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机构地区:[1]淮海工学院化学工程系,江苏连云港222005
出 处:《精细化工》2005年第12期952-954,共3页Fine Chemicals
基 金:江苏省教育厅自然科学基金资助项目(04KJD150017);江苏省高校高新技术产业发展项目(JHB05-50)~~
摘 要:研究了邻氰基甲苯用光氯化法制备邻氰基氯苄的中试工艺.把160 kg的邻氰基甲苯投入到300 L的搪瓷反应釜中,把3只100 W白炽灯的光照引入到邻氰基甲苯液体中,在130~155 ℃下以9~10 kg/h速度通入干燥的氯气,通氯约40 kg停止反应,冷却氯化液,用离心机分离析出的晶体,母液再投入到反应釜中,重复上述操作,通氯质量分别为16 kg、11 kg和6 kg,把所得的邻氰基氯苄合并,用乙醇重结晶,干燥,共得到产物168 kg,总收率81.3%,w(邻氰基氯苄)=99.2%.160 kg o-cyanotoluene was treated at 150 ~ 155 ℃ with about 40 kg dry Cl2 at flowrate of 9 ~ 10 kg/h under the light of white lamp of 3 × 100 W. Then the reactant was cooled and filtered to give o-cyanobenzyl chloride. The same operation was repeated with the mother liquor, and amounts of chlorine gas introduced were successively 16 kg, 11 kg and 6 kg. The crystals were combined and recrystallized with alcohol to get 168 kg o-cyanobenzyl chloride with overall yield of 81.3% and mass fraction of 99.2%.
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