维生素K3合成工艺优化  

Optimization of synthesis process of vitamin K3

作　　者：翁城武 朱鸿达 何意林[2] WENG Cheng-wu;ZHU Hong-da;HE Yi-lin(Comprehensive Technology Service Center Of Quanzhou Customs,Quanzhou 362000,China;College of Biotechnology and Pharmaceutical Engineering,Lanzhou Jiaotong University,Lanzhou 730070,China)

机构地区：[1]泉州海关综合技术服务中心,福建泉州362000 [2]兰州交通大学生物与制药工程学院,甘肃兰州730070

出　　处：《化学研究与应用》2023年第10期2517-2522,共6页Chemical Research and Application

基　　金：甘肃省科技计划项目(1508RJZA067)资助。

摘　　要：在维生素K3(亚硫酸氢钠甲萘醌,MSB)合成原有工艺基础上加入十二烷基磺酸钠和正己烷,通过正交试验确定其最佳工艺条件:铬离子浓度:2.75 mol·L^(-1),硫酸质量分数:17.5%;2-甲基萘(2-MN):氧化液(摩尔体积比)=1 mol:3.3 L;2-MN:十二烷基磺酸钠(质量比)=10:1;2-MN:正己烷(质量体积比)=1:3;投料顺序:先加入正己烷将2-MN溶解后,再加入十二烷基磺酸钠和氧化液;反应温度为30℃;反应时间为3 h;机械搅拌。并通过中试放大试验验证两步反应总收率能稳定在70%,MSB纯度可达94%,明显高于文献以及国内外各维生素K3生产厂家,为生产K系维生素其他产品提供了应用基础。On the basis of the original synthesis process of vitamin K3(menaphthoquinone sodium bisulfite,MSB),adding sodium dodecyl sulfonate and n-hexane,the optimal process conditions were determined by orthogonal experiment:chromium ion concentra-tion:2.75 mol·L^(-1),sulfuric acid mass fraction:17.5%;2-methylnaphthalene(2-MN):oxidizing liquid(molar volume ratio)=1 mol:3.3L;2-MN:Sodium dodecyl sulfonate(mass ratio)=10:1;2-MN:n-hexane(mass to volume ratio)=1:3;Feeding se-quence:added n-hexane to dissolve 2-MN,then added sodium dodecyl sulfonate and oxidation solution;the reaction temperature was 30℃.the reaction time was 3 h and mechanical stirring.The total yield of the two-step reaction was stable at 70%and the purity of MSB could reach 94%,which was significantly higher than the literature and other vitamin K3 manufacturers at home and abroad,and provided the application basis for the production of other K-series vitamin products.

关 键 词：维生素K3 合成 工艺优化 

分 类 号：O625.46[理学—有机化学]