摘要
以3-氯-1,2-丙二醇和氨水为原料合成了3-氨基-1,2-丙二醇,并引入活性炭脱色和氨回收工艺,及分子蒸馏技术。考察了原料摩尔比、反应温度和反应时间等因素对产物收率的影响,当n(氨):n(3-氯-1,2-丙二醇)=15:1,反应温度为50℃,反应时间为4 h,采用分子蒸馏分离产物时,3-氨基-1,2-丙二醇的收率为90%,产物纯度为99.6%。采用元素分析、IR、~1H NMR和^(13)C NMR对产物进行了表征。
3-Amino-I, 2-propanediol was prepared from 3-chloro-1,2-propanediol and ammonia. The process of activated charcoal decoloration, ammonia recovery and molecular distillation were intro- duced. The effects on the yield were investigated, such as the molar ratio of ammonia and 3-chloro-1,2-propanediol, reaction temperature and reaction time. The yield of product was 900//00 and the purity was 99.6% under optimized conditions that n(ammonia) : n(3-chloro-l,2-propanediol) =15 : 1, reac-tion temperature was 50 ℃, reaction time was 4 h, and the separation process was molecular distil-lation. The structure of target compound was characterized by elemental analysis, IR, ^1H NMR and 13 C NMR.
出处
《精细石油化工》
CAS
CSCD
北大核心
2012年第6期14-17,共4页
Speciality Petrochemicals
基金
陕西省科技厅工业攻关项目(2011K08-01)