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.
The main aim of this study was to investigate the effect of different coating materials (i.e. Na-alginate and chitosan) on the viability and release behavior of Bifidobacterium pseudocatenulatum G4 in the simulated gastric fluid (SGF) and simulated intestinal fluid (SIF). This study reports the viability of encapsulated B. pseudocatenulatum G4 coated using different alginate (2-4 g/100mL) and chitosan (0.2-0.8 g/100mL) concentrations. The results indicated that the highest concentration of alginate (4.4142 g/100mL) along with 0.5578 g/100mL chitosan resulted in the highest viability of B. pseudocatenulatum G4. The release behavior of the encapsulated probiotics in SGF (pH 1.5) in 2h followed by 4h in SIF (pH 7.4) was also assessed. The resistance rate of alginate-chitosan capsule in SGF was higher than SIF. The alginate-chitosan encapsulated cells had also more resistance than alginate capsules. The current study revealed that alginate encapsulated B. Pseudocatenulatum G4 exhibited longer survival than its free cells (control).
The aim of the present research work has focused on investigating the effect of cellulose nanofibers (CNFs) and nano clays (montmorillonite (MMT) & organoclay (OMMT)) at 0.75Wt % on the performance of kenaf/epoxy composites. Mechanical (tensile and flexural) and thermal properties of composites in terms of morphology, thermal stability, weight loss, and dynamic mechanical properties were analyzed. The obtained results revealed that the integration of stiff CNFs as filler enhanced the mechanical and thermal properties, storage and loss modulus while a considerable decrease in Tan δ was realized compared to kenaf/epoxy composites. Enhancement in the properties was observed for OMMT and CNFs composites compared to MMT/kenaf/epoxy composites, which is attributed to the uniform filler distribution and interfacial adhesion between CNFs, OMMT, kenaf and epoxy matrix. The obtained results revealed that OMMT and CNFs based kenaf/epoxy composites can be an efficient alternative for construction applications.
In this study, effect of degree of deacetylation on property and adsorption capacity of chitosan/polyvinyl Alcohol electrospun membrane has been investigated. Resulting nanofibers were characterized by FESEM, FTIR, XRD, TGA, tensile testing, weight loss test and adsorption test. FESEM result shows, finer nanofiber was fabricated from 42h hydrolyzed chitosan and PVA blend solution. FTIR and XRD result showed a strong interaction between chitosan and polyvinyl alcohol. Higher tensile strength was observed for the nanofiber having 42h hydrolyzed chitosan. Blend solution of chitosan/PVA having low DD chitosan had higher viscosity. The nanofibrous membrane was stable in distilled water, acidic and basic medium. The isotherm study shows that the adsorption capacity (qm) of nanofiber containing higher DD chitosan was higher for Cr(VI). In contrary, the membrane containing chitosan with lower DD showed the higher adsorption capacity for Fe(III) and methyl orange. Moreover, the effect of DD on removal percentage of adsorbate was dependent on the initial concentration of the adsorbate.
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.
Carboxymethyl starch (CMS) was produced from sago starch via carboxymethylation. The CMS with different degree of substitution (DS) ranges from 0.4 to 0.8 were mixed with polyethylene glycol (PEG) of different molecular weight and distilled water and the hydrogel was cured by electron beam irradiation with doses ranging from 25 to 35 kGy. The results revealed that CMS-PEG hydrogels with DS 0.4 give the optimum gel content when radiated at 30 kGy and with PEG 600. Thermogravimetric analysis (TGA) revealed that there are two phases exist in CMS with DS 0.4 in contrast to the three steps decomposition occurs in DS 0.6 and 0.8. It shows that the CMS with DS 0.4 is more thermally stable. Surface morphology revealed crosslinking among the blends when subjected into the radiation dose. The study shows both radiation and PEG addition improved most of the properties of CMS irrespective of the DS value.
This article presents an analysis of the influence of heat treatment on chitosan nanocomposite film. A series of samples comprising: pure chitosan film, chitosan film embedded with nanocrystalline cellulose (NCC), chitosan film crosslinked with tannic acid and chitosan film with a blend of NCC and tannic acid were heat treated using a convection oven. Fourier-transform-infrared spectroscopy (FTIR) and X-ray diffraction test (XRD) shows the changes in chemical interaction of the heat treated films. The heat treated films show significant improvements in moisture absorption. Tensile strength and Young's Modulus were increased up to 7MPa and 259MPa, respectively when the samples were subjected to heat treatment. For the NCC particles, a transmission electron microscope (TEM) was used to inspect the structural properties of cellulose particle in suspension form.
Composite sago starch-based system was developed and characterized with the aim to find an alternative to gelatin in the processing of pharmaceutical capsules. Dually modified (Hydrolyzed-Hydroxypropylated) sago starches were combined with κ-carrageenan (0.25, 0.5, 0.75, and 1%). The rheological properties of the proposed composite system were measured and compared with gelatin as reference material. Results show that combination of HHSS12 (Hydrolysed-hydroxypropylated sago starch at 12h) with 0.5% κ-carrageenan was comparable to gelatin rheological behavior in pharmaceutical capsule processing. The solution viscosity at 50 °C and sol-gel transition of the proposed composite system were comparable to those of gelatin. The viscoelastic moduli (G' and G") for the proposed system were lower than those of gelatin. These results illustrate that by manipulation of the constituents of sago starch-based composite system, a suitable alternative to gelatin can be produced with comparable properties and this could find potential application in pharmaceutical capsule industry.
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 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.
Cross-linked enzyme aggregates (CLEAs) are influenced by mass diffusion limitations such as the degree of molecular cross-linking attained, which affects substrate accessibility. Thus, this study seeks to improve substrate accessibility using macromolecular cross-linkers in cross-linked levanase aggregates (CLLAs) formation for levan-type fructooligosaccharides (L-FOS) production. Dialdehyde starch-tapioca (DAST) was successfully developed and used to cross-link levanase to form CLLAs-D and with bovine serum albumin (BSA) to form CLLAs-DB which showed activity recoveries of 65.6% and 81.6%, respectively. After cross-linking, the pH (6-10) and thermal stability (30-40 °C) increased, and organic solvent tolerance resulted in the activation of CLLAs. Likewise, CLLAs-DB had higher substrate affinity and accessibility and a higher effectiveness factors than CLLAs-D. The total L-FOS yield of CLLAs-DB (78.9% (w/v)) was higher than that of CLLAs-D (62.4% (w/v)). Therefore, as a cross-linker, DAST may have application prospects as a promising and green biocatalyst for product formation.
Biopolymer electrolytes containing corn starch, lithium hexafluorophosphate (LiPF6) and ionic liquid, 1-butyl-3-methylimidazolium hexafluorophosphate (BmImPF6) are prepared by solution casting technique. Temperature dependence-ionic conductivity studies reveal Vogel-Tamman-Fulcher (VTF) relationship which is associated with free volume theory. Ionic liquid-based biopolymer electrolytes show lower glass transition temperature (Tg) than ionic liquid-free biopolymer electrolyte. X-ray diffraction (XRD) studies demonstrate higher amorphous region of ionic liquid-added biopolymer electrolytes. In addition, the potential stability window of the biopolymer electrolyte becomes wider and stable up to 2.9V. Conclusively, the fabricated electric double layer capacitor (EDLC) shows improved electrochemical performance upon addition of ionic liquid into the biopolymer electrolyte. The specific capacitance of EDLC based on ionic liquid-added polymer electrolyte is relatively higher than that of ionic liquid-free polymer electrolyte as depicted in cyclic voltammogram.
The effect of incorporating common dodecyl anionic and cationic surfactants such as dodecyltrimethylammonium bromide (DTAB), dodecylethyldimethylammonium bromide (DDAB), and sodium dodecylsulfate (SDS) in nanocomposites of reduced graphene oxide and nanocellulose are described. The stabilization and electrical properties of the nanocomoposites of reduced graphene oxide (RGO) and nanofibrillated kenaf cellulose (NFC) were characterized using four-point probe electrical conductivity measurements. Raman spectroscopy, field emission scanning electron microscopy, and high-resolution transmission electron microscopy were used to investigate dispersion morphology and the quality of RGO inside the NFC matrices. Small-angle neutron scattering (SANS) was used to study the aggregation behavior of the aqueous surfactant systems and RGO dispersions. The cationic surfactant DTAB proved to be the best choice for stabilization of RGO in NFC, giving enhanced electrical conductivity five orders of magnitude higher than the neat NFC. The results highlight the effects of hydrophilic surfactant moieties on the structure, stability and properties of RGO/NFC composites.
Supercapacitor electrode based on conducting polymer of poly (3,4-ethylenedioxythipohene) (PEDOT) doped with nanocrystalline cellulose (NCC) films were prepared via electrochemical polymerization technique. Different applied potential, concentration and deposition time were varied to study the effect of electropolymerization potential, NCC concentration and deposition time on the formation of PEDOT/NCC film. The formation of electrochemically polymerized PEDOT/NCC composite was successfully proven with field emission scanning electron microscope (FESEM) and Fourier transform infrared spectroscopy (FTIR) techniques where the composites exhibited an interconnected network-like surface morphology. PEDOT/NCC deposited at 1.2 V in 1 mg/ml of NCC for 15 min showed the highest specific capacitance of 117.02 F/g at 100 mV/s with energy density and power density of 11.44 Wh/kg and 99.85 W/kg, respectively at the current density of 0.2 A/g. The incorporation of NCC into PEDOT revealed a lower resistance of charge transfers and improves the cycling stability by retaining 86% of capacitance after 1000 cycles.
The adsorption behavior of chitosan (CS) beads modified with 3-aminopropyl triethoxysilane (APTES) for the removal of reactive blue 4 (RB4) in batch studies has been investigated. The effects of modification conditions, such as the APTES concentration, temperature and reaction time on RB4 removal, were studied. The adsorbent prepared at a concentration of 2 wt% APTES for 8h at 50 °C was the most effective one for RB4 adsorption. The adsorption capacity of modified CS beads (433.77 mg/g) was 1.37 times higher than that of unmodified CS beads (317.23 mg/g). The isotherm data are adequately described by a Freundlich model, and the kinetic study revealed that the pseudo-second-order rate model was in better agreement with the experimental data. The negative values of the thermodynamic parameters, including ΔG° (-2.28 and -4.70 kJ/mol at 30 ± 2 °C), ΔH° (-172.18 and -43.82 kJ/mol) and ΔS° (-560.71 and -129.08 J/mol K) for CS beads and APTES modified beads, respectively, suggest that RB4 adsorption is a spontaneous and exothermic process.
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.
Cellulose carbamate (CC) was synthesized via hydrothermal process and mixed with graphene oxide (GO) to form a homogeneous cellulose matrix nanocomposite films. The properties of CC/GO nanocomposite films fabricated using simple solution-mixing method with different GO loadings were studied. Transmission electron microscope analysis showed the exfoliation of self-synthesized GO nanosheets within the CC matrix. X-ray diffraction results confirmed the crystalline structure of CC/GO films as the CC/GO mass ratio increased from 100/0 to 100/4. The mechanical properties of CC/GO film were significantly improved as compared to neat CC film. From thermogravimetric analysis result, the introduction of GO enhanced the thermal stability and carbon yields. The 3D homogeneous porous structures of the CC/GO films were observed under Field emission scanning electron microscope. These improvements in nanocomposite film properties could be confirmed by Fourier transform infrared spectroscopy due to the strong and good interactions between CC and GO.
Erlotinib-loaded carboxymethyl temarind gum-g-poly(N-isopropylacrylamide)-montmorillonite based semi-IPN nanocomposites were synthesized and characterized for their in vitro performances for lung cancer therapy. The placebo matrices exhibited outstanding biodegradability and pH-dependent swelling profiles. The molar mass (M¯ c) between the crosslinks of these composites was declined with temperature. The solid state characterization confirmed the semi-IPN architecture of these scaffolds. The corresponding drug-loaded formulations displayed excellent drug-trapping capacity (DEE, 86-97 %) with acceptable zeta potential (-16 to -13 mV) and diameter (967-646 nm). These formulations conferred sustained drug elution profiles (Q8h, 77-99 %) with an initial burst release. The drug release profile of the optimized formulation (F-3) was best fitted in the first order kinetic model with Fickian diffusion driven mechanism. The mucin adsorption to F-3 followed Langmuir isotherms. The results of MTT assay, AO/EB staining and confocal analyses revealed that the ERL-loaded formulation suppressed A549 cell proliferation and induced apoptosis more effectively than pristine drug.
Floating hydrogels were prepared from kappa carrageenan containing CaCO3 and NaHCO3 as pore forming agents. The effects of CaCO3 and NaHCO3 on hydrogel characterizations were investigated and compared. Amoxicillin trihydrate was used as a model drug. Characterizations of the hydrogels were carried out using Fourier transform infrared spectroscopy (FTIR), X-ray diffraction (XRD) and field emission scanning electron microscope (FESEM). As pore forming agents concentration increases, the porosity (%) and floating properties increased. NaHCO3 incorporated hydrogels showed higher porosity with shorter floating lag time (FLT) than CaCO3. Hydrogel which contained CaCO3 exhibited better gel stability over the control and NaHCO3 containing gel. Incorporation of CaCO3 into kappa carrageenan hydrogel showed smoother surface gels compared to those produced with NaHCO3. CaCO3 also showed higher drug entrapment efficiency and sustained drug release profile than NaHCO3. The results of these studies showed that, CaCO3 is an effective pore forming agents in κC hydrogels preparation as compare to NaHCO3. Thus, CaCO3 can be an excellent pore forming agent for an effective floating drug delivery system.
We developed tricalcium phosphate-chitosan-fucoidan biocomposite scaffold (TCP-Ch-Fu) by using the freeze-drying technique. The fabricated biocomposite scaffolds were analyzed by spectroscopy and porosity measurement. The biomechanical properties of scaffolds were assessed by compression test and the results suggested that the incorporation of Fucoidan into the biocomposite improves the compression strength of scaffolds. Biomineralization of scaffolds was evaluated by soaking them in simulated body fluid and the results revealed that the addition of Fucoidan into the scaffolds enhanced the formation of apatite layer on the surface of biocomposite after 7 days of immersion. Alamar Blue assay confirmed that the cell viability of human-derived bone marrow stromal cell was superior in the TCP-Ch-Fuscaffold. The addition of Fucoidan to TCP-Ch increased the release of osteocalcin, confirming that it can support osteogenic differentiation of human mesenchymal stromal cells in in vitro culture. Thus, TCP-Ch-Fu could be a potential candidate for bone-tissue engineering applications.