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

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...

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Main Authors: Md. Ziaul Karim, Zaira Zaman Chowdhury, Sharifah Bee Abd Hamid, Md. Eaqub Ali
Format: Article
Language:English
Published: MDPI AG 2014-10-01
Series:Materials
Subjects:
Online Access:http://www.mdpi.com/1996-1944/7/10/6982
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author Md. Ziaul Karim
Zaira Zaman Chowdhury
Sharifah Bee Abd Hamid
Md. Eaqub Ali
author_facet Md. Ziaul Karim
Zaira Zaman Chowdhury
Sharifah Bee Abd Hamid
Md. Eaqub Ali
author_sort Md. Ziaul Karim
collection DOAJ
description 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.
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spelling doaj.art-18db7be022d849b8b2b233187f560f0c2022-12-22T03:55:06ZengMDPI AGMaterials1996-19442014-10-017106982699910.3390/ma7106982ma7106982Statistical Optimization for Acid Hydrolysis of Microcrystalline Cellulose and Its Physiochemical Characterization by Using Metal Ion CatalystMd. Ziaul Karim0Zaira Zaman Chowdhury1Sharifah Bee Abd Hamid2Md. Eaqub Ali3Nanotechnology and Catalysis Center (NANOCAT), University Malaya, Kuala Lumpur 50603, MalaysiaNanotechnology and Catalysis Center (NANOCAT), University Malaya, Kuala Lumpur 50603, MalaysiaNanotechnology and Catalysis Center (NANOCAT), University Malaya, Kuala Lumpur 50603, MalaysiaNanotechnology and Catalysis Center (NANOCAT), University Malaya, Kuala Lumpur 50603, MalaysiaHydrolyzing 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.http://www.mdpi.com/1996-1944/7/10/6982microcrystalline cellulosehydrocelluloseresponse surface methodologypercentage of crystallinityamorphous sections
spellingShingle Md. Ziaul Karim
Zaira Zaman Chowdhury
Sharifah Bee Abd Hamid
Md. Eaqub Ali
Statistical Optimization for Acid Hydrolysis of Microcrystalline Cellulose and Its Physiochemical Characterization by Using Metal Ion Catalyst
Materials
microcrystalline cellulose
hydrocellulose
response surface methodology
percentage of crystallinity
amorphous sections
title Statistical Optimization for Acid Hydrolysis of Microcrystalline Cellulose and Its Physiochemical Characterization by Using Metal Ion Catalyst
title_full Statistical Optimization for Acid Hydrolysis of Microcrystalline Cellulose and Its Physiochemical Characterization by Using Metal Ion Catalyst
title_fullStr Statistical Optimization for Acid Hydrolysis of Microcrystalline Cellulose and Its Physiochemical Characterization by Using Metal Ion Catalyst
title_full_unstemmed Statistical Optimization for Acid Hydrolysis of Microcrystalline Cellulose and Its Physiochemical Characterization by Using Metal Ion Catalyst
title_short Statistical Optimization for Acid Hydrolysis of Microcrystalline Cellulose and Its Physiochemical Characterization by Using Metal Ion Catalyst
title_sort statistical optimization for acid hydrolysis of microcrystalline cellulose and its physiochemical characterization by using metal ion catalyst
topic microcrystalline cellulose
hydrocellulose
response surface methodology
percentage of crystallinity
amorphous sections
url http://www.mdpi.com/1996-1944/7/10/6982
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AT sharifahbeeabdhamid statisticaloptimizationforacidhydrolysisofmicrocrystallinecelluloseanditsphysiochemicalcharacterizationbyusingmetalioncatalyst
AT mdeaqubali statisticaloptimizationforacidhydrolysisofmicrocrystallinecelluloseanditsphysiochemicalcharacterizationbyusingmetalioncatalyst