二醋酸纤维素与β-环糊精接枝共聚物膜的制备与表征

Preparation and Characterization of Cellulose Diacetate Graftingβ-Cyclodextrin Copolymers Membrane

采用“两步法”合成了二醋酸纤维素与β-环糊精接枝共聚物（CDA-g-β-CD）。首先以二醋酸纤维素（CDA）与1，6-已二异氰酸酯（HDI）反应，得到端异氰酸酯预聚物（NCOCDA），然后将该预聚物与β-环糊精（β-CD）反应得到接枝共聚物CDA-g-β-CD。傅里时红外（FT-IR）和核磁氢谱（^1H-NMR）分析结果表明，β-CD是通过化学键连接到CDA上。采用正交实验法研究了β-CD与CDA质量比、HDI与CDA质量比、催化剂种类和用量对接枝反应的影响，确定了最佳配方和工艺。最佳工艺条件下制得的接枝共聚物接枝率为26.51％。采用沉浸相转化法制备了接枝共聚物膜，对葛根黄酮粗品进行循环式膜过滤实验。采用高效液相色谱（HPLC）法测定葛根素的分离效果，葛根素纯度从52．62％提高到65.77％。并用扫描电镜观察了接技共聚物膜的微观结构。

Cellulose diacetate grafting β-cyclodextrin copolymers （CDA-g-β-CD） were synthesized by two-step reactions of cellulose diacetate （CDA） with β-cyclodextrin （β-CD）. The isocyanate-terminated intermediate （NCOCDA） was prepared and β-cyclodextrin was grafted onto NCOCDA. The results of f fourier translation infrared spectroscopy （FT-IR） and ^1H nuclear magnetic resonance （^1H-NMR） analysis indicated that ,β-CD was connected to CDA by chemical bonding. The effects of mass ratio of β-CD to CDA, mass ratio of HDI to CDA, the type and dosage of catalyst were studied and the optimal formula and technology were determined by means of orthogonal experiments. The graft ratio of CDA-g-β-CD prepared under the optimal conditions was 26.51%. CDA-g-β-CD membrane was prepared via phase inversion and re-circulating filtration of total puerariae flavones solution was investigated. The purity ofpuerarin increased from 52.62% to 65.77% which was detected by HPLC method. The surface morphology of the graft copolymer membranes was observed by using scanning electron microscope （SEM）.