Search Results (28)

Waste wheat straw (WS) is a common agricultural waste with a low acquisition cost and a high annual yield, making it a promising feedstock for a biorefinery. In this work, efficient co-production of reducing sugars and xylo-oligosaccharides (XOSs) from WS was realized through FeCl₃-assisted p-toluene sulfonic acid (PTSA) pretreatment. The effects of reaction conditions (PTSA content, FeCl₃ loading, pretreatment duration, and temperature) on lignin and xylan elimination and enzymolysis were analyzed. The results manifested that the enzymolysis of WS substantially elevated from 22.0% to 79.3% through the treatment with FeCl₃-PTSA/water (120 °C, 60 min). The xylan removal and delignification were 79.7% and 66.6%, respectively. XOSs (4.0 g/L) were acquired in the pretreatment liquor. The linear fitting about LogR₀ with enzymolysis, delignification, xylan elimination and XOSs content was investigated to explain the reasons for the elevated enzymolysis and to clarify the comprehensive understanding of WS enzymolysis through the FeCl₃-PTSA/water treatment. In addition, the recycling test of FeCl₃-PTSA/water manifested a good recycling ability for WS treatment, which would reduce the pretreatment cost and enhance the economic benefit. To sum up, FeCl₃-assisted PTSA treatment of biomass for co-production of reducing sugars and XOSs is an alternative method of waste biomass valorization. Full article

This paper discusses the results of our investigation of the effect of processing parameters on the electrochemical properties of poly(vinylidene fluoride) single-walled carbon nanotube sheets and PVDF-CNTs modified by solution cast polyimide coating, followed by electrodeposition of polypyrrole. The polyimide-coated single-wall carbon nanotube sheet–PI/SWCNTs composite consists of SWCNT and PVDF (9:1) wt.% and 0.1–1 wt.% polyimide. The processing temperature varied from 90 to 250 °C. SEM images validated the nanostructure, while EDX confirmed the material composition. EIS analysis showed that the composite electrode material processed at 90 °C and followed by electrodeposition of polypyrrole has the lowest bulk resistance (65.27 Ω), higher porosity (4.59%), and the highest specific capacitance (209.16 F/g), indicating superior ion transport and charge storage. Cyclic voltammetry and cyclic charge–discharge analyses revealed that the hybrid composite electrode processed at 90 °C achieved a specific capacitance of 655.34 F/g at a scan rate of 5 mV/s, demonstrating excellent cycling stability over 10 cycles at a current density of 0.5 A/g. In contrast, composite electrodes processed at 180 °C and 250 °C showed decreased performance due in part to structural densification and low porosity. These findings underscore the critical role of processing temperatures in optimizing the electrochemical properties of PI/SWCNT composites, advancing their potential for next-generation energy storage systems. Full article

The reactivity of the benzenedithiolate (bdt)-bridged complex [Fe₂(CO)₆(µ-bdt)] with arsine, stibine and phosphine ligands has been studied. The new mono- and disubstituted complexes [Fe₂(CO)₅(EPh₃)(µ-bdt)] (E = As, 1; E = Sb 3) and [Fe₂(CO)₄(EPh₃)₂(µ-bdt)] (E = As, 2; E = Sb, 4) and the previously reported [Fe₂(CO)₄(PPh₂H)₂(µ-bdt)] (5) have been prepared by Me₃NO-initiated carbonyl substitution reactions of [Fe₂(CO)₆(µ-bdt)] with appropriate ligands at 80 °C. Spectroscopic and single-crystal X-ray diffraction studies reveal that in all cases the introduced ligands occupy apical coordination site(s) lying trans to the iron–iron bond. Their electrochemistry has been probed by cyclic voltammetry and selected complexes have been tested as proton reduction catalysts. Monosubstituted complexes 1 and 3 show two irreversible reductions at ca. −1.7 V and −2.0 V, respectively, relative to Fc⁺/Fc, while the disubstituted complexes 2 and 5 show a single irreversible reduction at ca. −2.2 V and −1.84 V, respectively. Complexes 1, 3 and 5 can catalyse electrocatalytic proton reduction in the presence of either p-toluene sulfonic acid (TsOH) or trifluoroacetic acid (CF₃CO₂H). Full article

This systematic review aims to evaluate whether the application of antioxidant solutions can enhance the bond strength of resin-based materials to sodium hypochlorite (NaOCl)-treated dentin. This study follows the PICOT strategy: population (sodium hypochlorite-treated dentin), intervention (application of antioxidants), control (distilled water), outcome (bond strength), and type of studies (in vitro studies). The systematic review and meta-analysis were conducted following PRISMA guidelines. Electronic databases were searched for in vitro studies evaluating the effects of antioxidants on bond strength to sodium hypochlorite-treated dentin. Two independent reviewers screened articles, extracted data, and assessed risk of bias. Meta-analyses were performed using a random-effects model to compare standardized mean differences in bond strength between antioxidant pretreatment and control groups. Inclusion criteria consisted of in vitro studies that examined the bond strength of resin-based materials to NaOCl-treated dentin with antioxidant application, while exclusion criteria included studies with incomplete data, those not using a control group, or those that did not directly measure bond strength. From 3041 initial records, 29 studies were included in the qualitative analysis and 25 in the meta-analysis. Ascorbic acid, sodium ascorbate, grape seed extract, green tea, and rosmarinic acid significantly improved bond strength to sodium hypochlorite-treated dentin (p < 0.05). The effectiveness of grape seed extract varied with adhesive system type. Hesperidin, p-toluene sulfonic acid, and sodium thiosulfate did not significantly improve bond strength. Most studies had a high risk of bias. This suggests that the conclusions drawn from these studies should be interpreted with caution, and further research with more robust methodologies may be needed to confirm the findings. In conclusion, this systematic review implies that certain antioxidants can improve bond strength to sodium hypochlorite-treated dentin, with efficacy depending on the specific agent and adhesive system used. Further standardized studies are needed to optimize protocols and confirm these findings. Full article

There is a continuous interest in cannabinoids like Δ⁹-tetrahydrocannabinol (Δ⁹-THC) and cannabidiol (CBD). Previous experimental research has described the conversion of CBD to either Δ⁸-THC or Δ⁹-THC, depending on the acid catalyst applied. The use of para-toluene sulfonic acid (pTSA) has led to the formation of Δ⁸-THC, while boron trifluoride etherate (BF₃·Et₂O) has mainly yielded Δ⁹-THC. The enormous difference in product selectivity between these two catalysts was investigated with Molecular Modeling, applying quantum chemical density functional theory. It was found that pTSA leads to fast isomerization of Δ⁹-CBD to Δ⁸-CBD and subsequent ring closure to Δ⁸-THC. BF₃·Et₂O catalysis leads to the formation of tertiary carbenium ions in the transition states, which yield Δ⁹-THC and some iso THC. Under dry conditions in refluxing toluene, it was found that pTSA is predominantly present as a dimer, and only a small fraction is available as monomeric catalyst. Applying the computationally derived activation barriers in transition state theory yielded reaction rates that predicted the amounts of cannabinoids that are in close agreement with the experimental findings from the previous literature. Full article

The application of a bidentate aromatic N,N’-donor ligand, 2,2′-biimidazole (BIIMH₂), as an extractant in the form of 1-octyl-2,2′-biimidazole (OBIIMH) and related derivatives in the solvent extraction of base metal ions (Mg²⁺, Mn²⁺, Fe³⁺, Fe²⁺, Co²⁺, Ni²⁺, Cu²⁺ and Zn²⁺) from an acidic sulfonate medium using dinonylnaphthalene disulfonic acid (DNNDSA) as a synergist was investigated. OBIIMH with DNNDSA as a co-extractant showed a lack of selectivity for base metals ions (Mg²⁺, Mn²⁺, Fe³⁺, Fe²⁺, Co²⁺, Ni²⁺, Cu²⁺ and Zn²⁺) despite its similarity with a related bidentate aromatic ligand, 2,2′-pyridylimidazole, which showed preference for Ni(II) ions. The nickel(II) specificity, through stereochemical “tailor-making”, was not achieved as expected and the extracted species were isolated to study the underlying chemistry. The homemade metal sulfonate salts, M(RSO₃)₂·6H₂O (R = Toluene and M²⁺ = Co²⁺, Ni²⁺, Cu²⁺ and Zn²⁺), were used as precursors of the metal complexes of BIIMH₂ using toluene-4-sulfonic acid as the representative sulfonate. Spectroscopic analysis and single-crystal X-ray analysis supported the formation of similar neutral distorted octahedral sulfonato complexes through the bis coordination of BIIMH₂ and two sulfonate ions rather than the formation of cationic complex species with anion coordination of sulfonates. We attributed the observation of similar complex species and the similar stability constants of the bis-complexes in solution as the cause for the lack of pH-metric separation of the later 3d metal ions. Full article

This paper presents the preparation and characterization of composite membranes based on chitosan (Chi), sulfonated ethylene–propylene–diene terpolymer (sEPDM), and polypropylene (PPy), and designed to capture hydrogen sulfide. The Chi/sEPDM/PPy composite membranes were prepared through controlled evaporation of a toluene dispersion layer of Chi:sEPDM 1;1, w/w, deposited by immersion and under a slight vacuum (100 mmHg) on a PPy hollow fiber support. The composite membranes were characterized morphologically, structurally, and thermally, but also from the point of view of their performance in the process of hydrogen sulfide sequestration in an acidic media solution with metallic ion content (Cu²⁺, Cd²⁺, Pb²⁺, and/or Zn²⁺). The operational parameters of the pertraction were the pH, pM, matrix gas flow rate, and composition. The results of pertraction from synthetic gases mixture (nitrogen, methane, carbon dioxide) indicated an efficient removal of hydrogen sulfide through the prepared composite membranes, as well as its immobilization as sulfides. The sequestration and the recuperative separation, as sulfides from an acid medium, of the hydrogen sulfide reached up to 96%, decreasing in the order: CuS > PbS > CdS > ZnS. Full article

We report the synthesis of silver anchored and para toluene sulfonic acid (pTSA) doped polyaniline/molybdenum disulfide nanocomposite (pTSA/Ag-Pani@MoS₂) for highly reproducible room temperature detection of ammonia and methanol. Pani@MoS₂ was synthesized by in situ polymerization of aniline in the presence of MoS₂ nanosheets. The chemical reduction of AgNO₃ in the presence of Pani@MoS₂ led to the anchoring of Ag to Pani@MoS₂ and finally doping with pTSA produced highly conductive pTSA/Ag-Pani@MoS₂. Morphological analysis showed Pani-coated MoS₂ along with the observation of Ag spheres and tubes well anchored to the surface. Structural characterization by X-ray diffraction and X-ray photon spectroscopy showed peaks corresponding to Pani, MoS_2, and Ag. The DC electrical conductivity of annealed Pani was 11.2 and it increased to 14.4 in Pani@MoS₂ and finally to 16.1 S/cm with the loading of Ag. The high conductivity of ternary pTSA/Ag-Pani@MoS₂ is due to Pani and MoS₂ π–π* interactions, conductive Ag, as well as the anionic dopant. The pTSA/Ag-Pani@MoS₂ also showed better cyclic and isothermal electrical conductivity retention than Pani and Pani@MoS_2, owing to the higher conductivity and stability of its constituents. The ammonia and methanol sensing response of pTSA/Ag-Pani@MoS₂ showed better sensitivity and reproducibility than Pani@MoS₂ owing to the higher conductivity and surface area of the former. Finally, a sensing mechanism involving chemisorption/desorption and electrical compensation is proposed. Full article

Phytosterol esters have attracted widespread academic and industrial interests due to their advantages in lowering cholesterol, as antioxidants, and in preventing or treating cancer. However, the generation of by-products limits the application of phytosterol esters in food fields. In this study, deep eutectic solvents (DESs), a series of green, nontoxic, low-cost and biodegradable solvents, were adopted as the catalyst for the synthesis of pine sterol esters. The results showed that the acidic DES which was prepared with choline chloride (ChCl) and p-toluene sulfonic acid monohydrate (PTSA) with a molar ratio of 1:3 performed best in the prescreening experiments. To further improve the efficiency of the pine sterol ester, the molar ratio of substrates, the amount of catalyst, the reaction temperature and the reaction time were optimized, and its yield was improved to 94.1%. Moreover, the by-products of the dehydration side reactions of the sterol can be efficiently inhibited. To make this strategy more universal, other fatty acids were also used as the substrate for the synthesis of pine sterol esters, and a yield of above 92.0% was obtained. In addition, the reusability of DES was also investigated in this study, and the efficiency of DES was well maintained within five recycled uses. Finally, DFT calculations suggested that the suitable H-bonds between ChCl and PTSA decreased the nucleophilic capacity and increased the steric hindrance of the latter, and further prevented the attack on ^βH and reduced the generation of by-products. This study developed a reliable and eco-friendly strategy for the preparation of high-quality phytosterol esters with low-dosage catalyst usage and high selectivity. Full article

Lithium-ion batteries have evolved and transcended in recent years to power every device across the spectrum, from watches to electrical vehicles and beyond. However, the lithium-ion battery requires the use of heavy and expensive transition metal oxides that have limited life cycles. Conductive polymer nanocomposites have been shown to possess good electrochemical and thermomechanical properties and are considered to be effective alternatives to transition metal oxides. The fabrication and properties of polyimide matrix-single wall carbon nanotube, SWCNT composite electrode materials, modified by the electrodeposition of polypyrrole, PPy was successfully carried out. The doping of PPy with p-Toluene sulfonic acid, T resulted in a dramatic transformation of the morphology and specific capacitance of the electrode material. Electrochemical impedance spectroscopy, EIS, cyclic voltammetry, CV, and galvanic charge–discharge tests were used to measure the electrode’s specific capacitance and specific capacity. Maximum specific capacitance values of up to 84.88 F/g and 127.13 F/g were obtained by CV and charge–discharge tests, respectively. A capacitance retention of over 80% was obtained after over 500 cycles of testing. The insertion of doped PPy into the electrode material by electrochemical polymerization was shown to positively correlate to the improved electrochemical performance of the nanocomposite. An increase in the porosity of about 34.68% over the non-doped polypyrrole was obtained from EIS measurement and supported by the optical microscope pictures. Increasing the process parameters, such as pyrrole, Py concentration and the amount of dopants, lead to a dramatic increase in the specific capacitance and capacity of the composite electrodes. Full article

During the last few years, there has been an increase in public awareness of antimicrobial fabrics, as well as an increase in commercial opportunities for their use in pharmaceutical and medical settings. The present study reports on the optimized fabrication of protonated polyaniline (PANI)-integrated polyester (PES) fabric. Para-toluene sulfonic acid (pTSA) was used to protonate the PANI fabric and thus grant it antibacterial performance. The results of a 1,1-diphenyl-2-picrylhydrazyl (DPPH) scavenging assay showed high antioxidant activity of protonated PANI fabric at a scavenging efficiency of 84.83%. Moreover, the findings revealed remarkably sensitive antibacterial performance of PANI-integrated fabric against the following Gram-positive bacteria: methicillin-resistant Staphylococcus aureus (MRSA), S. epidermidis, and S. aureus; and also against the following Gram-negative bacteria: P. aeruginosa, E. coli, and S. typhi. Attenuated total reflectance–Fourier transform infrared (ATR–FTIR) spectroscopy and energy dispersive X–ray fluorescence (EDXRF) were used to determine the changes in the structural and elemental compositions of PANI fabric upon treatment with bacterial strains. Electrochemical impedance spectroscopy (EIS) revealed that the electrical conductivity value of protonated PANI fabric decreased by one (1) order of magnitude against P. aeruginosa and S. aureus, from 3.35 ± 7.81 × 10⁻³ S cm⁻¹ to 6.11 ± 7.81 × 10⁻⁴ S cm⁻¹ and 4.63 ± 7.81 × 10⁻⁴ S cm⁻¹, respectively. Scanning electron microscopy (SEM) analysis showed the disruption of bacterial membranes and their structures when exposed to protonated PANI fabric; meanwhile, thermogravimetric analysis (TGA) demonstrated that the fabric retained its thermal stability characteristics. These findings open up potential for the use of antimicrobial fabrics in the pharmaceutical and medical sectors. Full article

This work aimed to use abietic acid (AA), as a widely available natural product, as a precursor for the synthesis of two new amphiphilic ionic liquids (AILs) and apply them as effective demulsifiers for water-in-crude oil (W/O) emulsions. AA was esterified using tetraethylene glycol (TEG) in the presence of p-toluene sulfonic acid (PTSA) as a catalyst obtaining the corresponding ester (AATG). AATG was reacted with 1-vinylimidazole (VIM) throughout the Diels–Alder reaction, forming the corresponding adduct (ATI). Following this, ATI was quaternized using alkyl iodides, ethyl iodide (EI), and hexyl iodide (HI) to obtain the corresponding AILs, ATEI-IL, and ATHI-IL, respectively. The chemical structure, surface activity, thermal stability, and relative solubility number (RSN) were investigated using different techniques. The efficiency of ATEI-IL and ATHI-IL to demulsify W/O emulsions in different crude oil: brine volumetric ratios were evaluated. ATEI-IL and ATHI-IL achieved promising results as demulsifiers. Their demulsification efficiency increased as the brine ratios decreased where their efficiency reached 100% at the crude oil: brine ratio (90:10), even at low concentrations. Full article

The increase in total Kjeldahl nitrogen (TKN) concentrations is correlated with increases in cyanobacterial bloom biomass. Standard methods for the measurement of TKN are tedious, costly, time-consuming and involve the use of hazardous catalysts, such as mercury, high temperatures and significant amounts of toxic acids and bases. Since TKN plays a pivotal role in influencing algal blooms, there is an urgent need to develop simpler, safer and more accurate methods for the determination of TKN. The simplified TKN method (s-TKN™) developed by Hach^® offers several advantages over the traditional TKN method, including eliminating the use of mercury, requiring low sample and reagent volumes and being cost-efficient and user-friendly. This communication presents preliminary results comparing the efficacy of s-TKN™ and the standard method, using commonly used primary standards and waste, estuarine and lake water matrices. For all primary standards analyzed, the s-TKN™ method exhibited good accuracy across a wide range of concentrations. The repeatability for the glycine–para-toluene sulfonic acid (Gly-PTSA) standard using the s-TKN™ method was 4.1% at the highest concentrations analyzed, with overall repeatability across concentrations comparable to the standard EPA method. For wastewater, estuarine and lake matrices, a good correlation (r² = 0.9917) between the two methods and no statistical difference in the values (p > 0.05) were obtained between two methods. Preliminary studies indicate that the s-TKN™ method has the potential to reduce the expenditure associated with the cost of analysis and has the potential to be a safer and cheaper alternative, while providing comparable analytical results to the standard method. Full article

In the present work, six protic ionic liquid (PIL) compounds based on p-toluene sulfonic acid [PTSA] anion along with different cations viz. tetraethylenepentammonium [TEPA], triethylammonium [TEA], pyridinium [Py], N-methylpiperidinium [Pip], 1-methylimidazolium [Im], and N-methylpyrrolidinium [Pyrr] were synthesized using the standard neutralization reaction method. The structural characterization of these compounds was achieved using FTIR, ¹H and ¹³C NMR spectroscopies. Thermal behavior was studied using differential scanning calorimetry to determine the melting point (T_m) and crystallization (T_c) temperatures. Thermogravimetric analysis was carried out to determine the thermal stability and degradation temperatures (Tdec) and to ascertain the hygroscopic or hydrophobic nature of the synthesized compounds. Structural effects on the outcome of various properties were witnessed and discussed in detail. Electrochemical impedance spectroscopy was utilized to study the electrical transport properties of the PILs at different temperatures. Cyclic voltammetry was performed to analyze the electrochemical stability of these PILs. Low values of activation energy indicating easy proton transportation along with good electrochemical stability make the PILs a potential candidate for use in the preparation of polymer electrolytes membranes for fuel cell applications. Full article

Combining the characteristics of rare earth extractants and water-soluble polymer complexants, a novel complexant phosphorylated chitosan (PCS) was synthesized by Kabachnik–Fields reaction with alkalized chitosan, dimethyl phosphonate, and formaldehyde as raw materials and toluene-4-sulfonic acid monohydrate (TsOH) as catalyst. The complexation properties of PCS and poly (acrylic acid) sodium (PAAS) for lanthanum ions in the solution were compared at the same pH and room temperature. In addition, the frontier molecular orbital energies of polymer–La complexes were calculated by the density functional theory method, which confirmed the complexation properties of the polymers to rare earths. The results indicate that the PCS has better water solubility compared with chitosan and good complex ability to rare earths, which can be used for rare earth separation by the complexation–ultrafiltration process. Full article