, reduce product quality and other problems, to achieve the effect of large implementation value and social and economic benefits, convenient catalyst and product separation, and avoid hydrodehalogenation

Inactive Publication Date: 2007-10-10
TSINGHUA UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Due to the influence of Al, the catalytic activity of this catalyst is lower than that of Raney Ni, and the catalytic activity decreases rapidly during the reaction process, which makes the catalyst usage per unit product larger, increases production costs, and dechlorination is relatively serious, reducing product quality
CN02148509.7 Using carbon nanotubes to support Pd or carbon nanotubes to support Pt as a catalyst to catalyze o-chloronitrobenzene or p-chloronitrobenzene or 3,4-dichloronitrobenzene or 3-chloro-4-fluoronitrobenzene Hydrogenation produces corresponding halogenated anilines, which can make the dechlorination rate less than 0.1%, but the catalyst is expensive, and dechlorination cannot be completely avoided, which reduces the product quality

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] 4wt%Au / ZrO 2 catalyst

[0029] Commercial zirconium oxychloride ZrOCl containing water of crystallization 2 ·8H 2 O is prepared into an aqueous solution with a concentration of 0.155mol / L for subsequent use, and the commercial ammonia water with a concentration of 25% is diluted 22 times as a precipitant, and the prepared ZrOCl is mixed with a speed of 3mL / min under continuous stirring. 2 The aqueous solution is added dropwise to the precipitating agent while controlling the final pH value of the solution between 9-11. Continue to stir for 0.5 hours after the dropwise addition, and leave it to stand for aging for 12 hours to obtain Zr(OH) 4 Hydrogels. Zr(OH) 4 After the hydrogel was washed and dried, it was calcined at 400 °C for 5 hours in flowing air (60 mL / min) to obtain ZrO 2 Carrier with a BET specific surface area of ​​123m 2 .g -1 .

[0030] Under the condition of continuous stirring, weigh 2.0 g of ZrO 2 Vehicle and 3.0 g of urea were added to 50 mL of...

Embodiment 2

[0032] 4wt%Au / P25TiO 2 catalyst

[0033] Under the condition of continuous stirring, weigh 2.0 g of P25 TiO 2 (Degussa company production, BET specific surface area 52m 2 .g -1 ) carrier and 3.0 g of urea were added to 50 mL of 8.1 mmol / L HAuCl 4 In aqueous solution, other preparation steps are the same as Example 1.

Embodiment 3

[0035] 4wt%Au / SiO2 catalyst

[0036] Under the condition of continuous stirring, weigh 2.0 g of SiO 2 (Degussa company production, BET specific surface area 90m 2 .g -1 ) carrier and 3.0 g of urea were added to 50 mL of 8.1 mmol / L HAuCl 4 In aqueous solution, other preparation steps are the same as Example 1.

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Abstract

A catalyst with high reaction activity, selectivity and stability for preparing halophenylamine by catalytic hydrogenation of halonitrobenzene is composed of carrier (ZrO2, TiO2, SiO3, or MgO) and active component (Au) (0.5-10 Wt %). Its preparing process includes such steps as providing chloroauric acid as precursor, depositing with urea, and ageing, washing, drying, and calcining at 200-350 deg.C.

Description

technical field [0001] The invention provides a catalyst for preparing halogenated aniline by catalytic hydrogenation of halogenated nitrobenzene and a preparation method thereof, belonging to the field of catalyst preparation. It is characterized in that the supported nano-Au is used as a catalyst to catalyze the liquid-phase hydrogenation of halogenated nitrobenzene to produce halogenated aniline. The catalyst catalyzes the liquid-phase hydrogenation of halogenated nitrobenzene to produce the corresponding halogenated aniline, which can completely avoid hydrogenation and dehalogenation. , and has the advantages of high reactivity, good selectivity and good stability, and can conveniently separate the catalyst and the product after the reaction is completed. Halogenated anilines are an important class of organic intermediates, which are widely used in the synthesis of fine chemical products such as medicines, dyes, and pigments, and are in great demand. Synthesis of haloanili...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/52B01J21/06C07C211/52C07C209/36
Inventor 徐柏庆何代平
Owner TSINGHUA UNIV
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