荷梗纤维素纳米晶须的制备及其表征分析
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武汉轻工大学

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湖北省重点研发计划项目(2022BBA0023, 2021BED006)、湖北省农产品加工与转化重点实验室开放课题(2023HBSQGDKFB03)、湖北省青年拔尖人才培养计划(2022020801010389)


Preparation and Characterization of Peduncle Cellulose Nanocrystalline Whiskers
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Wuhan Polytechnic University

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    摘要:

    该文优化了荷梗纤维素纳米晶须的制备工艺,并表征了晶须的形貌结构及理化特性。以纤维素纳米晶须的得率为指标, 以料液比、水解时间和水解温度为考察因素进行单因素实验, 结合Box-Behnken响应面实验对制备工艺进行优化。确定最佳提取工艺条件为料液比为5:100 g/mL、水解时间为3.5 h、水解温度为 49 ℃,此条件下荷梗纤维素纳米晶须的得率为65.61%。扫描电镜和透射电镜结果表明硫酸水解将纤维素转化为具有短棒状形态的均匀纳米结构;X射线衍射结果和红外数据表明荷梗纳米纤维素晶须的成功制备并仍保持着纤维素基本的化学结构;粒径分析和PDI值表明水解程度越高,制备的晶须的粒径越小,其zeta电位分析表明制备的晶须悬浮液zeta电位绝对值较大,证明纳米颗粒的表面状态和稳定性较好;热分析表明所制备的纳米纤维素晶须具有较好的热稳定性。该制备工艺方法常用且高效,且证明可以用于稳定Pickering乳液,不仅可充分利用莲藕副产物资源, 而且有助于行业减损增值及可持续发展。

    Abstract:

    In this paper, the preparation process of the nanocrystalline whiskers was optimized, and the morphology, structure and physicochemical properties of the whiskers were characterized. The yield of cellulose nanowhisker was taken as the index, and the one-way experiment was carried out with the feed-liquid ratio, the hydrolysis time and the hydrolysis temperature as the investigating factors, and then the preparation process was optimized by the Box-Behnken response surface experiment. The optimum extraction conditions were determined as 5:100 g/mL, 3.5 h, 49 ℃, and 65.61% for the yield of pedunculated cellulose nanowhisker. Under these conditions, the yield of nanowhisker was 65.61%. The results of scanning electron microscopy (SEM) and transmission electron microscopy (TEM) showed that the cellulose was transformed into short rod-like nanostructures by sulfuric acid hydrolysis. The results of X-ray diffraction and infrared data showed that the nanocellulose whisker was successfully prepared and the basic chemical structure of cellulose was still maintained. Particle size analysis and PDI value showed that the higher the degree of hydrolysis, the smaller the particle size of the prepared whisker. The zeta potential analysis showed that the zeta potential of the prepared whisker suspension was larger, which proved that the surface state and stability of the nanoparticles were better. Thermal analysis shows that the prepared nanocellulose whisker has good thermal stability. The preparation process is common and efficient, and proved to be suitable for stabilizing Pickering emulsion, which can not only make full use of lotus root by-product resources, but also contribute to the industry"s loss and increase and sustainable development.

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  • 收稿日期:2024-07-04
  • 最后修改日期:2024-08-20
  • 录用日期:2024-08-21
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