摘要
以环氧氯丙烷、三乙胺盐酸盐为原料,采用微波辐照合成3-氯-2-羟丙基三乙基氯化铵(CTA)。利用乙酸乙酯和乙醇混合溶液反复结晶提纯后,采用薄层色谱与化学滴定方法定性、定量分析产物纯度达到99%以上,使用红外吸收光谱、核磁共振对目标产物的结构进行分析鉴定;研究了微波功率、反应温度、反应时间和摩尔比对CTA合成产率的影响,从而得出CTA的最佳微波合成条件为:微波功率300W,反应温度50℃,反应时间为20min,三乙胺盐酸盐和环氧氯丙烷的摩尔比为1.15∶1,比传统加热工艺反应时间缩短340min,产率提高了16.58%;测定了CTA的表面张力、克拉夫点、临界胶束浓度和熔点等物理化学性能。
3-chlorine-2-hydroxypropyl triethyl ammonium chloride （ CTA ） was synthesized with epichlorohydrin, triethylamine muriate as raw materials under the irradiation of constant power microwave. Analysis by TLC and chemical titration indicated the purity of the product above 99.0% after the crystallization in the mixture of acetoacetate and ethanol. The structure of CTA was identified by IR and NMR. The factors which influenced the yield of CTA were investigated in terms of microwave power, reaction time, temperature and mole ratio of raw materials. Experimental results showed that the yield of CTA improved by 16.58% and the reaction time was 340 min shorter than the traditional method under the following reaction conditions： microwave power 300 W, 50℃, mole ratio of raw materials 1.15 ： 1, reaction time 20 min. Finally the CMC, surface tension, Krafft point and melting point of the CTA were determined.
出处
《化工学报》
EI
CAS
CSCD
北大核心
2009年第8期2130-2136,共7页
CIESC Journal
关键词
微波合成
结构表征
性能测定
microwave synthesis
structure characterization
performance
