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Enhanced crystallinity and thermal properties of cellulose from rice husk using acid hydrolysis treatment

Hafid HS, Omar FN, Zhu J, Wakisaka M

Carbohydr Polym, 2021 May 15;260:117789.
PMID: 33712137 DOI: 10.1016/j.carbpol.2021.117789

Cellulose was extracted from rice husk (RH) using an integrated delignification process using alkaline treatment and acid hydrolysis (concentrated HNO3) for lignocellulosic biomass dissolution. Cellulose yield and quality were assessed through analysis of lignocellulosic content, thermogravimetric, functional group, X-ray diffraction, and surface morphology. HNO3 treatment showed an increment (2.01-fold) in the cellulose content and some enhancement in the crystallinity of cellulose (up to 40.8%). A slight increase was observed in thermal properties from 334.6 °C to 339.3 °C. Economic analysis showed chlorine extraction produce higher cellulose recovery (58%) as compared to HNO3 (26.7%) with the total cost of operation using HNO3 was double compared to chlorine extraction. The economic feasibility of HNO3 can be improved using various progress in the pre-treatment process, chemical recycling and cellulose recovery process since adopting it is crucial for environmental sustainability.
Extraction and surface modification of cellulose fibers and its reinforcement in starch-based film for packaging composites

Hafid HS, Omar FN, Bahrin EK, Wakisaka M

Bioresour Bioprocess, 2023 Jan 25;10(1):7.
PMID: 38647891 DOI: 10.1186/s40643-023-00631-w

BACKGROUND: Cellulose extraction from gloss art paper (GAP) waste is a recycling strategy for the abundance of gloss art paper waste. Here, a study was conducted on the impact of ultrasonic homogenization for cellulose extraction from GAP waste to improve the particle size, crystallinity, and thermal stability.
RESULTS: At treatment temperature of 75.8 °C, ultrasonic power level of 70.3% and 1.4 h duration, cellulose with properties of 516.4 nm particle size, 71.5% crystallinity, and thermal stability of 355.2 °C were extracted. Surface modification of cellulose GAP waste with H3PO4 hydrolysis and 2,2,6,6-tetramethylpiperidine-1-oxyl radical (TEMPO) oxidation was done followed by starch reinforcement. Surface hydrophobicity and mechanical strength were increased for H3PO4 hydrolysis and TEMPO oxidation starch-cellulose. No reduction of thermal properties observed during the treatment, while increment of crystallinity index up to 47.65-59.6% was shown. Neat starch film was more transparent, followed by starch-TEMPO film and starch-H3PO4 film, due to better homogeneity.
CONCLUSIONS: The cellulose GAP reinforced starch film shows potential in developing packaging materials and simultaneously provide an alternative solution of GAP waste recycling.
Micromechanical modelling of oil palm empty fruit bunch fibres containing silica bodies

Omar FN, Hanipah SH, Xiang LY, Mohammed MAP, Baharuddin AS, Abdullah J

J Mech Behav Biomed Mater, 2016 09;62:106-118.
PMID: 27183430 DOI: 10.1016/j.jmbbm.2016.04.043

Experimental and numerical investigation was conducted to study the micromechanics of oil palm empty fruit bunch fibres containing silica bodies. The finite viscoelastic-plastic material model called Parallel Rheological Network model was proposed, that fitted well with cyclic and stress relaxation tensile tests of the fibres. Representative volume element and microstructure models were developed using finite element method, where the models information was obtained from microscopy and X-ray micro-tomography analyses. Simulation results showed that difference of the fibres model with silica bodies and those without ones is larger under shear than compression and tension. However, in comparison to geometrical effect (i.e. silica bodies), it is suggested that ultrastructure components of the fibres (modelled using finite viscoelastic-plastic model) is responsible for the complex mechanical behaviour of oil palm fibres. This can be due to cellulose, hemicellulose and lignin components and the interface behaviour, as reported on other lignocellulosic materials.
Oil palm fiber biodegradation: physico-chemical and structural relationships

Omar FN, Hafid HS, Samsu Baharuddin A, Mohammed MAP, Abdullah J

Planta, 2017 Sep;246(3):567-577.
PMID: 28620814 DOI: 10.1007/s00425-017-2717-5

MAIN CONCLUSION: X-ray microtomography results revealed that delignification process damaged the oil palm fibers, which correlated well with reduction of lignin components and increase of the phenolic content. Biodegradation investigation of natural fibers normally focuses on physico-chemical analysis, with less emphasis on physical aspect like fiber structures affect from microbial activity. In this work, the performance of Pycnoporus sanguineus to delignify oil palm empty fruit bunch fibers through solid-state fermentation utilizing various ratio of POME sludge was reported. In addition to tensile testing, physico-chemical and X-ray microtomography (µ-CT) analyses on the oil palm fibers were conducted to determine the effectiveness of the degradation process. The best ratio of fiber to fungi (60:40) was chosen based on the highest lignin loss and total phenolic content values and further investigation was performed to obtain fermentation kinetics data of both laccase and manganese peroxidase. µ-CT results revealed that delignification process damaged the pre-treated and untreated fibers structure, as evident from volume reduction after degradation process. This is correlated with reduction of lignin component and increase of the phenolic content, as well as lower stress-strain curves of the pre-treated fibers compared to the untreated ones (from tensile testing). It is suggested that P. sanguineus preferred to consume the outer layer of the fiber, before it penetrates through the cellular structure of the inner fiber.