β-环糊精聚合物微球的合成与表征

Synthesis and Characterization of β-Cyclodextrin Polymer Microspheres

以β-环糊精(β-CD)为原料,环氧氯丙烷(ECH)为交联剂,用反相乳液法合成了β-环糊精聚合物(β-CDP)微球。采用L16(45)正交实验得出了最佳合成工艺,利用扫描电镜、红外光谱仪、综合热分析仪和X射线衍射仪进行了表征。结果表明,最佳合成工艺条件是:n(ECH)/n(β-CD)=15、乳化剂用量1.2g、煤油用量60mL、乳化温度70℃、反应时间5h;影响因素的大小依次为:乳化温度>乳化时间>乳化剂用量>n(ECH)/n(β-CD)>油水体积比;最佳工艺条件下合成的β-CDP微球粒径分布比较均一,表面圆整,呈现无定形聚集态,热稳定性好,色谱可涂性强。

β-Cyclodextrin polymer（β-CDP）microspheres were synthesized in the inverse emulsion with β-cyclodextrin as material and epichlorohydrin as crosslinking agent.The L16（45）orthogonal test was used to obtain optimum technological parameters.The polymer microspheres were characterized by scan electron microscope,FT-IR spectroscopy,thermogravimetric analysis（TGA）and X-ray diffraction（XRD）.The results indicated that the best ratio of epichlorohydrin to β-cyclodextrin was 15∶1,the quantity of emulsifier was 1.2 g,the quantity of kerosene was 60 mL,emulsifying temperature was 70 ℃ and the emulsifying time was 5 h.The influencing factors were emulsifying temperature,emulsifying time,the quantity of emulsifier,the ratio of epichlorohydrin to β-cyclodextrin,weight ratio of oil to water.The particle diameter distribution of those β-CDP microspheres under optimal conditions was relative uniform.The surface of the particles was smooth.They showed an amorphous aggregate state and thermal stability.The coating of the chromatograph was strong.