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作 者:武宏科[1] 许建帼[2] 史鸿鑫[1] 项菊萍[1] 朱建萍[1]
机构地区:[1]浙江工业大学化材学院绿色化学合成技术国家重点实验室培育基地,浙江杭州310014 [2]浙江工业大学浙西分校,浙江衢州324006
出 处:《高校化学工程学报》2007年第6期1076-1079,共4页Journal of Chemical Engineering of Chinese Universities
基 金:浙江省自然科学基金(Y405396);浙江省科技厅(20051020);浙江省应用化学重中之重学科开放基金(2006-10)
摘 要:;利用全氟壬烯-甲苯两相体系研究甲苯的硝化反应。以全氟壬烯为甲苯硝化反应的溶剂,考察了硝化体系、甲苯和全氟壬烯的相比、反应时间和反应温度对硝基甲苯收率的影响。在反应温度下全氟壬烯可以和甲苯形成全氟壬烯-甲苯两相体系。在等摩尔量的甲苯和发烟硝酸中,在浓硫酸催化下,全氟壬烯使单硝基甲苯收率大大提高。在n(甲苯):n(发烟硝酸):n(浓硫酸):n(全氟壬烯)=1:1:0.2:0.52,50℃下反应5h,硝基甲苯收率达到95.2%。全氟壬烯回收率高达97.6%,直接套用6次,硝基甲苯收率变化不大。反应后又会分成两相处理方便,硫酸可以回收利用,是较好的绿色硝化方法。Perfluorous nonene (C9F18) can form fluorous biphase system with toluene at the nitration reaction temperature of toluene. Nitration of toluene with fluorous biphase system was studied by using the perfluorous nonene as solvent. The effects of nitration system, phase ratio of perfluorous nonene and toluene, reaction time and temperature on the yield of nitrotoluene were investigated. Experiments show that the yield of nitrotoluene can be increased by using perfluorous nonene in the nitration of equal molars of toluene and fuming nitric acid. When the nitration system is consisted ofn (toluene) : n( fuming HNO3): n (concentrated H2SO4):n (C9F18) = 1 :1 : 0.2 : 0.52, the yield of nitrotoluene can reach 95.2% with reaction temperature of 50℃ for 5 h. It was found that 97.6% used C9F18 can be recovered, and the yields of nitrotoluene have little change during reusing the recovered C9F18 for 6 times. The post-treatment of the nitration process proposed is very simple, and the used H2SO4 can be recovered and reused too. All these show that the proposed nitration process is a good green toluene nitration process.
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