In this study cellulose nanocrystals were isolated from oil palm trunk (Elaeis guineensis) using acid hydrolysis method. The morphology and size of the nanocrystals were characterized using scanning electron microscopy and transmission electron microscopy. The results showed that the nanocrystals isolated from raw oil palm trunk (OPT) fibers and hot water treated OPT fibers had an average diameter of 7.67 nm and 7.97 nm and length of 397.03 nm and 361.70 nm, respectively. Fourier Transform Infrared spectroscopy indicated that lignin and hemicellulose contents decreased. It seems that lignin was completely removed from the samples during chemical treatment. Thermogravimetric analysis demonstrated that cellulose nanocrystals after acid hydrolysis had higher thermal stability compared to the raw and hot water treated OPT fibers. The X-ray diffraction analysis increased crystallinity of the samples due to chemical treatment. The crystalline nature of the isolated nanocrystals from raw and hot water treated OPT ranged from 68 to 70%.
Previously, studies have demonstrated that topical application of simvastatin can promote wound healing in diabetic mice via augmentation of angiogenesis and lymphangiogenesis. This study aimed to formulate and characterize simvastatin in alginate-based composite film wound dressings. Biopolymers used for composite films were sodium alginate blended with pectin or gelatin. The films were prepared and characterized based on their physical properties, surface morphology, mechanical strength and rheology. Then, in vitro drug releases from the films were investigated and, finally, the cell viability assay was performed to assess the cytotoxicity profile. From the pre-formulation studies, alginate/pectin composite film showed to possess desirable wound dressing properties and superior mechanical properties. The in vitro drug release profile revealed that alginate/pectin film produced a controlled release drug profile, and cell viability assay showed that the film was non-toxic. In summary, alginate/pectin composite film is suitable to be formulated with simvastatin as a potential wound dressing.
The hydrothermal pretreatment on kenaf core pulp (KCP) was carried out using an autoclave heated in a oil bath at 140°C for 0.5/1/3/5h. The hydrothermal pretreated kenaf (HPK) was dissolved in a LiOH/urea aqueous solution and subsequently used to produce cellulose membrane and hydrogel. The effects of hydrothermal pretreatment time on solubility, viscosity, crystallinity and morphology of the cellulose membrane and hydrogel were investigated. The hydrothermal pretreatment leads to higher cellulose solubility and higher viscosity of the cellulose solution. The formation of cellulose II and crystallinity index of the cellulose membrane and hydrogel were examined by X-ray diffraction (XRD). The pore size of the cellulose membrane and hydrogel displayed an upward trend with respect to the hydrothermal pretreatment period observed under a field emission scanning electron microscope (FESEM). This finding provides an efficient procedure to improve the solubility, viscosity and properties of regenerated cellulose products.
Bleached kenaf core pulps (BKC) were hydrolyzed in H2SO4 (0.5M) at different time (0min to 90min) at room temperature. After the hydrolysis process, the viscosity average molecular weight (Mŋ) for BKC sample has reduced from 14.5×10(4) to 2.55×10(4). The hydrolyzed BKC was then dissolved in NaOH:urea:water and in LiOH:urea:water mixed solvent at the ratio of 7:12:81 and 4.6:15:80.4, respectively. The increased in hydrolysis time has decreased Mŋ of cellulose leading to easy dissolution process. Higher porosity and transparency with lower crystallinity index (CrI) of regenerated membrane produced can be achieved as the Mŋ reduced. The properties of membrane were observed through FESEM, UV-vis spectrophotometer and XRD. This study has proven that acid hydrolysis has reduced the Mŋ of cellulose, thus, enhanced the properties of regenerated membrane produced with assisted by alkaline/urea system.
Chitosan nanoparticles (CNP) were synthesized via ionic gelation and used for the preparation of starch-based nanocomposite films containing different concentration of CNP (0, 5, 10, 15, 20% w/w). Antimicrobial properties of starch/CNP films was evaluated via in vitro (disc diffusion analysis) and in vivo (microbial count in wrapped cherry tomatoes) study. It was found that inhibitory zone of the 15 and 20% of starch/CNP films were clearly observed for all the tested bacteria including Bacillus cereus, Staphylococcus aureus, Escherichia coli and Salmonella typhimurium. In vivo study revealed that the starch/CNP film (15% w/w) was more efficient to inhibit the microbial growth in cherry tomatoes (7 × 102 CFU/g) compared to neat starch film (2.15 × 103 CFU/g) thus confirmed the potential application of the films as antimicrobial food packaging.
Photocatalytic oxidation of crosslinked chitosan-epichlorohydrin (CS-ECH) film was successfully achieved via an immobilized TiO2/CS-ECH photocatalyst system on a glass plate. Oxidation process of CS-ECH film was carried out by irradiating the system with a 45-W fluorescent lamp for 10h in ultra-pure water. The results indicate the formation of carbonyl functional groups and partial elimination of amine groups in the molecular structure of the oxidized CS-ECH film. This oxidized CS-ECH film has different optical properties, ionic conductivity, degree of transparency, swelling index and chemical stability than the fresh CS-ECH film. In the environmental applications, the TiO2/oxidized-CS-ECH photocatalyst system can have photodegradation and faster mineralization rate of phenol than both fresh TiO2/CS-ECH and TiO2/oxidized-CS photocatalyst systems. This simple photocatalyst system, therefore can be considered as an environmental friendly method to oxidize synthetic biopolymer and to improve the photocatalytic efficiency of TiO2 to treat wastewater.
In this study cellulose nanocrystals were isolated through acid hydrolysis process from parenchyma and vascular bundle of oil palm trunk (Elaeis guineensis). The morphological properties of obtained cellulose nanocrystals were studied by scanning electron microscopy (SEM) and transmission electron microscopy (TEM). The microscopy images showed smoother and cleaner surface of parenchyma cellulose nanocrystals when compared to vascular bundle cellulose nanocrystals. The TEM image shows a higher length and diameter for parenchyma cellulose nanocrystals compared to vascular bundle cellulose nanocrystals. The Fourier transform infrared (FTIR) spectra showed changes in functional groups after acid hydrolysis due to removal of lignin, hemicelluloses and other impurities in both type of cellulose nanocrystals. Crystallinity index of cellulose nanocrystals was observed higher for vascular bundle as compared to parenchyma. Thermogravimetric analysis (TGA) was performed to study the thermal stability of cellulose nanocrystals and it was observed higher for parenchyma cellulose nanocrystals compared to vascular bundle.
Recently, surface functionality and thermal property of the green nanomaterials have received wide attention in numerous applications. In this study, microcrystalline cellulose (MCC) was used to prepare the nanocrystalline celluloses (NCCs) using acid hydrolysis method. The NCCs was treated with TEMPO [(2,2,6,6-tetramethylpiperidin-1-yl)oxy radical]-oxidation to prepare TEMPO-oxidized NCCs. Cellulose nanofibrils (CNFs) also prepared from MCC using TEMPO-oxidation. The effects of rapid cooling and chemical treatments on the thermo-structural property studies of the prepared nanocelluloses were investigated through FTIR, thermogravimetric analysis-derivative thermogravimetric (TGA-DTG), and XRD. A posteriori knowledge of the FTIR and TGA-DTG analysis revealed that the rapid cooling treatment enhanced the hydrogen bond energy and thermal stability of the TEMPO-oxidized NCC compared to other nanocelluloses. XRD analysis exhibits the effect of rapid cooling on pseudo 2Ihelical conformation. This was the first investigation performed on the effect of rapid cooling on structural properties of the nanocellulose.
Catalytic ionic liquid hydrolysis of cellulosic material have been considered as a green and highly efficient dissolution process. However, application of a pre-treatment process, i.e; ultrasonication enhances the hydrolysis of cellulose in ionic liquid by providing mechanical force. In this paper, we describe the impact of both chemical and mechanical approaches to produce nanocrytalline cellulose (NCC) with anticipated particle size, and crystallinity with improved yields. The ultrasonication treatment was evaluated in terms of treatment time and vibration amplitude. It was found that the lowest ultrasonication time (5 min) produced the NCC of highest crystallinity (73 %), but the lowest yield (84 %). In contrary, the highest ultrasonication vibration amplitude at 90 % produced NCC with highest crystallinity value (67 %) as well as yields (90 %). It concludes that ultrasonic pre-treatment improves the hydrolysis process of cellulose in ionic liquid with increasing yield and crystallinity of NCC.
In the present research work, dicationic ionic liquids, containing 1,4-bis(3-methylimidazolium-1-yl) butane ([C4(Mim)2]) cation with counter anions [(2HSO4)(H2SO4)0], [(2HSO4)(H2SO4)2] and [(2HSO4)(H2SO4)4] were synthesised. ILs structures were confirmed using 1H NMR spectroscopy. Thermal stability, Hammett acidity, density and viscosity of ILs were determined. Various types of lignocellulosic biomass such as rubber wood, palm oil frond, bamboo and rice husk were converted into levulinic acid (LA). Among the synthesized ionic liquids, [C4(Mim)2][(2HSO4)(H2SO4)4] showed higher % yield of LA up to 47.52 from bamboo biomass at 110°C for 60min, which is the better yield at low temperature and short time compared to previous reports. Surface morphology, surface functional groups and thermal stability of bamboo before and after conversion into LA were studied using SEM, FTIR and TGA analysis, respectively. This one-pot production of LA from agro-waste will open new opportunity for the conversion of sustainable biomass resources into valuable chemicals.
The aim of this research was to enhance the survivability of Lactobacillus rhamnosus NRRL 442 against heat exposure via a combination of immobilization and microencapsulation processes using sugarcane bagasse (SB) and sodium alginate (NaA), respectively. The microcapsules were synthesized using different alginate concentration of 1, 2 and 3% and NaA:SB ratio of 1:0, 1:1 and 1:1.5. This beneficial step of probiotic immobilization before microencapsulation significantly enhanced microencapsulation efficiency and cell survivability after heat exposure of 90°C for 30s. Interestingly, the microcapsule of SB-immobilized probiotic could obtain protection from heat using microencapsulation of NaA concentration as low as 1%. SEM images illustrated the incorporation of immobilized L. rhamnosus within alginate matrices and its changes after heat exposure. FTIR spectra confirmed the change in functional bonding in the presence of sugarcane bagasse, probiotic and alginate. The results demonstrated a great potential in the synthesis of heat resistant microcapsules for probiotic.
In this article, silver and magnetite nanofillers were synthesized in modified κ-carrageenan hydrogels using the in situ method. The effect of metallic nanoparticles in gastro-intestinal tract (GIT) release of a model drug (methylene blue) has been investigated. The effect of nanoparticles loading and genipin cross-linking on GIT release of nanocomposite is also studied to finally provide the most suitable drug carrier system. In vitro release studies revealed that using metallic nanocomposites hydrogels in GIT studies can improve the drug release in intestine and minimize it in the stomach. It was found that cross-linking and nanofiller loading can significantly improve the targeted release. Therefore, applying metallic nanoparticles seems to be a promising strategy to develop GIT controlled drug delivery.
Polymer electrolytes were developed by solution casting technique utilizing the materials of cellulose acetate (CA), lithium bis(trifluoromethanesulfonyl)imide (LiTFSI) and deep eutectic solvent (DES). The DES is synthesized from the mixture of choline chloride and urea of 1:2 ratios. The increasing DES content well plasticizes the CA:LiTFSI:DES matrix and gradually improves the ionic conductivity and chemical integrity. The highest conducting sample was identified for the composition of CA:LiTFSI:DES (28 wt.%:12 wt.%:60 wt.%), which has the greatest ability to retain the room temperature ionic conductivity over the entire 30 days of storage time. The changes in FTIR cage peaks upon varying the DES content in CA:LiTFSI:DES prove the complexation. This complexation results in the collapse of CA matrix crystallinity, observed from the reduced intensity of XRD diffraction peaks. The DES-plasticized sample is found to be more heat-stable compared to pure CA. Nevertheless, the addition of DES diminishes the CA:LiTFSI matrix's heat-resistivity but at the minimum addition the thermal stability is enhanced.
A series of polymer electrolytes composed of corn starch (CS), lithium bis(trifluoromethanesulfonyl)imide (LITFSI) and deep eutectic solvent (DES) were fabricated by solution casting technique. The DES was synthesized from a mixture of choline chloride and urea at a molar ratio of 1:2. The addition of DES is crucial in enhancing the room temperature ionic conductivity by increasing the amorphous elastomeric phase in CS:LITFSI matrix. The ionic transport mechanism is improved and appreciable amount of ion conducting polymer electrolytes is produced. The highest ionic conductivity achieved for the polymer electrolyte composition CS:LiTFSI:DES (14wt.%:6wt.%:80wt.%) is 1.04×10-3Scm-1. The anomalies that were observed with the addition of DES upon formation of neutral ion multiples were visually revealed by the SEM micrographs. The possible dipole-dipole interaction between the constituents was visualized by the FTIR spectroscopy upon change in cage peaks.
In this study, a novel fibrous membrane of hydroxyethyl cellulose (HEC)/poly(vinyl alcohol) blend was successfully fabricated by electrospinning technique and characterized. The concentration of HEC (5%) with PVA (15%) was optimized, blended in different ratios (30-50%) and electrospun to get smooth nanofibers. Nanofibrous membranes were made water insoluble by chemically cross-linking by glutaraldehyde and used as scaffolds for the skin tissue engineering. The microstructure, morphology, mechanical and thermal properties of the blended HEC/PVA nanofibrous scaffolds were characterized by scanning electron microscope, Fourier transform infrared spectroscopy, differential scanning colorimetry, universal testing machine and thermogravimetric analysis. Cytotoxicity studies on these nanofibrous scaffolds were carried out using human melanoma cells by the MTT assays. The cells were able to attach and spread in the nanofibrous scaffolds as shown by the SEM images. These preliminary results show that these nanofibrous scaffolds that supports cell adhesion and proliferation is promising for skin tissue engineering.
This research involves the rare utilisation of the kapok fibre (Ceiba pentandra) as a raw material for the fabrication of cellulose nanocrystal (CNC) and self-assembled CNC membranes. The isolation of CNC from Ceiba pentandra began with the extraction of cellulose via the chemical alkali extraction by using 5wt% NaOH, followed by the typical acidified bleaching method and, finally, the CNC production through acid hydrolysis with 60wt% H2SO4 at the optimum time of 60min. The prepared CNC was then employed for the preparation of self-assembled membrane through the water suspension casting evaporation technique. The obtained CNC membrane was characterised in terms of its composition, crystallinity, thermal stability, as well as, structural and morphological features with the use of several techniques including FTIR, XRD, AFM, TEM, FESEM, and TGA. The FESEM and AFM analyses had illustrated the achievement of a self-assembled CNC membrane with a smooth surface and a well-distributed nano-porous structure, with the porosity of 52.82±7.79%. In addition, the findings proved that the self-assembled CNC membrane displayed good adsorption capability indicated by the recorded efficiency of 79% and 85% for 10mg/L and 5mg/L of methylene blue in an aqueous solution, respectively.
Graft copolymerisation of methyl methacrylate (MMA) onto Agave angustifolia was conducted with ceric ammonium nitrate (CAN) as the redox initiator. The maximum grafting efficiency was observed at CAN and MMA concentrations of 0.91 × 10(-3) and 5.63 × 10(-2)M, respectively, at 45°C for 3h reaction time. Four characteristic peaks at 2995, 1738, 1440, and 845 cm(-1), attributed to PMMA, were found in the IR spectrum of grafted cellulose. The crystallinity index dropped from 0.74 to 0.46, while the thermal stability improved upon grafting. The water contact angle increased with grafting yield, indicating increased hydrophobicity of cellulose. SEM images showed the grafted cellulose to be enlarged and rougher. The changes in the physical nature of PMMA-grafted cellulose can be attributed to the PMMA grafting in the amorphous regions of cellulose, causing it to expand at the expense of the crystalline component.
The aim of the present study was to investigate the effects of different purification and drying methods on the viscoelastic behaviour and rheological properties of durian seed gum. The results indicated that the purified gum A (using isopropanol and ethanol) and D (using hydrochloric acid and ethanol) showed the highest and lowest viscosity, respectively. Four drying techniques included oven drying (105 °C), freeze drying, spray drying and vacuum oven drying. In the present work, all purified gums exhibited more elastic (gel-like) behaviour than the viscous (liquid-like) behaviour (G″
The enhancement of lignocellulose hydrolysis using enzyme complexes requires an efficient pretreatment process to obtain susceptible conditions for the enzyme attack. This study focuses on removing a major part of the lignin layer from kenaf (Hibiscus cannabinus) while simultaneously maintaining most of the hemicellulose. A two-stage pretreatment process is adopted using calcium hydroxide, Ca(OH)₂, and peracetic acid, PPA, to break the recalcitrant lignin layer from other structural polysaccharides. An experimental screening of several pretreatment chemicals, concentrations, temperatures and solid-liquid ratios enabled the production of an optimally designed pretreatment process for kenaf. Our results showed that the pretreatment process has provide 59.25% lignin removal while maintaining 87.72% and 96.17% hemicellulose and cellulose, respectively, using 1g of Ca(OH)₂/L and a 8:1 (mL:g) ratio of liquid-Ca(OH)₂ at 50 °C for 1.5 h followed by 20% peracetic acid pretreatment at 75 °C for 2 h. These results validate this mild approach for aiding future enzymatic hydrolysis.
This work reports on a complete isolation and characterization of lignocellulosic compounds from oil palm empty fruit bunch (OPEFB) by ionic liquid (IL) treatment and alkaline treatment processes. The fractionated lignocellulosic compounds were confirmed by FTIR and CP/MAS 13CNMR analyses. The yield of the cellulose, hemicellulose and lignin fractions was 52.72±1.50% wt., 27.17±1.68% wt. and 16.82±1.15% wt. with molecular weight of 1869g/mol, 1736g/mol and 2695g/mol, and degradation temperature of 325.65°C, 236.25°C, and 201.40°C, respectively. The SEM image illustrates the bundle-like fiber of cellulose fraction and smaller particle size of hemicellulose and lignin fractions with inconsistent shape. The XRD patterns depict the crystalline cellulose, amorphous lignin and partially amorphous hemicellulose fractions property. The IL could be recovered and reused with an overall recovery of 48% wt. after the fourth cycle.