摘要
以硬脂酸、N,N-二甲基乙醇胺(DMEA)和γ-氯丙基三甲氧基硅烷为原料合成酯基三甲氧基有机硅季铵盐,采用FTIR,ESI-MS和1HNMR对中间体及终产物进行了结构表征,结果与目标结构一致。通过正交试验,得到中间体硬脂酸二甲基乙醇胺酯的优化合成工艺条件:反应温度为180℃,反应时间为8 h,n(硬脂酸)∶n(DMEA)=1∶1.6,催化剂用量为原料总质量的0.5%。季铵化合成产物的优化工艺条件:在N2保护下,反应温度为110℃,n(硬脂酸二甲基乙醇胺酯)∶n(γ-氯丙基三甲氧基硅烷)=1∶1.4,催化剂用量为原料总质量的0.5%,反应时间为28 h。并通过稳态荧光法测得产物在298 K下的临界胶束浓度为0.009 3 g·L-1。
An ester group trimethoxy organosilicon quaternary ammonium salt was synthesized with stearic acid, dimethylethanolamine （DMEA） and y - chloropropyl trimethoxy siloxane as starting materials. Structure of the product was characterized by FTIR, ESI - MS and 1HNMR, and the characterization results showed that the product is accord with the target. Via orthogonal designed experiments, the optimum reaction conditions for preparing the intermediate stearic acid dimethylethanolamine ester were obtained as： reaction temperature, 180 ℃ ; reaction time, 8 h ; mole ratio, n （ stearic acid） ： n （DMEA） = 1 ： 1.6 ; dosage of the catalyst, 0. 5 % ; and for the quaternarization, reaction temperature, 110 ℃ under nitrogen atmosphere ; mole ratio, n （ stearic acid dimethylethanolamine ester）： n（γ- chloropropyl trimethoxy siloxane） = 1：1.4;dosage of the catalyst,0. 5% ; reaction time, 28 h. The cmc of the product under 298 K were determined by steady - state fluorescence analysis as 0. 009 3 g . L-1.
出处
《日用化学工业》
CAS
CSCD
北大核心
2014年第11期611-614,643,共5页
China Surfactant Detergent & Cosmetics
基金
产学研合作重大科技成果转化专题资助项目(20120913)
关键词
酯基三甲氧基有机硅季铵盐
合成
表面活性
稳态荧光法
ester group trimethoxy organosilicon quaternary ammonium salt
synthesis
surface activity
steady- state fluorescence analysis
