Preparation method and application of nitrogen-doped activated carbon supported alkali metal modified nickel-based catalyst

A nickel-based catalyst, activated carbon technology, applied in catalyst activation/preparation, amino compound preparation, organic compound preparation and other directions, can solve the problems of complex preparation process, low recovery rate, large hydrogen consumption, etc., and achieves simple preparation process, The effect of reducing production costs and improving production conditions

Active Publication Date: 2016-09-07
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0011] Rh/α-Al prepared by ion exchange method by Alini et al. 2 o 3 The catalyst is used in the liquid-phase partial hydrogenation of adiponitrile. Under the reaction conditions of 3 MPa hydrogen pressure, 500 psi ammonia pressure, and 100°C, when the conversion rate of adiponitrile is 60%, the selectivity of aminocapronitrile It can reach 99%, but the recycling rate of precious metal catalysts is low, and it is easy to deactivate. At the same time, it is necessary to add a large amount of ammonia or alkali metal hydroxide to inhibit the formation of by-products
[0012] To sum up, the above catalysts for the hydrogenation of adiponitrile either have complex preparation processes, or use a large amount of noble metals as active components, or are not very active, which ma...

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036]Weigh 30g of wood charcoal material, put it in a 1000mL single-neck flask, add 450mL of nitric acid solution with a mass fraction of 50% according to a solid-to-liquid ratio of 1:15, put it in a magnet, and stir in a water bath with a constant temperature of 30°C. (stirring speed is 1000rpm) for 12 hours, the suspension is suction filtered, washed repeatedly with distilled water until neutral, and dried at 100°C for 2 hours to obtain the desired activated carbon material. Weigh the above 10g of activated carbon and place it in a 100mL single-neck flask, add 20ml of deionized water, 10g of melamine, and 20ml of 38% formaldehyde solution by mass, put it into a 75°C oil bath and stir (stirring speed is 1000rpm), while the stirring process Add 5ml of 0.5mol / L NaOH solution, stir (stirring rate is 1000rpm) for 60min; cool the obtained mixture to room temperature, add 5ml of acetic acid, stir (stirring rate is 1000rpm) for 12 hours, centrifuge, filter, at 100 ℃ drying for 10 h...

Embodiment 2

[0039] Weigh 1 gram of the above 1%K-20%Ni / N-AC catalyst and place it in the 100mL lining of the high temperature reaction kettle, add 50mL of absolute ethanol, 5g of adiponitrile, put it into the magnet, seal the autoclave, use nitrogen The air in the autoclave was replaced 4 times, the autoclave was evacuated by a vacuum pump, and then the autoclave was placed in an oil bath. After reaching the set reaction temperature of 70 °C, hydrogen was introduced to pressurize it to 2 MPa, and the magnetic stirring was started (stirring rate was 1000 rpm), and the reaction timing started. After the reaction, the reaction mixture was filtered, and the content of each substance in the filtrate was analyzed by gas chromatography. The conversion of adiponitrile was 92.32%, the selectivity of 6-aminocapronitrile was 11.95%, and the selectivity of hexamethylenediamine was 80.36%.

Embodiment 3

[0041] Weigh 1 gram of the above 1%K-20%Ni / N-AC catalyst and place it in the 100mL lining of the high temperature reaction kettle, add 50mL of absolute ethanol, 5g of adiponitrile, put it into the magnet, seal the autoclave, use nitrogen The air in the autoclave was replaced 4 times, the autoclave was evacuated by a vacuum pump, and then the autoclave was placed in an oil bath. After reaching the set reaction temperature of 80 °C, hydrogen was introduced to pressurize it to 2 MPa, and the magnetic stirring was started (stirring rate was 1000 rpm), and the reaction timing started. After the reaction, the reaction mixture was filtered, and the content of each substance in the filtrate was analyzed by gas chromatography. The conversion of adiponitrile was 99.49%, the selectivity of 6-aminocapronitrile was 1.12%, and the selectivity of hexamethylenediamine was 86.96%.

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Abstract

The invention discloses a preparation method and application of a nitrogen-doped activated carbon supported alkali metal modified nickel-based catalyst. The preparation method includes the steps that firstly, acid activation or acid modification is conducted on a wooden charcoal material, nitrogen doping treatment is conducted on the wooden charcoal material, and then the wooden charcoal material is impregnated and supported with nickel and alkali metals. The nitrogen-doped activated carbon supported alkali metal modified nickel-based catalyst is applied to an adiponitrile hydrogenation process and can have high activity and high overall selectivity on 6-aminocapronitrile and hexamethylenediamine under relatively mild reaction conditions. Usage of a large number of precious metals serving as active components is avoided, equipment is not corroded (a large amount of additional ammonia or alkali metal hydroxide for inhibiting the formation of by-products is not needed), the cost is low, the catalyst is friendly to the environment, the preparation process of the catalyst is simple, the used active charcoal material is cheap and easy to obtain, and the preparation method is simple and has a very good application prospect.

Description

technical field [0001] The invention relates to the fields of material preparation and chemical engineering, in particular to a preparation method and application of a nitrogen-doped activated carbon-supported alkali metal-modified nickel-based catalyst. Background technique [0002] The hydrogenation of adiponitrile mainly produces 6-aminocapronitrile and hexamethylenediamine, and 6-aminocapronitrile is cyclized to synthesize caprolactam. Caprolactam is one of the important organic chemical raw materials, mainly used to synthesize nylon-6 fiber and nylon-6 engineering plastics . Due to its excellent thermal stability, high mechanical strength, chemical resistance and processability, caprolactam has a wide range of applications and is mainly used in automobiles, medical equipment, ships, electrical and electronic, daily necessities and other fields. From a global perspective, the consumption areas of caprolactam mainly include three categories of fibers (civilian silk, indu...

Claims

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Application Information

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IPC IPC(8): B01J27/24C07C253/30C07C255/24C07C209/48C07C211/12
CPCB01J27/24B01J37/084B01J37/18C07C209/48C07C253/30C07C255/24C07C211/12
Inventor 刘平乐吕扬郝芳罗和安
Owner XIANGTAN UNIV
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