通过γ-氯丙基三甲氧基硅烷的偶联,将水溶性聚乙烯亚胺(PEI)接枝在纳米SiO2表面,随后分别用1-溴己烷和碘甲烷对接枝的PEI进行N-烷基化修饰,使PEI中的部分氨基转变成季铵盐,得到水不溶性QPEI/SiO2微粒。通过测定PEI/SiO2上PEI的接枝量,考察了各种反应条件对QPEI/SiO2微粒制备的影响规律。研究结果表明,纳米SiO2表面接枝PEI的适宜条件为:反应溶剂为DMF,反应温度90-100℃,反应时间8h,氯丙基化SiO2与PEI质量比为4:1,在此条件下制备的QPEI/SiO2微粒中PEI接枝量为14.8%。QPEI/SiO2微粒经甲基化修饰后,季铵盐含量由0.96%增加到3.37%,其抗菌性能显著增强。
Water-soluble polyethylenimine (PEI) was grafted onto the surface of nano-SiO2 particles through the couple effect of γ-chloropropyltrimethoxysilane, and the water-insoluble antimicrobial SiO2 particles grafted with quaternized polyethylenimines ( QPEI/SiO2 ) was prepared followed by the N-alkylation of coated PEI with 1-bromohexane and idomethane ,respectively. The influences of various factors on the preparation of QPEI/SiO2 were examined via measuring the grafted amount of PEI on the composite of QPEI/SiO2. The results show that the optimum reaction conditions are as follows:the reaction temperature is 90 - 100 ℃ ,the reaction time is 8 h ,the mass ratio of CP-SiO2 to PEI is 4 : 1 ,and the reaction solvent is dimethyl formamide (DMF). The grafted amount of PEI in the QPEI/SiO2 prepared at the above conditions is 14.8%. Compared to the QPEI/SiO2 without methylation, the amount of quaternary ammonium salts in the methylated QPEI/SiO2 was added from 0.96% to 3.37%, and its antimicrobial activities against bacteria and yeast were enhanced obviously.