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Statistical Optimization for Acid Hydrolysis of Microcrystalline Cellulose and Its Physiochemical Characterization by Using Metal Ion Catalyst

机译：金属离子催化剂对微晶纤维素酸水解的统计优化及其理化特性

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摘要

Hydrolyzing the amorphous region while keeping the crystalline region unaltered is the key technology for producing nanocellulose. This study investigated if the dissolution properties of the amorphous region of microcrystalline cellulose can be enhanced in the presence of Fe3+ salt in acidic medium. The process parameters, including temperature, time and the concentration of metal chloride catalyst (FeCl3), were optimized by using the response surface methodology (RSM). The experimental observation demonstrated that temperature and time play vital roles in hydrolyzing the amorphous sections of cellulose. This would yield hydrocellulose with higher crystallinity. The factors that were varied for the production of hydrocellulose were the temperature (x1), time (x2) and FeCl3 catalyst concentration (x3). Responses were measured in terms of percentage of crystallinity (y1) and the yield (y2) of the prepared hydrocellulose. Relevant mathematical models were developed. Analysis of variance (ANOVA) was carried out to obtain the most significant factors influencing the responses of the percentage of crystallinity and yield. Under optimum conditions, the percentage of crystallinity and yield were 83.46% and 86.98% respectively, at 90.95 °C, 6 h, with a catalyst concentration of 1 M. The physiochemical characteristics of the prepared hydrocellulose were determined in terms of XRD, SEM, TGA and FTIR analyses. The addition of FeCl3 salt in acid hydrolyzing medium is a novel technique for substantially increasing crystallinity with a significant morphological change.
机译：在保持结晶区域不变的同时水解无定形区域是生产纳米纤维素的关键技术。本研究探讨了在酸性介质中存在Fe 3 + 盐的条件下微晶纤维素无定形区的溶解性能是否可以增强。通过使用响应表面方法（RSM）优化了工艺参数，包括温度，时间和金属氯化物催化剂（FeCl3）的浓度。实验观察表明，温度和时间在水解纤维素的无定形部分中起着至关重要的作用。这将产生具有较高结晶度的水纤维素。生产纤维素的因素有多种：温度（x1），时间（x2）和FeCl3催化剂浓度（x3）。用所制备的水纤维素的结晶度百分比（y1）和产率（y2）来测量响应。开发了相关的数学模型。进行方差分析（ANOVA），以获得影响结晶度百分比和产率的响应的最重要因素。在最佳条件下，催化剂浓度为1 M，在90.95°C 6 h，结晶度和收率分别为83.46％和86.98％。制备的纤维素的理化特性由XRD，SEM， TGA和FTIR分析。在酸水解介质中添加FeCl3盐是一种新的技术，可显着提高结晶度并具有显着的形态变化。

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