摘要
四氢呋喃(THF)与一甲胺(MA)经自制负载γ-A12O3床层的固定床反应器,催化脱水一步法合成N-甲基四氢吡咯,200吨/年生产装置工艺优化参数为:床层温度330℃,n(THF)/n(MA)=1.30,泵料速度33000ml/hr,床内径1000mm,净床高3000mm,催化剂装填量2500Kg,床层装填高1050mm,列管径76mm,温度梯度T1-4=240-345,压力梯度P1-3=0.2-04-0.01Mpa,一次合成粗品含量即达97%,采用共沸精馏技术,产品纯度≥99.5%,水分<0.1%,总收率≥97.5%,质量优于国外试剂的水平,催化剂长期使用无需再生,稳定性好。
The preparation of 1-methylpyrrolidine under the condition of effective catalystγ-Al_2O_3 for catalytic synthesis by dehydration of tetrohydrofuran with methylamine.Yield 97.5%purily≥99.5%moisture 0.1%was achieved on the optimized 200t/ y producing process conditions:Reaction temperature 330 Y,methylamine(MA)/tetrohydrofuran(THF)(molar ratio):1.30,speed of injecting raw materials:33000ml/hr,stop time:15s.Purity of first crude product from the self-made fixed-bed reactor:97.5%, Temperature gradient:T1-4=240-345℃,presure gradient:P1-3=0.2-0.4-0.01Mpa,The catalyst has high catalytic activities and rate, good chemical stability and little waste discharge in 10 years' synthesis.
