新型酯基有机硅季铵盐的设计合成、表征及其性能研究

Study on the Synthesis,Characterization and Properties of New Ester-based Silicone Quaternary Ammonium Salts

研究设计了L16(45)正交试验,探讨了反应物摩尔比、反应时间、微波作用功率、催化剂用量和溶剂用量等因素对月桂酸甲基二乙醇胺单(双)酯与γ-氯丙基三甲氧基硅烷反应的影响,最终得出了较佳季铵化的工艺条件.分别是:γ-氯丙基三甲氧基硅烷与酯胺的摩尔比为1.5∶1,催化剂KI为酯胺摩尔数的20%,溶剂N,N-二甲基甲酰胺用量为反应物总质量的50%,微波作用功率为810 W,回流反应70 min.通过溴酚蓝法测定了有机硅季铵盐的含量.结果表明酯基有机硅季铵盐的收率达到74.5%.用合成的产物对棉布进行浸渍、脱水和干燥处理.选取大肠杆菌为测试菌,通过营养肉汤稀释法和营养琼脂法测定了被处理的棉织物的抗菌性能和耐洗涤性能.当处理液中产物的质量浓度为200μg/m L,干燥温度为120℃,干燥时间为15 min,被处理的样品经8次水洗后,对大肠杆菌的杀菌率仍然大于99%,表明制备的有机硅季铵盐有良好的抗菌活性和缓释性能.

The L16(4^5)orthogonal tests were designed to investigate the effect of molar ratio of reactants,reaction time,microwave power,catalyst and solvent dosage etc.On the reaction between lauric acid methyl two ethanolamine single(double)of ester and(γ-chloropropyl)trimethoxysilane,and the optimum conditions of quaternization were obtained.The molar ratio ofγ-(chloropropyl)trimethoxysilane to N-methyldiethanolamine is 1.5∶1,the catalyst(KI)is 20%of the moles of the N-methyldiethanolamine,and the amount of the solvent N,N-dimethylformamide is 50%of the total reactants mass,microwave power 810 W,refluxing reaction for 70 min.The results showed that the yield of ester-based organic silicon quaternary ammonium salt reached 74.5%by bromophenol blue method.And the cotton cloth was impregnated with the aqueous solution of the synthesized product,then dehydrated and dried.The antibacteria and resistance to washing performances of the treated cotton cloth were determined by nutrient broth dilution method and nutrient agar method.The results showed that the treated sample had a bactericidal ratio more than 99%although after 8 times washing when the sample was processed of by the aqueous solution of the product at 200μg/mL,dehydrated and dried at 120℃for 15 min,indicating that the prepared organosilicone quaternary ammonium salt has a good antibacteria and sustained-release properties.