Namli Serap, Guven Ozge, Simsek Feyza Nur, Gradišek Anton, Sumnu Gulum, Yener Meryem Esra, Oztop Mecit
Middle East Technical University, Department of Food Engineering, Ankara, Turkey.
Jozef Stefan Institute, Department of Solid State Physics and Department of Intelligent Systems, Jamova cesta 39, SI-1000 Ljubljana, Slovenia.
Int J Biol Macromol. 2023 Oct 1;250:126123. doi: 10.1016/j.ijbiomac.2023.126123. Epub 2023 Aug 4.
Chitosan aerogels, obtained by (supercritical) CO drying of hydrogels, are novel adsorbents because of their large surface area and high porosity. Intrinsic properties of chitosan such as molecular weight (MW) and degree of deacetylation (DDA) had large impacts on the characteristics of chitosan aerogels. Although there are a few studies about the effects of solely DDA or MW on aerogel structure, none of them has focused on the mutual effects. The study aims to investigate the combined effects of MW and DDA of chitosan on aerogel properties. Hydrogels were produced in beads form by physical gelation of the chitosan solutions (2 % w/v in acetic acid of 1 %, v/v) in an alkaline environment (NaOH, 4 N). Supercritical CO dried aerogels were examined with respect to the bulk density, diameter as well as pore characteristics, and surface area by Barrett-Joyner-Halenda (BJH) and Brunauer-Emmett-Teller (BET) methods, respectively. Morphologies of aerogels were also examined by Scanning Electron Microscopy (SEM) images and structural changes of aerogels were observed by Fourier Transform Infrared (FTIR) Spectroscopy. Additional to BET-BJH analysis, proton relaxation dispersion was measured by Fast Field Cycling NMR (FFC-NMR) to determine the pore volume of the aerogels. Compact structures were obtained for higher MW chitosan and lower MW chitosans with higher DDA increasing the aerogel diameters. All types of aerogels obtained by different chitosan characteristics (MW and DDA) showed a porous structure and the highest DDA with the lowest MW caused the minimum bulk density with the highest water absorption rate. Although different N adsorption-desorption profiles were obtained in terms of pore volumes; all aerogels had Type IV isotherms with Type H hysteresis curve. FFC-NMR experiments showed that the coherence length values were associated with the pore volumes and FFC-NMR experiments were found to be meaningful as supportive experiments for the characterization of aerogels.
通过水凝胶的(超临界)CO2干燥获得的壳聚糖气凝胶,因其具有大表面积和高孔隙率而成为新型吸附剂。壳聚糖的内在性质,如分子量(MW)和脱乙酰度(DDA),对壳聚糖气凝胶的特性有很大影响。虽然有一些关于单独的DDA或MW对气凝胶结构影响的研究,但都没有关注它们的相互影响。本研究旨在探讨壳聚糖的MW和DDA对气凝胶性能的综合影响。通过壳聚糖溶液(在1%(v/v)乙酸中为2%(w/v))在碱性环境(4N NaOH)中物理凝胶化制备珠状水凝胶。分别采用巴雷特-乔伊纳-哈伦达(BJH)法和布鲁瑙尔-埃米特-特勒(BET)法对超临界CO2干燥的气凝胶的堆积密度、直径以及孔隙特征和表面积进行了研究。还通过扫描电子显微镜(SEM)图像检查了气凝胶的形态,并通过傅里叶变换红外(FTIR)光谱观察了气凝胶的结构变化。除了BET-BJH分析外,还通过快速场循环核磁共振(FFC-NMR)测量质子弛豫色散以确定气凝胶的孔体积。对于较高MW的壳聚糖获得了致密结构,而较低MW且较高DDA的壳聚糖会增加气凝胶直径。通过不同壳聚糖特性(MW和DDA)获得的所有类型的气凝胶均呈现多孔结构,且MW最低、DDA最高时导致堆积密度最小、吸水率最高。尽管就孔体积而言获得了不同的N吸附-脱附曲线;但所有气凝胶均具有IV型等温线和H型滞后曲线。FFC-NMR实验表明,相干长度值与孔体积相关,并且发现FFC-NMR实验作为气凝胶表征的辅助实验是有意义的。