Oil palm frond-derived cellulose nanocrystals: Effect of pretreatment and elucidating its reinforcing potential in hydrogel beads.

Herein, cellulose nanocrystals were synthesized from oil palm fronds (CNC-OPF) involving two pretreatment approaches, viz. autohydrolysis and soda pulping. The pretreatments were applied individually to OPF fibers to assess their influence on CNCs' physicochemical and thermal properties. CNC-OPF samples were assessed using complementary characterization techniques, which confirmed their purity and characteristics. CP/MAS 13C NMR and TEM studies revealed that autohydrolysis pretreatment yielded CNCs with effective hemicellulose and extractives removal compared to that of soda pulping. XRD analysis demonstrated that autohydrolysis-treated CNC-OPF contained a much higher crystallinity index compared to soda pulping treatment. BET measurement disclosed a relatively higher surface area and wider pore diameter of autohydrolysis-treated CNC-OPF. Autohydrolysis-treated CNCs were applied as a reinforcement filler in alginate-based hydrogel beads for the removal of 4-chlorophenol from water, which attained a qmax of 19.168 mg g-1. BET analysis revealed the less porous nature of CNC-ALG hydrogel beads which could have contributed to hydrogel beads' relatively lower adsorption capacity. The point of zero charge of CNC-ALG hydrogel beads was 4.82, suggesting their applicability only within a short solution pH range. This study directs future studies to unveil the possibilities of functionalizing CNCs in order to enhance the adsorption performance of CNC-immobilized hydrogel beads towards 4-chlorophenol and other organic contaminants.

Conversion of archeological iron rust employing coconut husk lignin.

Rust powder collected from an archeological iron was evaluated by complementary analyses such as FTIR, XRD, XRF, and SEM/EDX. The analyses revealed that lepidocrocite (L) was the major component in the archeological iron. Coconut husk (CH) can be classified as a type of lignocellulosic biomass of renewable resources that are widely available, especially in coastal areas. In this research, the isolated lignin extracted from CH is being studied as a potential alternative for environmentally friendly applications. The isolated lignin from soda and organosolv pulping went through several analyses such as FTIR, NMR (13C and 2D-HSQC), and TGA analyses. The analyses showed that lignin isolated via soda pulping has superior antioxidant capabilities due to its greater phenolic-OH content compared to lignin isolated from organosolv pulping. The effects of lignin concentrations, pH, and reaction time were utilized in rust conversion studies of an archeological iron. 5 wt% of soda lignin (SL) was revealed as the ideal condition in this rust conversion study with a value of 84.21 %. The treated rust powder with 5 wt% of SL was then further gone through several complementary analyses, which revealed that the treated rust had nearly transformed into an amorphous state.

Preparation and characterization of nanosized lignin from oil palm (Elaeis guineensis) biomass as a novel emulsifying agent.

A study was carried out to determine the effectiveness of lignin, extracted from oil palm (Elaeis guineensis) biomass as water-in-oil (W/O) emulsifying agent. To achieve this goal, soda lignin (SL) was extracted via soda pulping process and a series of nanosized soda lignin (NSL) were prepared using homogenizer at three different speed i.e. 10,400 rpm (NSL 10), 11,400 rpm (NSL 11) and 12,400 rpm (NSL 12) for one hour. All prepared samples were characterized by FT-IR, UV-Vis spectroscopy, thermogravimetric analysis (TGA), zeta potential analyser, Transmission Electron Microscope (TEM) and Extreme High Resolution Field Emission Scanning Electron Microscope (XHR-FESEM). The result of FTIR showed that there is no prominent change occurred in spectra of all samples while a good stability was reflected by TGA curves. The percentage of creaming index and visual observations of all samples demonstrated that NSL 12 and dosage 2 g (out of 1 g, 1.5 g and 2 g) were found to be the best among all samples. Furthermore, the results of IFT indicate that NSL 12 was proven to be more stable than the commercial product. Therefore, NSL 12 is selected for toxicological studies and was found safe in both, in vitro and in vivo studies.

Preparation and characterizations of oil palm fronds cellulose nanocrystal (OPF-CNC) as reinforcing filler in epoxy-Zn rich coating for mild steel corrosion protection.

Oil palm frond (OPF) is one of largest contributions to the biomass waste from oil palm plantation. In this work, OPF has been successfully utilized to prepare cellulose nanocrystal (OPF-CNC) by acid hydrolysis. OPF was initially treated with autohydrolysis treatment. The obtained OPF-CNC was characterized via complementary analyses. The produced OPF-CNC showed a high crystallinity index value (60%) and high BET surface area (26.10 m2 g-1) as compared to α-cellulose (crystallinity index: 54% and BET surface area:7.14 m2g-1). The surface analyses via scanning electron microscope (SEM) and transmission electron microscopy (TEM) demonstrated that the OPF-CNC has a smooth surface with a needle-like shape, where the average length and diameter are 95.09 nm and 6.81 nm, respectively. The corrosion analyses via electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization (PD) illustrate that the coated mild steel with the inclusion of 0.5 wt% OPF-CNC has managed to sharply reduce the corrosion (99%). The coated mild steel with the inclusion of 0.5 wt% OPF-CNC showed the highest hydrophobicity (100.5 ± 0.7°) and has lowest amount of O via water contact angle and energy dispersive X-ray spectroscopy (EDX) analyses respectively, indicating lowest corrosion rate.

The structural characterization and antioxidant properties of oil palm fronds lignin incorporated with p-hydroxyacetophenone.

This study reports on the effects of unmodified autohydrolyzed ethanol organosolv lignin (AH EOL) and modified autohydrolyzed ethanol organosolv lignin on the structural characteristics and antioxidant properties upon incorporation of p-hydroxyacetophenone (AHP EOL). The lignin samples isolated from black liquor of oil palm fronds (OPF) were evaluated and compared using various complementary analyses; FTIR, 1H and 13C NMR spectroscopy, 2D-NMR spectroscopy (HMBC and HSQC), CHN, GPC, HPLC and thermal analyses (TGA and DSC). Chemically modified organosolv lignin (AHP EOL) provided lignin with lower molecular weight (Mw), which has smaller fragments that leads to higher solubility rate in water in comparison to unmodified organosolv lignin, AH EOL (DAHP EOL: 19.8% > DAH EOL: 14.0%). It was evident that the antioxidant properties of modified organosolv lignin has better reducing power in comparison to the unmodified organosolv lignin. Therefore, the functionalization of lignin polymers enhanced their antioxidant properties and structural features towards a various alternative approach in lignin-based applications.

Electrochemical data of single and hybrid sol-gel coating precursors for aluminum alloy corrosion protection in 3.5% NaCl.

The anti-corrosion performances of single(TEOS) and hybrid (APTES-TEOS) sol-gel coatings on Al alloy samples exposed to 3.5 wt% NaCl were evaluated employing electrochemical techniques such as electrochemical impedance spectroscopy (EIS) and potentiodynamic polarization. The data acquired using the three corrosion analysis techniques were in accordance with each other where hybrid sol-gel coating offered the lowest corrosion rate and current density in comparison to the single precursor silanol coating. Tafel curves suggested that the hybrid silane coatings mitigate both the anodic and cathodic reactions simultaneously (mixed type inhibitor). These techniques justified that incorporation of hybrid sol-gel improved the Al corrosion protection performance considerably.

Modification of oil palm fronds lignin by incorporation of m-cresol for improving structural and antioxidant properties.

Lignin extracted from oil palm fronds (OPF) underwent chemical modification by incorporating m-cresol into the lignin matrix. This study reports on the physicochemical properties and antioxidant activity of unmodified autohydrolyzed ethanol organosolv lignin (AH EOL) and the modified autohydrolyzed ethanol organosolv lignin (AHC EOL). The lignin samples were analyzed by FTIR, 1H and 13C NMR spectroscopy, 2D NMR: HSQC spectroscopy, CHN analysis, molecular weight distribution analysis; GPC and thermal analysis; DSC and TGA. The lignin modification has reduced the hydrophobicity of its complex structure by providing better quality lignin with smaller fragments and higher solubility rate in water (DAHCEOL: 42%>DAHEOL: 25%). It was revealed that the modification of lignin has improved their structural and antioxidant properties, thus venture their possible applications.

The effect of p-nitrophenol toward the structural characteristics and antioxidant activity of oil palm fronds (OPF) lignin polymers.

This article reports on the structural characteristics and antioxidant activity of unmodified autohydrolyzed ethanol organosolv lignin (AH EOL) extracted from oil palm fronds (OPF) and modified autohydrolyzed ethanol organosolv lignin via incorporation of p-nitrophenol (AHNP EOL). The isolated lignin were analyzed by FTIR, 1H and 13C NMR spectroscopy, 2D NMR; HSQC and HMBC, CHN analysis, molecular weight distribution using GPC analyzer, thermal analysis; TGA and DSC. The chemical modification by utilizing an organic scavenger during delignification process provided smaller lignin fragments and enhanced the solubility of lignin by reducing its hydrophobicity properties. It was revealed that the antioxidant properties increased as compared to the unmodified organosolv lignin. Additionally, the modified lignin has better solubility in water (DAHNP EOL=35%>DAH EOL=25%).

Influence of alkaline hydrogen peroxide pre-hydrolysis on the isolation of microcrystalline cellulose from oil palm fronds.

In the present study, microcrystalline cellulose (MCC) was isolated from oil palm fronds (OPF) using chemo-mechanical process. Wherein, alkaline hydrogen peroxide (AHP) was utilized to extract OPF fibre at different AHP concentrations. The OPF pulp fibre was then bleached with acidified sodium chlorite solution followed by the acid hydrolysis using hydrochloric acid. Several analytical methods were conducted to determine the influence of AHP concentration on thermal properties, morphological properties, microscopic and crystalline behaviour of isolated MCC. Results showed that the MCC extracted from OPF fibres had fibre diameters of 7.55-9.11nm. X-ray diffraction (XRD) analyses revealed that the obtained microcrystalline fibre had both celluloses I and cellulose II polymorphs structure, depending on the AHP concentrations. The Fourier transmission infrared (FTIR) analyses showed that the AHP pre-hydrolysis was successfully removed hemicelluloses and lignin from the OPF fibre. The crystallinity of the MCC was increased with the AHP concentrations. The degradation temperature of MCC was about 300°C. The finding of the present study showed that pre-treatment process potentially influenced the quality of the isolation of MCC from oil palm fronds.

Physicochemical of microcrystalline cellulose from oil palm fronds as potential methylene blue adsorbents.

The present study sheds light on the physical and chemical characteristics of microcrystalline cellulose (MCC) isolated from oil palm fronds (OPF) pulps. It was found that the OPF MCC was identified as cellulose II polymorph, with higher crystallinity index than OPF α-cellulose (CrIOPFMCC: 71%>CrIOPFα-cellulose: 47%). This indicates that the acid hydrolysis allows the production of cellulose that is highly crystalline. BET surface area of OPF MCC was found to be higher than OPF α-cellulose (SBETOPFMCC: 5.64m2g-1>SBETOPFα-cellulose:Qa0 2.04m2g-1), which corroborates their potential as an adsorbent. In batch adsorption studies, it was observed that the experimental data fit well with Langmuir adsorption isotherm in comparison to Freundlich isotherm. The monolayer adsorption capacity (Qa0) of OPF MCC was found to be around 51.811mgg-1 and the experimental data fitted well to pseudo-second-order kinetic model.

Exploring the effect of cellulose nanowhiskers isolated from oil palm biomass on polylactic acid properties.

In this work, polylactic acid (PLA) reinforced cellulose nanowhiskers (CNW) were prepared through solution casting technique. The CNW was first isolated from oil palm empty fruit bunch microcrystalline cellulose (OPEFB-MCC) by using 64% H2SO4 and was designated as CNW-S. The optical microscopy revealed that the large particle of OPEFB-MCC has been broken down by the hydrolysis treatment. The atomic force microscopy confirmed that the CNW-S obtained is in nanoscale dimension and appeared in individual rod-like character. The produced CNW-S was then incorporated with PLA at 1, 3, and 5 parts per hundred (phr) resins for the PLA-CNW-S nanocomposite production. The synthesized nanocomposites were then characterized by a mean of tensile properties and thermal stability. Interestingly to note that incorporating of 3 phr/CNW-S in PLA improved the tensile strength by 61%. Also, CNW-S loading showed a positive impact on the Young's modulus of PLA. The elongation at break (Eb) of nanocomposites, however, decreased with the addition of CNW-S. Field emission scanning electron microscopy and transmission electron microscopy revealed that the CNW-S dispersed well in PLA at lower filler loading before it started to agglomerate at higher CNW-S loading (5phr). The DSC analysis of the nanocomposites obtained showed that Tg,Tcc and Tm values of PLA were improved with CNW-S loading. The TGA analysis however, revealed that incopreated CNW-S in PLA effect the thermal stability (T10,T50 and Tmax) of nanocomposite, where it decrease linearly with CNW-S loading.