过硫酸铵引发法制备维生素K_3的合成研究  

Study on ammonium persulfate initiation synthesis of Vitamin K_3

作　　者：李运涛[1] 郝文强[1] 关琳[1] 党蓓君 

机构地区：[1]陕西科技大学化学与化工学院,陕西西安710021

出　　处：《陕西科技大学学报（自然科学版）》2015年第4期75-79,共5页Journal of Shaanxi University of Science & Technology

基　　金：陕西省科技厅工业攻关科技计划项目(2012K08-22)

摘　　要：以过硫酸铵为引发剂,双氧水为氧化剂,冰乙酸为溶剂,将2-甲基萘氧化为2-甲萘醌,进而制得亚硫酸氢钠甲萘醌.研究了反应时间、反应温度、引发剂的用量及反应物与氧化剂、溶剂的物料比等因素对产品收率的影响.确定了最佳的反应条件是2-甲萘醌的合成条件为:反应时间3h,反应温度85℃,引发剂的用量为反应物总量的2%,n(2-甲基萘)∶n(冰乙酸)∶n(双氧水)=1∶15∶11.5.亚硫酸氢钠甲萘醌的合成条件为:反应温度45℃,反应时间1h,n(2-甲萘醌)∶n(亚硫酸氢钠)=1∶1.5.在以上条件下,2-甲萘醌的收率为54%,亚硫酸氢钠甲萘醌的收率为70%.Synthesis of 2-methylnaphthoquinone with ammonium persulfate as initiator in the acetic-H202 system by oxidation of 2-methylnaphthalene was researched.The effects of reaction temperature,reaction time,amount of initiator,reactant and solvent material ratio and other factors onβ-methylnaphthoquinone yeild were investigated.The best performences were achieved.The synthesis conditions of 2-methylnaphthoquinone：reaction time 3h,reaction temperature 85 ℃,molar ratio of 2-methylnaphthalene to acetic acid and Hydrogen peroxide 1∶11.5∶15,amoout of initiator is 2% of the total amount of reactant.The synthesis conditions of menadione sodium bisulfite：reaction time 1h,reaction temperature 45℃,molar ratio of 2-methylnaphthoquinone to sodium bisulfite 1∶1.5.In these conditions,the yelid of2-methylnaphthoquinone was 54%,the yelid of menadione sodium bisulfite was 70%.

关 键 词：2-甲基萘 过硫酸铵 2-甲萘醌 亚硫酸氢钠甲萘醌 

分 类 号：TQ466.6[化学工程—制药化工]