卟啉修饰的壳聚糖光敏新材料的制备与表征

Synthesis and Characterization of the Chitosan-Porphyrin Complexes

关键词:  卟啉  壳聚糖  表征  正交实验  接枝率

Key words:  porphyrin  chitosan  characterization  orthogonal test  grafting rate

摘要:

目的 合成卟啉修饰的壳聚糖光敏新材料，对其进行表征，并优化其合成工艺。方法 以溴己烷苯基卟啉衍生物和壳聚糖为原料，以K₂CO₃为碱，采用四丁基溴化铵为相转移催化剂，合成卟啉-壳聚糖复合物，采用茚三酮法测定卟啉接枝率。通过单因素实验研究反应温度、反应时间、混合溶剂比例、催化剂当量等对接枝率的影响，采用正交实验法优化获得最佳制备工艺条件。结果 最佳合成条件为温度55℃、反应时间为5.5 h、混合溶剂中水和氯仿的比例为1：2、催化剂为1当量、无机碱使用K₂CO₃，卟啉的平均接枝率为41.30%。结论 通过共价偶联合成卟啉修饰壳聚糖光敏新材料的方法可行。

Abstract:

OBJECTIVE To synthesis and characterize the chitosan-porphyrin complexes(CS-BHP), and to optimize the experimental condition. METHODS CS-BHP was synthesized from 5-p-(6-bromohexylaminophenyl)-10,15,20-triphenyl porphyrin(BHP) and chitosan by using K₂CO₃ as a base and tetrabutylammonium bromide as a phase transfer catalyst. The porphyrin grafting rate of CS-BHP was detected with ninhydrin by UV-Vis. In the single factor analysis, the effect of temperature, reaction time, the volume ratio of water to chloroform in the component solvent, equivalent of the catalyst were investigated. The orthogonal test was used to optimize the condition of synthesis. RESULTS The optimized condition of the reaction was as follows:the temperature was 55℃, the reaction time was 5.5 h, the volume ratio of water to chloroform in the component solvent was 1:2, catalyst was 1 equivalent, and K₂CO₃ was used as base, the average porphyrin grafting rate of CS-BHP was 41.30%. CONCLUSION It is feasible to synthesize CS-BHP by the method of covalent coupling.