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Materials 2014, 7(10), 6982-6999; doi:10.3390/ma7106982

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

Nanotechnology and Catalysis Center (NANOCAT), University Malaya, Kuala Lumpur 50603, Malaysia
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Received: 1 July 2014 / Revised: 8 August 2014 / Accepted: 12 August 2014 / Published: 13 October 2014
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Abstract

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. View Full-Text
Keywords: microcrystalline cellulose; hydrocellulose; response surface methodology; percentage of crystallinity; amorphous sections microcrystalline cellulose; hydrocellulose; response surface methodology; percentage of crystallinity; amorphous sections
This is an open access article distributed under the Creative Commons Attribution License which permits unrestricted use, distribution, and reproduction in any medium, provided the original work is properly cited. (CC BY 4.0).

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Karim, M.Z.; Chowdhury, Z.Z.; Hamid, S.B.A.; Ali, M.E. Statistical Optimization for Acid Hydrolysis of Microcrystalline Cellulose and Its Physiochemical Characterization by Using Metal Ion Catalyst. Materials 2014, 7, 6982-6999.

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