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Supported urushibara nickel catalyst and preparation method thereof

A lacquer original nickel and catalyst technology, which is applied in the field of supported lacquer original nickel catalyst and its preparation, can solve the problems of low catalytic strength, small specific surface area, and unreported research, and achieve increased catalyst strength, excellent hydrogenation performance, and specific surface area. increased effect

Inactive Publication Date: 2012-10-24
SEDIN ENG +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0007] At present, in the published research, Zn powder is used to reduce Ni to lacquer nickel. 2+ solution, and then prepared by developing with a developing agent. Although the catalyst prepared by this method has good hydrogenation performance, it has the disadvantages of small specific surface area and low catalytic strength, which limits its industrial application
Loading is an effective method to increase the specific surface area and catalyst strength of catalysts, but there is no report on the research on supported lacquer nickel catalysts

Method used

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  • Supported urushibara nickel catalyst and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Carrier pretreatment: 60-80 mesh SiO 2 Dry at 110°C for 10 hours to remove the moisture in the carrier.

[0028] ·Impregnation: according to the Fe load of 40wt%, using the equal volume impregnation method, put the dried carrier into FeCl 3 solution, and soaked at 40 ° C for 20 h under stirring conditions.

[0029] ·Drying and roasting: put the impregnated sample into an oven and dry at 110°C for 5h, grind the dried powder and place it in a muffle furnace and roast at 350°C for 3h to obtain Fe 2 o 3 / SiO 2 Prebody.

[0030] Hydrogen reduction: Fe 2 o 3 / SiO 2 Composition in volume is 5% H 2 with 95%N 2 Fe / SiO was obtained after reduction at 550°C for 12 hours in a mixed atmosphere 2 .

[0031] Reduction reaction: preparation of NiCl 2 solution, the prepared Fe / SiO 2 Dispersed in water to obtain Fe / SiO 2 Suspension, control Fe / Ni 2+ =4, then the NiCl 2 Solution added to Fe / SiO 2In the suspension, stir and react at 80°C for 11 hours to obtain a suspension...

Embodiment 2

[0035] Carrier pretreatment: 60-80 mesh SiO 2 Dry at 90°C for 2 hours to remove the moisture in the carrier.

[0036] ·Impregnation: according to the Fe load of 5wt%, using the equal volume impregnation method, put the dried carrier into FeCl 3 solution, and soaked at 40°C for 0.5h under agitation.

[0037] ·Drying and roasting: put the impregnated sample into an oven and dry at 90°C for 5h, grind the dried powder and place it in a muffle furnace and roast at 300°C for 1h to obtain Fe 2 o 3 / SiO 2 Prebody.

[0038] Hydrogen reduction: Fe 2 o 3 / SiO 2 Composition in volume is 10% H 2 with 90% N 2 Fe / SiO was obtained after reduction at 450°C for 12 hours in a mixed atmosphere 2 .

[0039] Reduction reaction: preparation of NiCl 2 with MoCl 2 The mixed solution, in which the amount of Mo added accounted for 4.4wt% of Ni, the prepared Fe / SiO 2 Dispersed in water, control Fe / Ni 2+ = 3, then add the mixed solution of Ni above to Fe / SiO 2 In the suspension, stir and r...

Embodiment 3

[0042] Carrier pretreatment: 80-100 mesh SiO 2 Dry at 100°C for 4 hours to remove the moisture in the carrier.

[0043] ·Impregnation: according to the Fe load of 8wt%, using the equal volume impregnation method, put the dried carrier into FeCl 3 solution, and soaked at 50°C for 4h under agitation.

[0044] Drying and roasting: put the impregnated sample into an oven and dry at 100°C for 6h, grind the dried powder and place it in a muffle furnace and roast at 350°C for 2h to obtain Fe 2 o 3 / SiO 2 Prebody.

[0045] Hydrogen reduction: Fe 2 o 3 / SiO 2 Composition in volume is 15% H 2 with 85% N 2 Fe / SiO was obtained after reduction at 500°C for 10 h in a mixed atmosphere of 2 .

[0046] Reduction reaction: preparation of NiCl 2 with CoCl 2 The mixed solution, wherein the addition of Zr accounted for 3wt% of Co, the prepared Fe / SiO 2 Dispersed in water, control Fe / Ni 2+ = 4, then the mixed solution of Ni above was added to Fe / SiO 2 In the suspension, stir and rea...

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Abstract

A supported urushibara nickel catalyst comprises 1-20wt% of Ni, 0.5-9wt% of Fe, an assistant having a weight being 0-30wt% of the Ni content, and 65-98wt% of a carrier. The catalyst has the advantages of low price and excellent catalytic hydrogenation performance.

Description

technical field [0001] The invention belongs to a nickel catalyst and a preparation method thereof, in particular to a loaded lacquer nickel catalyst and a preparation method thereof. Background technique [0002] Aromatic amino compounds are important chemical raw materials and chemical intermediates in the chemical industry. The common ones are aniline, toluidine, toluenediamine and chloronitroaniline. In industry, it is usually synthesized by hydrogenation of nitro compounds under the action of catalysts. The commonly used catalysts mainly include supported Pd / C and Pt / C and other noble metal catalysts and skeleton nickel catalysts. Among them, precious metal catalysts such as supported palladium, platinum and rhodium have high activity, but the cost is high and easy to deposit carbon; although the skeleton nickel is cheap, in the preparation process, due to the use of a large amount of caustic soda to extract aluminum, serious damage is caused. Environmental pollution, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/755B01J23/883B01J23/83B01J23/89C07C209/36C07C211/46C07C211/47C07C211/51C07C211/52
Inventor 范辉闫少伟崔晓曦李忠
Owner SEDIN ENG
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