Studies On Process Of Beckmann Rearrangement Of Cyclohexanone Oxime To Caprolactam

Method of determination of cyclohexanone oxime concentration in esters gained in liquid phase Beckmann rearrangement is set up in the paper, which is a basis of the above reaction kinetics. Furthermore, kinetics of liquid phase Beckmann rearrangement is studied at temperature range of 20-45 ℃. Rate equation of the above reaction kinetics is put forward:in which cyclohexanone oxime reaction progression a is 2, H2SO4 reactionprogression b is 1 , activation energy is -1 9.86kJ/mol, and frequency factor ko is1.35 × 1027. Results of rearrangement reaction showed that dissociative SO3 does not participate in the reaction when H2SO4 is a catalyst, and acts only as absorbent. The above information supplies Jinlun plant of Juhua Group Corporation with good data for technology renovation in cyclohexanone oxime liquid phase Beckmann rearrangement.Through theoretical studies and according to production and technology renovation, two gtage rearrangement reaction pilot test passed. The optimum reaction conditions are that first stage circulation ratio is 250-400, temperature is 85 ℃; second stage circulation ratio is 200-270, temperature is 95℃ ; good ratio of oxime in first stage to oxime in second stage is 87:13-80:20; acid-oxime ratio in first atage is 1.7, D is less than 0.6;acid-oxime ratio in first atage is 145-1.57, D is less than 0.8. Acid-oxime ratio decreases from 1.7 to 1.40-1.45 in present production , which reaches the aim of technology renovation and is successful in production.