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

Materials

Md. Ziaul Karim²  Zaira Zaman Chowdhury²  Sharifah Bee Abd Hamid¹  Md. Eaqub Ali² 

[1] Nanotechnology and Catalysis Center (NANOCAT), University Malaya, Kuala Lumpur 50603, Malaysia;

关键词: microcrystalline cellulose;    hydrocellulose;    response surface methodology;    percentage of crystallinity;    amorphous sections;   

DOI  :  10.3390/ma7106982

来源: mdpi

【 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.

【 授权许可】

CC BY   
© 2014 by the authors; licensee MDPI, Basel, Switzerland.