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Sepiolite-loaded nickel-based catalyst modified by two metals, as well as preparation method and application of sepiolite-loaded nickel-based catalyst

A nickel-based catalyst, catalyst technology, applied in the preparation of amino compounds, metal/metal oxide/metal hydroxide catalysts, catalyst supports, etc., can solve the problem of low recycling rate of precious metal catalysts, not very high activity, and complicated preparation processes and other problems, to achieve the effects of improving production conditions, inhibiting the formation of by-products, and simplifying the preparation process

Active Publication Date: 2015-09-23
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Rh / α-Al was prepared by ion exchange method by Alini et al. 2 o 3 The catalyst is used in the partial hydrogenation reaction of adiponitrile in liquid phase. Under the reaction conditions of 3MPa hydrogen pressure, 500psi ammonia pressure and 100℃, when the conversion rate of adiponitrile is 60%, the selectivity of aminocapronitrile reaches 99%. %, but the recycling rate of noble metal catalysts is low, and it is also easy to deactivate, and it is also necessary to add a large amount of ammonia or alkali metal hydroxide to suppress the formation of by-products
[0006] To sum up, the above catalysts used for the hydrogenation of adiponitrile either have complex preparation process, serious equipment corrosion, or use a large amount of precious metals as active components, and are easy to deactivate, or the activity is not very high, so that higher cost

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028]Weigh 30 grams of sepiolite, put it in a 1000mL single-necked flask, add 450mL of 1moL / L hydrochloric acid solution according to the solid-to-liquid mass ratio of 1:15, put it into a magnet, and place it in an oil bath with a constant temperature of 75°C The pot was vigorously stirred for 24 hours, the suspension was filtered with suction, washed with distilled water, neutralized, and dried at 100°C for 2 hours to obtain the required acid-modified sepiolite, which was used as a carrier. Weigh 5 grams of the above-mentioned acid-modified sepiolite (SEP), place it in a 100 mL one-necked flask, impregnate it with 25 mL of distilled water, and place it in a constant temperature water bath at 30°C with vigorous stirring for later use. Weigh 4.95 grams of Ni(NO 3 ) 2 . 6H 2 O, 0.06474 g KNO 3 , 0.3115 g La(NO 3 ) 2 . 6H 2 O was placed in a 50mL beaker and dissolved in 10mL of distilled water. The solution after the solution was added to the vigorously stirred acid-mod...

Embodiment 2

[0031] Weigh 1 gram of the above-mentioned 0.5% K-2% La-20% Ni / SEP catalyst and place it in a 100 mL lining of a high-temperature reactor, add 50 mL of absolute ethanol and 5 grams of adiponitrile, put it into a magnet, seal the autoclave, The air in the kettle was replaced with nitrogen for 4 times, the kettle was evacuated to a vacuum by a vacuum pump, and then the reaction kettle was placed in an oil bath. After rising to the set reaction temperature of 110°C, hydrogen was introduced to pressurize to 2 MPa, magnetic stirring was started, 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 rate of adiponitrile was 97.06%, the selectivity of 6-aminocapronitrile was 20.83%, and the selectivity of hexamethylenediamine was 58.29%.

Embodiment 3

[0033] Weigh 30 grams of sepiolite, put it in a 1000mL single-necked flask, add 450mL of 1moL / L hydrochloric acid solution according to the solid-to-liquid mass ratio of 1:15, put it into a magnet, and place it in an oil bath with a constant temperature of 75°C The pot was vigorously stirred for 24 hours, the suspension was filtered with suction, washed with distilled water, neutralized, and dried at 100°C for 2 hours to obtain the required acid-modified sepiolite, which was used as a carrier. Weigh 5 grams of the above-mentioned acid-modified sepiolite (SEP), place it in a 100 mL one-necked flask, impregnate it with 25 mL of distilled water, and place it in a constant temperature water bath at 30°C with vigorous stirring for later use. Weigh 4.95 grams of Ni(NO 3 ) 2 . 6H 2 O, 0.09711 g KNO 3 , 0.3115 g La(NO 3 ) 2 . 6H 2 O was placed in a 50mL beaker and dissolved in 10mL of distilled water. The solution after the solution was added to the vigorously stirred acid-mo...

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Abstract

The invention relates to sepiolite-loaded nickel-based catalyst modified by two metals of potassium and lanthanum, as well as a preparation method and application of the sepiolite-loaded nickel-based catalyst to adiponitrile hydrogenation. The preparation method comprises the following steps: taking adiponitrile as a raw material and ethanol as a solvent, and taking sepiolite as a carrier of a catalyst to prepare a nickel-based sepiolite-loaded catalyst modified by potassium and lanthanum as additives. The preparation process of the catalyst comprises acid treatment on sepiolite, and steeping, drying, roasting and reducing of sepiolite after acid treatment. During the adiponitrile hydrogenation process, the reaction pressure is 1-2 MPa, and the reaction temperature is 100-120 DEG C. The catalyst has relatively high activity and 6-aminocapronitrile and hexamethylendiamine selectivity under relatively mild reaction conditions, the raw material of sepiolite is cheap and easy to obtain, and low in cost, and the catalyst is simple in preparation method, and has a good application prospect.

Description

technical field [0001] The invention relates to a nickel-based catalyst loaded with bimetallic potassium and lanthanum modified by sepiolite, its preparation method, and its application in the process of hydrogenating adiponitrile to prepare 6-aminocapronitrile and hexamethylenediamine. 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 corrosion resistance and processability, caprolactam has a wide range of applications, mainly in the fields of automobiles, medical equipment, ships, electronic appliances, and daily necessities. From a global perspective, the consumption fields of caprolactam mainly include three categories:...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J23/83B01J32/00C07C253/30C07C255/24C07C211/12C07C209/48
Inventor 刘平乐吕扬郝芳罗和安
Owner XIANGTAN UNIV
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