摘要
采用邻苯二甲酸酐保护壳寡糖的氨基制备了N-邻苯二甲酰化壳寡糖中间体,又通过引发剂辛酸亚锡引发ε-己内酯开环接枝聚合和脱去保护基的方法制备了新型生物医用功能材料前驱体壳寡糖接枝聚己内酯共聚物,该前驱体可进一步进行活性氨基的化学修饰。采用傅立叶红外光谱(FT-IR)、X射线衍射(XRD)、示差扫描量热仪(DSC)对N-邻苯二甲酰化壳寡糖接枝聚己内酯共聚物的化学结构、结晶性和热性能进行了表征。结果表明随着ε-己内酯与N-邻苯二甲酰化壳寡糖的摩尔比增加,接枝共聚物的DSC曲线出现了聚己内酯侧链的熔融峰,XRD也表明,壳寡糖分子不完善的结晶区被破坏,并在此基础上形成了新的均聚物聚己内酯(PCL)侧链的结晶区。
A novel biomedical functional material precursor, chitosan oligosaccharide-g-polycaprolactone, was synthesized via the amino groups protection procedure with phthalic anhydride to prepare phthaloyl chitosan oli- gosaccharide precursor. The graft polymerization was carried out by coupling the hydroxyl group via the ring-o- pening graft copolymerization of ε- caprolactone in the presence of tin( Ⅱ ) 2-ethylhexanoate ( stannous octoate) catalyst and removing the protective N- phthaloyl group. The prepared copolymers precursor can be used to further undergo chemoselective modification reactions through the active amino groups. The chemical structure , crystallinity and thermol propertity of the obtained N-phthaloyl chitosan oligosaccharide-g-polycaprolactone were characterized by Fourier transform infrared (FTIR) spectra, X-ray diffraction (XRD)and DSC. It was found that the copolymer could form melting endothermol peak of polycaprolactone side chains in DSC curve with the increasing of the mole ratio of ε- caprolactone to phthaloyl chitosan oligosaccharide. X-ray diffraction also showed that a new crystal domain of polycaprolactone occurred in the N-phthaloyl-chitosan oligosaccharide- g-polycaprolactone copolymer while the crystal structure of chitosan oligosaccharide was damaged.
出处
《功能材料》
EI
CAS
CSCD
北大核心
2008年第9期1511-1514,共4页
Journal of Functional Materials
基金
国家自然科学基金资助项目(50673015)
国家高技术研究发展计划(863计划)资助项目(2006AA02Z291)
关键词
壳寡糖
己内酯
功能材料前驱体
制备
表征
chitosan oligosaccharide
ε-caprolactone
functional material precursor
preparation
characterizations