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Method for preparing halogenated nitrobenzene selective hydrogenation high-activity nano-ruthenium catalyst

A technology of selective hydrogenation of halogenated nitrobenzene, which is applied in the direction of catalyst activation/preparation, amino compound preparation, organic compound preparation, etc., to achieve the effects of not easy to lose, high catalytic activity, and avoid organic pollution

Inactive Publication Date: 2009-11-04
JIANGSU KANGHENG CHEM
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The carbon monoxide reduction method has been studied in the laboratory, but there is no industrialization report

Method used

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Experimental program
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Effect test

Embodiment 1～4

[0025] Carrier is treated with lye before using in embodiment 1~4, and method is:

[0026] Prepare an appropriate amount of 4% sodium hydroxide aqueous solution, wet all the treated alumina by spraying, and dry it at 120-125°C.

Embodiment 1

[0028] 0.1g Ru(NO 3 ) 3 Dissolve in 50mL of water, adjust pH=1.0-1.1 with 30% hydrochloric acid, add 3.9mL of 5g / L PVP solution into Ru(NO 3 ) 3 In the aqueous solution, stir for 1 h, add 4.5 g / L NaBH dropwise, 40 mL of the aqueous solution, and obtain the PVP-protected metal ruthenium colloid after the reduction is completed. Then add 2 g of aluminum oxide, stir for 2 hours, filter and wash, and prepare Ru / AL with ruthenium loading of 3%. 2 o 3 catalyst.

Embodiment 2

[0030] 0.1gRuCl 3 h 2 Dissolve O in 50 mL of water, adjust the pH to 1.0-1.1 with 30% hydrochloric acid, add 5 mL of 5 g / L PVP solution into RuCl aqueous solution and stir for 1 h, then add 4.5 g / L NaBH dropwise. Aqueous solution 40mL, PVP-protected metal ruthenium colloid was obtained after the reduction was completed. Then add 2 g of aluminum oxide, stir for 2 hours, filter and wash, and prepare Ru / Ru / AL with a ruthenium loading of 3%. 2 o 3 catalyst.

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PUM

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Abstract

The invention discloses a method for preparing a halogenated nitrobenzene selective hydrogenation high-activity nano-ruthenium catalyst, which comprises the following steps: evenly mixing surfactant aqueous solution with pre-dissolved ruthenium salt solution; adding a reducer to deoxidize the mixture so as to form surfactant stable nano-ruthenium colloidal solution; adding a carrier to the ruthenium colloidal solution for adsorption, and filtering the mixture after the adsorption; and washing the catalyst until the filtrate is neutral to obtain the highly-dispersed supported nano-ruthenium catalyst. The method has the advantages of simplicity, low cost, good repeatability and environmental protection, and the prepared catalyst has high dispersion degree and long service life.

Description

Technical field: [0001] The present invention relates to a catalyst. Background technique: [0002] Halogenated anilines are an important class of organic intermediates, widely used in the synthesis of fine chemical products such as dyes, medicines, pesticides, and spices. In industry, chloroanilines are generally prepared by reducing chloronitrobenzenes. At present, the methods for reducing halonitrobenzene compounds to chloroarylamine compounds mainly include the following methods: chemical reduction method, electrolytic reduction method, carbon monoxide Reduction method, catalytic hydrogenation reduction method. The chemical reduction method, such as using iron powder, alkali sulfide, hydrazine hydrate, borohydride, etc. to organize production, has a long process flow, many wastes, and great environmental pollution. Due to the consideration of electrode materials, electrolysis equipment, cost and other aspects, the electrolytic reduction method has not been reported on ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/46B01J37/00C07C209/36C07C211/52
Inventor 邱志刚
Owner JIANGSU KANGHENG CHEM
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