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利用离子凝胶法将低分子量的壳聚糖(CS)制成纳米CS,为探讨影响纳米CS粒径的因素,采用正交试验设计分析CS浓度、CS与三聚磷酸钠(TPP)溶液的体积比、搅拌时间和超声时间对粒径大小的影响,通过直观分析和方差分析优化选择。结果表明:CS与TPP溶液的体积比影响最大,其次为CS浓度、超声时间和搅拌时间。最佳工艺条件为CS浓度2.5g/L,CS∶TPP=5∶1,搅拌时间为10min,超声时间为30min。用红外光谱(FT-IR)、X射线衍射(XRD)、热重(TG)、X射线光电子衍射(XPS)对其进行表征,FT-IR和XPS分析表明,纳米CS、低分子量CS与原CS的主要化学成分相同;XRD结果表明,随着分子量和粒径的减小,水溶性增强;TG表明3种CS的热稳定性顺序:CS>纳米CS>低分子量CS。
In order to explore the factors that affect the particle size of nanocrystals, the CS concentration was determined by orthogonal design. The effects of CS and TPP solution Volume ratio, stirring time and ultrasonic time on the size of the particle size, through visual analysis and analysis of variance to optimize the choice. The results showed that the volume ratio of CS to TPP solution had the greatest effect, followed by CS concentration, ultrasonic time and stirring time. The optimum conditions for the CS concentration of 2.5g / L, CS: TPP = 5: 1, stirring time was 10min, ultrasonic time was 30min. FT-IR, XRD, TG and XPS were used for characterization. The results of FT-IR and XPS indicated that the nanoscale CS, low molecular weight CS and the original The main chemical components of CS were the same. The results of XRD showed that water solubility increased with the decrease of molecular weight and particle size. TG showed that the order of thermal stability of the three CSs was CS> nano CS> low molecular weight CS.