TEMPO氧化法制备纳米几丁质晶须粒子的优化及其产品特性表征

以虾壳几丁质为原料,利用TEMPO-NaBr-NaClO选择性氧化体系制备羧基化纳米几丁质晶须粒子。测定了反应体系中pH值与NaClO(13%有效氯)含量的变化对几丁质羧基化的影响,研究了生产高羧基含量和小颗粒粒度纳米几丁质晶须的最佳反应条件。利用傅里叶变换红外光谱、透射电子显微镜、动态光散射对制备的负电荷纳米几丁质晶须粒子进行结构表征,测定产品水悬浮液的有效粒径和有效电位;采用电导率法测定负电荷纳米几丁质的羧基含量。实验结果表明:在反应体系B1(pH=10.5,V(NaClO)=15mL)中,制备的负电荷纳米几丁质羧基含量最大,达(3.16±0.23)mmol/g,纳米晶须粒子流体动力学粒径(Z-average)为(113.97±2.29)nm,Zeta电位为(-38.73±4.49)mV;在反应体系B0(pH=10.5,V(NaClO)=18mL)中,制备的NC-晶须的羧基含量、粒子Z-average和Zeta电位分别为(3.00±0.41)mmol/g、(106.13±0.38)nm和(-41.41±6.83)mV。上述两种条件制备的纳米几丁质晶须粒子羧基含量和Zeta电位没有显著差异,但B0晶须粒子有效粒径最小。由于纳米材料的小尺寸效应是影响纳米材料生物活性的关键因素,因此制备高生物活性的纳米几丁质晶须的最佳条件是B0,即制备条件为pH=10.5,V(NaClO)=18mL(13%)。     

Super-Macroporous Lightweight Materials Templated from Bicontinuous Intra-Phase Jammed Emulsion Gels Based on Nanochitin (Small 39/2023)

Non-equilibrium multiphase systems are formed by mixing two immiscible nanoparticle dispersions, leading to bicontinuous emulsions that template cryogels with interconnected, tortuous channels. Herein, a renewable, rod-like biocolloid (chitin nanocrystals, ChNC) is used to kinetically arrest bicontinuous morphologies. Specifically, it is found that ChNC stabilizes intra-phase jammed bicontinuous systems at an ultra-low particle concentration (as low as 0.6 wt.%), leading to tailorable morphologies. The synergistic effects of ChNC high aspect ratio, intrinsic stiffness, and interparticle interactions produce hydrogelation and, upon drying, lead to open channels bearing dual characteristic sizes, suitably integrated into robust bicontinuous ultra-lightweight solids. Overall, it demonstrates the successful formation of ChNC-jammed bicontinuous emulsions and a facile emulsion templating route to synthesize chitin cryogels that form unique super-macroporous networks.