High dispersing supported type nickel catalyst prepared by lamellar precursor and preparation method thereof

A nickel catalyst, supported technology, applied in the direction of catalyst activation/preparation, chemical instruments and methods, physical/chemical process catalysts, etc., can solve the problems of no catalyst separation and recovery, difficult separation and recovery, poor catalyst dispersion, etc. Achieve high activity and use stability and life effect

Inactive Publication Date: 2004-03-24
BEIJING UNIV OF CHEM TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, such catalysts have poor dispersion in liquid-solid catalytic systems and are difficult to separate and recover
In the above-mentioned U.S. patents and other related patents and academic papers, the separation and recovery of catalysts are not involved

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] Weigh 3g γ-Al 2 o 3 , put in 120ml 0.2M Ni(NO 3 ) 2 ·6H 2 O and 40ml 0.5M NH 4 NO 3 Stir in the mixed solution, adjust the pH value of the mixed solution to 8 with 1% ammonia solution during the stirring process, keep the temperature of the mixed solution at 40 ° C, and stir for 10 h; then use secondary deionized water to wash, and the washed sample is Dry at 100°C, put it into a muffle furnace and roast at 300°C for 6 hours, and finally place the sample in a fixed-bed reduction device, use H 2 :N 2 =0.1:1 mixed gas was reduced at 300° C. for 6 hours to obtain a catalyst. The Ni content of the catalyst was measured to be 14%, and its degree of dispersion was 27%.

[0020] In a 300ml stainless steel tank reactor, use this catalyst to carry out the reaction of liquid phase nitrobenzene catalytic hydrogenation to produce aniline, the reaction conditions are: reaction temperature 100 ℃, H 2 The partial pressure is 10atm, the catalyst dosage is 100g / L nitrobenzene, ...

Embodiment 2

[0022] Weigh 4gη-Al 2 o 3 , put in 120ml 2M Ni(SO 4 ) 2 ·6H 2 O and 40ml 5M NH 4 NO 3Stir in the mixed solution, adjust the pH value of the mixed solution to 11 with 5% NaOH solution during the stirring process, keep the temperature of the mixed solution at 100°C, and stir for 2h; then use secondary deionized water to wash, and the washed sample is in Dry at 100°C, put it into a muffle furnace and bake at 900°C for 24 hours, and finally place the sample in a fixed-bed reduction device, and use 0.5:1 ratio of H 2 / N 2 The mixed gas was reduced at 900°C for 24 hours to obtain the catalyst. The Ni content of the catalyst was measured to be 13%, and its degree of dispersion was 17%.

[0023] The application performance test of the catalyst was carried out under the same conditions as in Example 1, and the conversion rate of nitrobenzene was 88%, and the selectivity of aniline was 90%.

Embodiment 3

[0025] Weigh 4g γ-Al 2 o 3 , put in 100ml 0.5M Ni(NO 3 ) 2 ·6H 2 O and 60ml 2M NH 4 NO 3 Stir in the mixed solution, adjust the pH value of the mixed solution to 9 with 2% KOH solution during the stirring process, keep the temperature of the mixed solution at 60 ° C, and stir for 12 hours; then use secondary deionized water to wash, wash the sample in Dry at 100°C, put it into a muffle furnace and bake at 500°C for 6 hours, and finally place the sample in a fixed-bed reduction device, use 0.2:1 ratio of H 2 / N 2 The mixed gas was reduced at 500°C for 6 hours to obtain the catalyst. The Ni content of the catalyst was found to be 16%, and its degree of dispersion was 24%.

[0026] The application performance test of the catalyst was carried out under the same conditions as in Example 1, and the conversion rate of nitrobenzene was 94%, and the selectivity of aniline was 95%.

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Abstract

The present invention provides a high-dispersion loaded type nickel catalyst prepared by using lamellar precursor and its preparation method. Said invention uses Al2O3 as carrier, in the surface layer internal hole of Al2O3 the lamellar precursor hydrotalcite (LDHs) containing Ni metal ions is assembled so as to obtain the NiAl-LDHs / Al2O3 composite material, then the composite material is roasted at high temp. and unverted into the correspondent composite metal oxide. Before application the composite metal oxide is undergone the process of reduction treatment so as to obtain the loaded type Ni base catalyst in which the metal Ni is highly dispersed in the surface of internal hole of Al2O3 carrier. Said catalyst has high activity and selectivity, and can be used in catalytic hydrogenation reaction.

Description

Technical field: [0001] The invention relates to a highly dispersed and supported nickel catalyst prepared from a layered precursor and a preparation method thereof. The catalyst is mainly used to catalyze the hydrogenation reduction of nitrobenzene to prepare aniline. technical background: [0002] Industrially, two types of catalysts are mainly used to prepare aniline by catalytic hydrogenation reduction of nitrobenzene: supported noble metals such as Pd, Pt, Ru catalysts and Ni-based catalysts such as Raney nickel (Appl. Catal. A: General 2000, 202: 17). The Raney nickel catalyst needs to use a large amount of NaOH strong alkali solution in the preparation process, which has serious environmental pollution problems; while the use of noble metal catalysts is economically unacceptable. The development of new supported Ni-based hydrogenation catalysts that are cheap, efficient and non-polluting to the environment, avoiding the use of strong alkali solutions to improve enviro...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J37/02
Inventor 段雪张法智李殿卿毛纾冰
Owner BEIJING UNIV OF CHEM TECH
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