摘要
以三正丙胺(TPA)和环氧氯丙烷为原料合成了缩水甘油基三丙基氯化铵(GTPA),并进行了分离纯化。采用元素分析、熔点测定、FT—IR及1^H NMR手段对产物进行了表征,用电位滴定法分析了产物含量。结果表明氯仿作为萃取剂、乙酸乙酯作为重结晶溶剂可有效去除产物中残留的环氧氯丙烷和TPA,产物中GTPA质量分数大于98%。GTPA适宜的合成条件为:乙醇作为反应介质,反应温度65℃,反应时间10h,n(环氧氯丙烷):n(TPA)=1.10:1,在此条件下GTPA收率可达88%以上。
The glycidyl tripropylammonium chloride (GTPA) was prepared through reaction between tripropyl amine and epichlorodrin. The product was purified through extraction and recrystallization, and characterized by elemental analysis, melting point measurement, FT-IR and 1^H NMR. The results indicated that epichlorodrin and tripropylamine could be removed effectively with chloroform as extractant and ethyl acetate as recrystallizing solvent. The content of GTPA in the product was found to be above 98%. The optimum conditions were found as follows: reaction temperature 65.0 ℃, reaction time 10.0 h, mass ratio of epichlorodrin to tripropylamine 1.10 and ethanol as solvent. The yield of GTPA reached above 88% under these conditions.
出处
《精细石油化工》
CAS
CSCD
北大核心
2008年第2期67-70,共4页
Speciality Petrochemicals
基金
国家科技支撑计划资助项目(2006BAD06B10)
盐城工学院应用化学重点学科建设基金(XKY2007031)