摘要
以芥酸和N,N-二甲基-1,3-丙二胺为原料经缩合反应生成芥酸酰胺丙基二甲基胺,再与亚硫酸氢钠和环氧氯丙烷反应生成的3-氯-2-羟基丙磺酸钠进行季铵化反应,合成出芥酸酰胺丙基羟基磺基甜菜碱。研究了合成的优化工艺条件,用红外光谱法对产品进行表征,并对其性能进行了评价。结果表明,缩合反应的优化工艺条件为:n(芥酸)∶n(N,N-二甲基-1,3-丙二胺)=1∶1.1,反应温度为160℃,反应时间为10 h,催化剂用量为1.5%,此条件下产率为82.7%;季铵化反应的优化工艺条件为:n(芥酸酰胺丙基二甲基胺)∶n(3-氯-2-羟基丙磺酸钠)=1∶1.1,反应温度为85℃,反应时间为8 h,此条件下产率为88.1%。产物溶液的cmc为1.78×10-5mol·L-1,30℃时γcmc为40.1 mN·m-1,60℃时γcmc为30.6 mN·m-1;对Ca2+的容忍度达8 g·L-1;质量分数为2%时溶液表观黏度可达204 mPa·s。
Erucic acid and N, N -dimethyl- 1,3 -propane diamine were used as starting materials for preparation of erucoylamidopropyl dimethylamine via condensation. The latter was further quaterized with sodium 3 -chloro -2 -hydroxy propane sulfonate, which was formed by reaction between sodium hydrosulfite and epichlorihydrin, for synthesis of the targeted product erucoylamidopropyl hydroxysulfobetaine. Optimization of the synthesis conditions was studied. The targeted product was characterized by IR, and its performance was evaluated. Experimental results showed that the optimum conditions for the condensation are as follows: n( erucic acid):n( N, N- dimethyl- 1,3 -propane diamine) = 1:1.1, reaction temperature 160 ℃, reaction time 10 h, catalyst dosage 1.5%. Under the above mentioned conditions the yield can achieve 82. 7%. The optimum conditions for the quaterization are : n ( erucoylamidopropyl dimethylamine ) : n ( sodium 3 - chloro - 2 - hydroxy propane sulfonate) = 1 : 1.1, reaction temperature 85 ℃, reaction time 8 h. Under these conditions the yield of the quarterization can achieve 88. 1%. The cmc of the targeted product is 1.78 x 10-5 tool · L-1. The γcmc achieves 40. 1 mN · m- 1 at 30 ℃, and 30. 6 mN· m-1 at 60 ℃. Tolerance to Ca2+ achieves 8 g · L-1. Apparent viscosity of a solution of the targeted product with mass fraction of 2% achieves 204 mPa · s.
出处
《日用化学工业》
CAS
CSCD
北大核心
2014年第1期19-22,30,共5页
China Surfactant Detergent & Cosmetics