Preparation method of N-doped Cu-modified nickel-based activated carbon catalyst and application of N-doped Cu-modified nickel-based activated carbon catalyst in nitrocyclohexane hydrogenation reaction

A technology of nitrocyclohexane and activated carbon, applied in catalyst activation/preparation, catalyst, carbon compound catalyst and other directions, can solve the problems of high cost, high requirements, environmental pollution, etc., achieves less environmental pollution, improved conversion rate, cost reduction effect

Pending Publication Date: 2020-07-17
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

This method uses an amine borane compound as a reducing agent, which is expensive, inflammable and explosive, and has high requirements on the storage environment, and at the same time causes pollution to the environment
To sum up, th...

Method used

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  • Preparation method of N-doped Cu-modified nickel-based activated carbon catalyst and application of N-doped Cu-modified nickel-based activated carbon catalyst in nitrocyclohexane hydrogenation reaction
  • Preparation method of N-doped Cu-modified nickel-based activated carbon catalyst and application of N-doped Cu-modified nickel-based activated carbon catalyst in nitrocyclohexane hydrogenation reaction

Examples

Experimental program
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Effect test

Embodiment 1

[0028] Weigh 20g of commercial activated carbon, place it in a single-necked flask, add concentrated nitric acid according to the solid-to-liquid mass ratio of 1:20, stir and soak at room temperature for 24h, filter the suspension, wash with distilled water until neutral, and dry at 80°C for 12h to obtain Modified activated carbon. Take by weighing 1 g of the above-mentioned modified activated carbon and 1 g of melamine and place them in a single-necked flask, weigh 0.85 g of Ni(CH 3 COO) 2 4H 2 O, 0.04gCu(NO 3 ) 2 ·3H 2 O, after dissolving with 30g of deionized water, the resulting solution was added to a one-necked flask equipped with activated carbon, and a magnet was added, and stirred and impregnated at 30°C for 24h. Put the stirred suspension in a beaker and dry it in a drying oven at 80°C for 12 hours. Grind the dried solid into powder with an agate mortar, put it into a tube furnace for roasting and reduction, and protect the first stage under nitrogen. Heat up a...

Embodiment 2

[0030] Weigh 0.12g of the 1%Cu-20%Ni / N(melamine)-AC catalyst gained in Example 1 and place it in a 50mL liner of a high-temperature reactor, add 0.5g of nitrocyclohexane, 5.2g of ethylenediamine, and put Insert the magnet, seal the autoclave, replace the air in the autoclave with hydrogen for 4 times, evacuate the autoclave to a vacuum with a vacuum pump, and then place the autoclave in a heating jacket. After rising to the set reaction temperature of 100°C, hydrogen gas was introduced to pressurize to 0.3MPa, magnetic stirring was started, and the reaction timing started. After reacting for 8 hours, the reaction mixture was filtered, and the content of each substance in the filtrate was analyzed by gas chromatography. The conversion rate of nitrocyclohexane is 99.46%, and the selectivity of cyclohexanone oxime is 86.59%.

Embodiment 3

[0032] Weigh 0.12g of the 1%Cu-20%Ni / N(melamine)-AC catalyst gained in Example 1 and place it in a 50mL liner of a high-temperature reactor, add 0.5g of nitrocyclohexane, 5.2g of ethylenediamine, and put Insert the magnet, seal the autoclave, replace the air in the autoclave with hydrogen for 4 times, evacuate the autoclave to a vacuum with a vacuum pump, and then place the autoclave in a heating jacket. After rising to the set reaction temperature of 80°C, hydrogen gas was introduced to pressurize to 0.3 MPa, magnetic stirring was started, and the reaction timing started. After reacting for 8 hours, the reaction mixture was filtered, and the content of each substance in the filtrate was analyzed by gas chromatography. The conversion rate of nitrocyclohexane is 83.62%, and the selectivity of cyclohexanone oxime is 78.81%.

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Abstract

The invention discloses a preparation method of an N-doped Cu-modified nickel-based activated carbon catalyst and application of the N-doped Cu-modified nickel-based activated carbon catalyst in nitrocyclohexane hydrogenation reaction. The preparation method comprises the following steps: performing acid modification on activated carbon, taking the modified activated carbon as a carrier, performing N doping and nickel-copper loading at the same time, and applying the obtained N-doped Cu-modified nickel-based activated carbon catalyst to nitrocyclohexane hydrogenation reaction. Cu is used for modification, nickel acetate is used as a nickel source, the cost is low, pollution is small, equipment corrosion is avoided, non-noble metal nickel is used as an active component, melamine and urea are used as nitrogen sources, and activated carbon is used as a carrier, so that the cost can be obviously reduced. The obtained catalyst is used in nitrocyclohexane hydrogenation reaction, the conversion rate of nitrocyclohexane and the selectivity of cyclohexanone-oxime can be improved under relatively mild reaction conditions, and therefore the purpose that high-quality cyclohexanone-oxime is produced through the low-cost catalyst is achieved.

Description

technical field [0001] The invention relates to the preparation of an activated carbon catalyst, in particular to a preparation method of an N-doped Cu-modified nickel-based activated carbon catalyst and its application in the hydrogenation reaction of nitrocyclohexane. Background technique [0002] The hydrogenation of nitrocyclohexane mainly produces cyclohexanone oxime, and cyclohexanone oxime synthesizes caprolactam. Caprolactam is one of the important organic chemical raw materials, and is 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: fibers (civilian silk, industrial silk, carpet...

Claims

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Application Information

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IPC IPC(8): B01J27/24B01J37/08B01J37/18C07C251/44C07C249/10
CPCB01J27/24B01J37/18B01J37/088B01J37/08C07C249/10C07C2527/24C07C251/44
Inventor 刘平乐姚方勃熊伟吕扬郝芳罗和安
Owner XIANGTAN UNIV
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