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机构地区:[1]浙江工业大学浙西分校化工系,浙江衢州324000 [2]浙江工业大学化材学院,浙江杭州310014
出 处:《精细化工中间体》2006年第4期51-53,共3页Fine Chemical Intermediates
基 金:浙江省教育厅科研项目(20050448)
摘 要:以全氟己烯(PFH)为氟溶剂,混酸为硝化剂,在氟双相体系中对甲苯进行硝化。实验表明:在反应温度为50℃,n(甲苯)∶n(硝酸)=1∶1.05,m(全氟己烯)∶m(甲苯)=1∶1.8,反应时间为4h,甲苯的转化率达99.5%,产品硝基甲苯总质量分数为98.3%,邻对位异构体质量比为1.51,硫酸、氟溶剂很容易通过相分离而得到回收利用。Nitration of toluene was studied with nitro-sulfuric acid using perfluorous hexene (PFH) as solvent, and effect of reaction temperature, the molar ratio of PFH to organic solvent and reaction time on the nitration were investigated. It was observed that the optimum conditions for fluorous phase nitration of toluene was reaction temperature 50℃, n(toluene) : n(HNO3)=1 : 1.05, n (HNO3) : n(HESO4)=1 : 1.2, m(PFH) : m(toluene) =1 : 1.8, reaction for 4 h. Conversion of toluene was 99.5%. The yield of the product mononitrotoluene was more than 98.3%, and the mass ratio of its o-and p-isomer was 1.51. The fluorous solvent and sulfuric acid can be recovered easily by simple phase separation, and reused for a number of times.
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