液相贝克曼重排合成ε-己内酰胺分析-analysis of liquid phase beckmann rearrangement synthesis of ε -caprolactam.docxVIP

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液相贝克曼重排合成ε-己内酰胺分析-analysis of liquid phase beckmann rearrangement synthesis of ε -caprolactam.docx

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液相贝克曼重排合成ε-己内酰胺分析-analysis of liquid phase beckmann rearrangement synthesis of ε -caprolactam

Abstractε-caprolactam（CPL） is an important organic chemical intermediates. It is widely used to spinning, electron, automobile, shipping, machinery trades and medicine. At present, the last step of commercial processes for nearly 95% caprolactam is Beckmann rearrangement of cyclohexanone oxime, which is catalyzed by concentrated sulfuric acid or fuming sulfuric acid. The process brings serious corrosion of the equipment, forms a large amount of low-value ammonium sulfate asby-product with a high cost, and causes environmental pollution seriouly. In this work, we explored the liquid-phase Beckmann rearrangement of cyclohexanone oxime and improved the traditional process. The catalyzed systems of H2SO4/Cr/SiO2and cyanuric chloride (CNC) were examined.The main worksare as follows:First of all, the liquid-phase Beckmann rearrangement over H2SO4/Cr/SiO2 had been researched. The influences of reaction temperature, amount of catalyst, reaction time and amount of solvent were examined, and obtained the optimized reaction conditions. Results indicate that under the condition of cyclohexanone oxime 1.0g,H2SO4/Cr/SiO2 0.6g, reaction temperature 40 ℃ reaction time 5 h, amount ofsolvent12ml, cyclohexanone oxime conversion is 96.9% and selectivity of caprolactam reaches 92.5%. Cyclohexanone is the main by-product under this catalyzed system.Moreover, the liquid-phase Beckmann rearrangement over cyanuric chloridehad been researched. The influences of reaction temperature, amount of catalyst, reaction time, solvent ratio, amount of solvent and cocatalyst were examined, and obtained the optimized reaction conditions. Results indicate that under the condition ofcyclohexanone oxime 2.76g, cyanuric chloride 36mg, reaction temperature 80℃reaction time 2.5h, solvent ratio 1.25, amount of solvent20ml, cyclohexanone oxime conversion can reach 98.4% and selectivity of caprolactam can reach97.2%. Cyclohexanone is the main by-product under this catalyzed system, and