PDF全文下载:2011040342
李玉成a, 唐英俊b, 李露a*
(青岛科技大学 a.化工学院;b.化学与分子工程学院,山东 青岛 266042)
摘要: 采用浓硫酸和甲醇预混液滴加到单氰胺与甲醇混合液的方法合成了O-甲基异脲硫酸氢盐。考察了物料配比、反应时间、反应温度、浓硫酸滴加方式及洗涤溶液的种类对产品收率和纯度的影响。得到较佳的工艺条件为:n(单氰胺)∶n(硫酸)∶n(甲醇)=1∶1.5∶5,反应温度5 ℃,反应时间3 h,丙酮洗涤。产品收率可达74.4%,产品纯度可达98.1%。产品用FT-IR进行了表征。
关键词: 单氰胺; 合成; O-甲基异脲硫酸氢盐
中图分类号: O 643.32文献标志码: A
Synthesis of O-Methyl-isoure Hydrogen Sulphate
LI Yu-chenga, TANG Ying-junb, LI Lua
(Qingdao University of Science and Technology a.College of Chemical Engineering;
b.College of Chemistry and Molecular Engineering,Qingdao 266042,China)
Abstract: O-methyl-isoure hydrogen sulphate was synthesized using cyanogenamide,methanol and sulfuric acid as starting materials. The effect of n(cyenogenamide):n(sulfuric acid):n(methanol), reaction time, reaction temperature,the addition method of sulfuric acid and washing agents on the yield and purity of product were investigated. The obtained optimum reaction conditions were n(cyanogenamide)∶n(sulfuric acid)∶n(methanol) =1∶1.5∶5,reaction temperature 5 ℃, reaction time 3 h and using acetone as washing agent.Under above conditions, the yield and purity of product were 74.4% and 98.1% respectively. The structure of the obtained product was characterized by FT-IR.
Key words: cyanogenamide; synthesis; O-methyl-isoure hydrogen sulphate
收稿日期:2010-11-18
作者简介: 李玉成(1984—),男,硕士研究生.*通信联系人.