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Preparation method of Fe-doped nickel-based activated carbon catalyst and application thereof in hydrogenation reaction of nitrocyclohexane

A technology of nitrocyclohexane and activated carbon, applied in oxime preparation, organic chemistry, etc., can solve the problems of high catalyst cost, low catalyst activity, serious environmental pollution, etc., and achieve the effect of improving conversion rate, low cost and reducing cost

Inactive Publication Date: 2017-05-31
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

This method has the problems of high catalyst cost when supporting noble metals and low catalyst activity when supporting non-noble metals.
[0007] In summary, the current nitrocyclohexane hydrogenation process has problems such as high catalyst cost and serious environmental pollution, and the direct replacement of noble metals with non-precious metals to reduce costs will result in low yields

Method used

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  • Preparation method of Fe-doped nickel-based activated carbon catalyst and application thereof in hydrogenation reaction of nitrocyclohexane

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0023] Weigh 10g 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, soak at room temperature for 12 hours, filter the suspension with suction, wash with distilled water until neutral, and dry at 100°C for 12 hours to obtain activation After activated carbon. Take by weighing the activated carbon 1g after above-mentioned pretreatment and place in single-necked flask, weigh 1.13gNi (NO 3 ) 2 ·6H 2 O, 0.0734gFe(NO 3 ) 3 9H 2 O, after dissolving with 34g of distilled water, add the solution into a single-necked flask equipped with activated carbon, add a magnet, and stir and impregnate at 30°C for 10h. Put the stirred suspension in a beaker and put it in a drying oven at 110°C to dry for 12 hours, grind the dried solid into powder with a mortar, put it into a tube furnace for roasting and reduction, and the first stage is in Under nitrogen protection, 30-350°C is used to heat u...

Embodiment 2

[0025] Weigh 0.12g of the 1%Fe-20%Ni / AC catalyst obtained 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 in a magnet, Seal the autoclave, replace the air in the autoclave with hydrogen for 4 times, evacuate the autoclave to vacuum with a vacuum pump, and then place the autoclave in an oil bath. After rising to the set reaction temperature of 60°C, hydrogen 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 was 87.55%, and the selectivity of cyclohexanone oxime was 83.09%.

Embodiment 3

[0027] Weigh 0.12g of the 1%Fe-20%Ni / AC catalyst obtained 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 in a magnet, Seal the autoclave, replace the air in the autoclave with hydrogen for 4 times, evacuate the autoclave to vacuum with a vacuum pump, and then place the autoclave in an oil bath. After rising to the set reaction temperature of 50°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 was 75.63%, and the selectivity of cyclohexanone oxime was 81.21%.

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Abstract

The invention provides a preparation method of an Fe-doped nickel-based activated carbon catalyst and application thereof in hydrogenation reaction of nitrocyclohexane. According to the preparation method, activated carbon is acidified first, then the acidified activated carbon is used as a carrier to be loaded with nickel and iron simultaneously, and then the Fe-doped nickel-based activated carbon catalyst is applied to the hydrogenation reaction of nitrocyclohexane. The preparation method uses Fe for carrying out doping modification, has low cost and low pollution, cannot corrode equipment, and adopts the non-noble metal nickel as the active component and activated carbon as the carrier, thus obviously reducing the cost; and the prepared catalyst is used in the hydrogenation reaction of the nitrocyclohexane and can improve the conversion rate of nitrocyclohexane and the selectivity of cyclohexanone-oxime in relatively mild reaction conditions, thereby realizing production of high-quality cyclohexanone-oxime with a low-cost catalyst.

Description

technical field [0001] The invention belongs to the field of material preparation, in particular to a preparation method of Fe-doped nickel-based activated carbon catalyst and its application in nitrocyclohexane hydrogenation reaction. 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 silk), engineering plastics and fo...

Claims

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Application Information

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IPC IPC(8): B01J23/755C07C249/10C07C251/44
CPCB01J23/755C07C249/10C07C251/44
Inventor 刘平乐唐珊珊郝芳熊伟熊绍锋罗和安
Owner XIANGTAN UNIV
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