Method for synthesizing cyclohexanone-oxime and caprolactam

A technology for caprolactam and cyclohexanone oxime, which is applied in the field of synthesizing cyclohexanone oxime and caprolactam, can solve the problems of many side reactions, low utilization rate of raw materials, difficult operation and the like

Active Publication Date: 2015-02-11
XIANGTAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

The yield of caprolactam in this method is very low, the catalyst is expensive and difficult to separate
[0007] Similar reactions generally have problems such as large energy and material...

Method used

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  • Method for synthesizing cyclohexanone-oxime and caprolactam

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0033] The catalyst used is Pd / H-ZSM-5. The composition of the catalyst is: Pd=5%, and the rest is carrier H-ZSM-5. 0.3 g of the catalyst was pre-activated with hydrogen, and the activation conditions were as follows: the flow rate of hydrogen gas was 40 mL / min, normal pressure, the heating rate was 10 °C / min, 250 °C, and the reduction time was 3 h. Choose a fixed bed reactor. Add the raw material nitrocyclohexane, the reaction temperature is 350°C, the hydrogen pressure is 0.1MPa, the flow rate of the raw material is 40mL / min, and the liquid space velocity is 0.3h -1 The reaction time was 72h under certain conditions, and samples were taken for analysis. The liquid product was analyzed by gas chromatography. In the product, nitrocyclohexane was 25.66%, caprolactam was 53.65%, cyclohexanone oxime was 9.33%, and cyclohexylamine was 11.36%.

Embodiment 2

[0035] The synthesis reaction was carried out in the same manner as in Example 1, except that the raw material was replaced with a mixed solution of nitrocyclohexane and methanol at a volume ratio of 1:10. Through gas chromatography analysis, the nitrocyclohexane in the product is 22.24%, the caprolactam is 10.77%, the cyclohexanone oxime is 8.70%, and the cyclohexylamine is 58.19%.

Embodiment 3

[0037] In addition to changing the liquid space velocity to 3h -1 Except, carry out the synthetic reaction according to the same method as in Example 2, and analyze by gas chromatography, the nitrocyclohexane in the product is 25%, the caprolactam is 0.14%, the cyclohexanone oxime is 58.54%, and the cyclohexanone is 0.49%.

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Abstract

The invention relates to a method for synthesizing cyclohexanone-oxime and caprolactam, particularly a method for synthesizing cyclohexanone-oxime and caprolactam by performing catalytic hydrogenation on nitrocyclohexane used as a raw gas phase. The method has the advantages of high controllability, low cost, environmental protection, higher conversion ratio of raw materials and higher yield, and has industrialization application prospects. The reaction process is simple, no coproduct ammonium sulfate is generated in the reaction process, and no wastewater or waste gas is generated to pollute the environment, and thus, the method is an environment-friendly production technique.

Description

technical field [0001] The invention relates to a method for synthesizing cyclohexanone oxime and caprolactam. Background technique [0002] Caprolactam is an important petrochemical raw material, mainly used in the production of nylon 6 fiber, nylon 6 resin and film, widely used in textiles, automobiles, electronics, machinery and other fields, and can also be used in the production of antiplatelet drug 6-aminocaproic acid and laurocaprazine, etc. Among them, the demand for caprolactam for the production of nylon 6 fiber accounts for about 60% of the world's total demand, and the demand for resin products accounts for about 30%. The demand for nylon 6 resin in economically developed regions such as Japan, Western Europe, and the United States is one of the main growth drivers for the caprolactam market demand. [0003] There are many production techniques and routes for caprolactam. At present, the industrial production of caprolactam mainly uses benzene, phenol, and tolu...

Claims

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Application Information

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IPC IPC(8): C07C249/10C07C251/44C07D201/04C07D223/10
CPCY02P20/52
Inventor 刘平乐刘四化罗和安郝芳游奎一
Owner XIANGTAN UNIV
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