基于水溶液相分离的壳聚糖分离膜制备：成膜机理与微结构调控研究

壳聚糖作为一种环境友好型可再生生物聚合物，在推动膜分离领域的可持续发展中展现出巨大潜力。尽管水溶液相分离（aqueous phase separation，APS）凸显了浸没沉淀过程中完全水溶液环境的特点，但目前的研究尚未能够对不同壳聚糖水溶液在不同组分的凝胶浴水溶液中成膜的动力学过程进行深度解析，并在动力学分析的基础上揭示壳聚糖分离膜呈现出多样化微结构特征的规律。因此，本研究致力于改进基于光学相干断层成像（optical coherence tomography，OCT）的原位表征技术，并以此为基础深入探究在APS过程中调控壳聚糖微结构的潜在机理。

在将OCT技术与浸没沉淀过程相集成的同时，本研究对微型凝胶装置进行了技术性改造，使得凝胶浴能够以主动或者被动的方式与铸膜液层发生接触。一方面，主动接触模式被用于比较分析不同的凝胶过程；在这些凝胶过程中，壳聚糖被溶解在不同的水溶液中，且在APS中引入溶剂与非溶剂之间的非对称交换，进而改变凝胶阻抑物的移除方式。另一方面，被动接触模式能够以6.25 ms的时间分辨率精准捕捉初始形成的凝胶浴-铸膜液界面，其应用成功揭示了APS过程中界面振荡与反应势变化（氢氧化钠凝胶浴浓度由0.2 M增大至0.8 M）之间的紧密关联。同时，本研究还将基于OCT的表征技术与传统方法相结合，不但对分离膜的多孔网络进行了可视化对比分析，还深入剖析了在不同凝胶条件下（包括纯水和不同浓度的水/乙醇混合物）形成的微结构对示踪剂颗粒（0.1 μm）的截留机制，并在此基础上对分离膜微结构几何与拓扑特性（分别相应于多孔结构的非对称性和孔隙连通度）的变化进行合理推断。表征结果揭示了在浓度低于30 wt%临界值的情况下，乙醇在凝胶浴中存在能够有助于更曲折次级结构的形成，将分离膜纯水渗透通量降低为0 wt%乙醇凝胶浴条件下的25 。这些表征结果不仅为壳聚糖分离膜多孔形态的优化设计开辟了新的思路，也为在APS框架下制备拥有优化形态的壳聚糖分离膜提供了坚实的数据和理论支撑。

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