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作 者:王信锐 尚小琴[1,2] 赖雅平[1,2] 刘汝锋[1,2] 陈浩亮[1] 王捷[1]
机构地区:[1]广州大学化学化工学院,广东广州510006 [2]广东省节能环保精细化学品工程技术研究开发中心,广东广州510006
出 处:《精细化工》2017年第3期268-273,333,共7页Fine Chemicals
基 金:国家自然科学基金项目(21303026);广东省科技计划项目(2016A010103044;2013B010403030);广州市科技计划项目(2013J4300043);大学生创新创业训练项目(201611078108;201611078002;201611078035)~~
摘 要:以棕榈酸、N,N-二甲基-1,3-丙二胺为原料,通过酰胺缩合反应合成中间产物——棕榈酰胺丙基二甲基叔胺,再与氯乙酸钠反应合成了两性表面活性剂——棕榈酰胺丙基甜菜碱(PAPB),并考察了反应温度和时间、反应物物质的量比、催化剂KOH用量和4A分子筛对棕榈酸转化率的影响;通过红外光谱和核磁共振氢谱对产物结构进行了表征;测试合成产物及其复配体系的表面活性。得到的酰胺缩合反应的最佳条件为:反应温度160℃、反应时间10 h、n(N,N-二甲基-1,3-丙二胺)∶n(棕榈酸)=1.05∶1.00,KOH用量为反应物总质量的0.5%,在该条件下,棕榈酸的转化率可达92.4%;产物的临界胶束浓度CMC为1.12×10^(-4)mol/L,γ_(CMC)为31.63 m N/m,对苯的增溶能力为X=4 980 m L/mol。Intermediate palmit amidopropyl dimethylamine was obtained by an amidation reaction between palmitic acid and N,N-dimethyl-1,3-propane diamine. Then,it reacted with sodium chloroacetate to afford palmitamidopropyl betaine( PAPB) amphoteric surfactant. The reaction temperature and time,the molar ratio between N,N-dimethyl-1,3-propane diamine and palmitic acid,the amount of catalyst,and 4 A molecular sieves were varied to study their influence on the conversion rate of palmitic acid. Meanwhile,the structure of the resulting product was characterization by FTIR and1 HNMR. Finally,the properties of palmitamidopropyl betaine and the mixed surfactant systems were investigated. The results show that the optimum conditions of amidation reaction were as follows: the reaction temperature was 160 ℃,the reaction time was 10 h,the molar ratio of reactants was 1. 05 ∶1,and the amount of catalyst KOH was 0. 5%( based on total mass of reactant). Under the above conditions,the conversion rate of palmitic acid reached 92. 41%. The critical micelle concentration( CMC) and surface tension( γCMC) of palmitamidopropyl betaine were 1. 12 × 10^-4mol / L and 31. 63 m N / m,respectively. And this synthesized surfactant showed good solubilization capacity of benzene( 4 980 m L/mol).
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