β-环糊精聚合物微球的合成与表征

Synthesis and Characterization of β-Cyclodextrin Polymer Microspheres

摘要:

摘要：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）正交试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)为15∶1、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。

Abstract:

Abstract: β-cyclodextrin polymer (β-CDP) microspheres were synthesized in 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 1.2g, the quantity of kerosene was 60mL emulsifying temperature was 70℃ and the emulsifying time was 5h. Influence factors were emulsifying temperature, emulsifying time, the quantity of emulsifier, the ratio of epichlorohydrin to β-cyclodextrin , weight ratio of oil to water in order. The particle diameter distribution of those β-CDP microspheres under optimal conditions was relative uniform. The surface of the particles was smooth. They showed amorphous aggregate state and thermal stablity. The coating of the chromatograph was strong.