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Method for preparing cyclohexanone oxime by catalysis of transferring and hydrogenating of nitrocyclohexane

A technology for catalytic transfer hydrogenation and nitrocyclohexane, applied in chemical instruments and methods, oxime preparation, physical/chemical process catalysts, etc. The effect of the reaction effect, the effect of the good reaction effect

Active Publication Date: 2019-01-08
HUNAN UNIV OF SCI & ENG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] At present, the process of preparing cyclohexanone oxime by hydrogenation of nitrocyclohexane (CN105772053A, CN102125840A, CN104341318A, CN105777577A) needs to be prepared by using flammable and explosive hydrogen as a hydrogen source through a high-pressure reactor, and these processes generally have reaction Problems of high device cost and complicated operation process
In addition, the existing nitrocyclohexane hydrogenation process often requires the use of special solvents to provide an alkaline environment,

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0024] 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, 0.0381gCu(NO 3 ) 2 ·3H 2 O. After dissolving with 34g of distilled water to form a solution, add the solution to 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 dry it in a drying oven at 110°C for 12 hours, grind the dried solid into powder with a mortar, put it into a tube furnace for roasting and reduction, the first stage is in nitrogen Under protection, the temperature is ra...

Embodiment 2

[0027] Weigh 0.12g of the catalyst 1%Cu-20%Ni / AC obtained in Example 1 and place it in a three-necked flask, add 0.5g of nitrocyclohexane and 10g of aminoborane. Stir magnetically at 60°C and heat to reflux. After reacting for 8 hours, the reaction mixture was filtered, and the content of each substance in the filtrate was quantitatively analyzed by gas chromatography. The conversion rate of nitrocyclohexane was 73.90%, and the selectivity of cyclohexanone oxime was 81.45%.

Embodiment 3

[0029] Weigh 0.12g of the catalyst 1%Cu-20%Ni / AC obtained in Example 1 and place it in a three-necked flask, add 0.5g of nitrocyclohexane, 3g of ethylenediamine, and 1g of aminoborane, and stir magnetically at 60°C, Heat to reflux. After reacting for 8 hours, the reaction mixture was filtered, and the content of each substance in the filtrate was quantitatively analyzed by gas chromatography. The conversion rate of nitrocyclohexane was 75.25%, and the selectivity of cyclohexanone oxime was 80.52%.

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Abstract

The invention discloses a method for preparing cyclohexanone oxime by catalysis of transferring and hydrogenating of nitrocyclohexane. The method comprises the following steps: adding catalyst cupper-nickel-loaded activated carbon, nitrocyclohexane and an amine borane compound in a reactor according to the mass ratio of 0.1-0.4 to 1 to 2-20.8; reacting for 6 to 12 hours at 50 to 80 DEG C under stirring conditions to obtain a reaction liquid; filtering and separating the obtained reaction liquid to obtain the cyclohexanone oxime. According to the method, hydrogenation reaction of the nitrocyclohexane is catalyzed by taking a hydrogen storage material as a hydrogen donor; a preparation process can be completed through a common glass instrument without the equipment, such as a high-pressure reaction kettle, so that the cost of a reaction device is reduced, the operation of the reaction is simplified, and the safety of a reaction process is improved.

Description

technical field [0001] The invention relates to the field of material preparation, in particular to a method for preparing cyclohexanone oxime by catalytic transfer hydrogenation 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, 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 food packaging films. In addition, caprola...

Claims

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Application Information

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IPC IPC(8): C07C251/44C07C249/10B01J23/755
CPCB01J23/755C07C249/10C07C2601/14C07C251/44
Inventor 唐珊珊肖新生李杨燕
Owner HUNAN UNIV OF SCI & ENG
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