High-yield graphene exfoliation using sodium dodecyl sulfate accompanied by alcohols as surface-tension-reducing agents in aqueous solution

The exfoliation of graphite was investigated in aqueous solutions containing sodium dodecyl sulfate (SDS) as a surfactant. The exfoliation was greatly enhanced near the surface aggregation concentration (SAC) of SDS, 2.6 mM, and then decreased for higher SDS contents. However, the flakes exfoliated near the SAC were graphite, whereas graphene was obtained above the critical micelle concentration (CMC). The effect of the use of alcohols as surface-tension-reducing agents (STRAs) on the exfoliation was then investigated. With ethyl alcohol, a dispersion of 2.1 mg ml⁻¹ graphene was achieved from 2.6 mM SDS after only 1 h of sonication, whereas a dispersion of 0.2 mg ml⁻¹ was obtained above the CMC in the absence of STRAs. The results demonstrate that the SDS content near the SAC is highly beneficial for exfoliation as long as the surface tension is maintained near 41.0 mN ml⁻¹. This finding supports the notion that the structure of the adsorbed SDS, depending on its concentration, strongly affects the exfoliation of graphite into graphene.     

Syntheses and surface active properties of cationic surfactants having multi ammonium and hydroxyl groups

In this study, cationic surfactants having mono-, di-, and tri-amminium groups were synthesized by the condensation reaction of alkyl glycidyl ether and alkyl amine followed by the quarternization with dimethyl sulfate. The structure of the product was elucidated by ¹H NMR and FT-IR. The minimum surface tension achieved using C12-BHDM surfactant was around 28.88 mN/m, which suggests that C12-BHDM can be used to reduce the surface tension of primarily aqueous formulations and to act as emulsifiers. Dynamic surface tension measurement using a maximum bubble pressure tensiometer indicated that much longer time was required to reach an equilibrium value presumably due to the low mobility rate of a surfactant molecule with high molecular weight. The interfacial tensions measured between 1 wt.% surfactant solution and n-decane were found to be in the same order of magnitude as those exhibited between micellar solutions and nonpolar hydrocarbon oils. It has been observed that the results for foam stability measurement are consistent with those of CMC and contact angle. That is, the percentage of foam volume decrease has been observed to increase with an increase in number of ammonium and hydroxyl groups.     

Fractionated extraction of saponins from Brazilian ginseng by sequential process using supercritical CO2, ethanol and water

Saponins are surfactants that reduce the surface tension of aqueous solutions, besides having pharmacological actions. In order to extract and fractionate saponins from Pfaffia glomerata roots and Hebanthe eriantha roots using supercritical technology, fractionated extracts were obtained from a sequential process in fixed bed using supercritical CO₂ (scCO₂), ethanol, and water as solvents. All extractions were carried out in four sequential steps, at 50 °C and 300 bar. In the first step, pure scCO₂ was used as solvent, while (a) scCO₂/etanol (70:30, w/w); (b) ethanol, and (c) ethanol/water (70:30, v/v) were used as solvents in the three subsequent steps. The extracts were analyzed by thin layer chromatography (TLC) and surface tension. The extraction yields of the four steps were 0.16, 0.55, 1.00, and 6.90% for P. glomerata roots, and 0.17, 0.58, 0.89, and 28% for H. eriantha roots, showing a predominance of high polarity compounds in these species. TLC analysis showed that the extraction process was selective according to the polarity of the solvent, and provided extracts containing different saponins, except for scCO₂ extraction. The extracts from the extraction using ethanol + scCO₂ (Step 2) showed the greatest ability to reduce the surface tension of water from 72 mN m⁻¹ (pure water) to 25 mN m⁻¹, suggesting that this step was the best for extraction of less polar saponins in the extracts. The critical micelle concentration (CMC) values were approximately 2 and 8 g L⁻¹ for P. glomerata and H. Eriantha, respectively. These results confirmed the efficacy of the extraction process under study.     

Interfacial properties of cationic and anionic Gemini surfactant mixtures

The possibility and the prospect of cationic/anionic (“catanionic”) surfactant mixtures based on sulfonate Gemini surfactant (SGS) and bisquaternary ammonium salt (BQAS) in the field of enhanced oil recovery was investigated. The critical micelle concentration (CMC) of SGS/BQAS surfactant mixtures was 5.0 × 10⁻⁶ mol/L, 1–2 orders of magnitude lower than neat BQAS or SGS. A solution of either neat SGS or BQAS, could not reach an ultra-low interfacial tension (IFT); but 1:1 mol/mol mixtures of SGS/BQAS reduced the IFT to 1.0 × 10⁻³ mN/m at 100 mg/L. For the studied surfactant concentrations, all mixtures exhibited the lowest IFT when the molar fraction of SGS among the surfactant equaled 0.5, indicating optimal conditions for interfacial activity. The IFT between the 1:1 mol/mol SGS/BQAS mixtures and crude oil decreased and then increased with the NaCl and CaCl₂ concentrations. When the total surfactant concentration was above 50 mg/L, the IFT of SGS/BQAS mixtures was below 0.01 mN/m at the studied NaCl concentrations. Adding inorganic salt reduced the charges of hydrophilic head groups, thereby making the interfacial arrangement more compact. At the NaCl concentration was above 40,000 mg/L, surfactant molecules moved from the liquid–liquid interface to the oil phase, thus resulting in low interfacial activity. In addition, inorganic salts decreased the attractive interactions of the SGS/BQAS micelles that form in water, decreasing the apparent hydrodynamic radius (D_{H, app}) of surfactant aggregates. When the total concentration of surfactants was above 50 mg/L, the IFT between the SGS/BQAS mixtures and crude oil decreased first and then increased with time. At different surfactant concentrations, the IFT of the SGS/BQAS mixtures attained the lowest values at different times. A high surfactant concentration helped surfactant molecules diffuse from the water phase to the interfacial layer, rapidly reducing the IFT. In conclusion, the cationic-anionic Gemini surfactant mixtures exhibit superior interfacial activity, which may promote the application of Gemini surfactant.     

Sequential extraction of bioactive compounds from Melia azedarach L. in fixed bed extractor using CO2, ethanol and water

Melia azedarach L. is a plant with wide use in folk medicine since it contains many bioactive compounds of interest. The present study aimed to extract bioactive compounds from M. azedarach fruits by a sequential process in fixed bed using various solvent mixtures. Extractions were performed at 50 °C and 300 bar in four sequential steps using supercritical CO₂ (scCO₂), scCO₂/ethanol, pure ethanol, and ethanol/water mixture as solvents, respectively. The efficacy of the extraction process was evaluated by extraction yield and kinetics, and analysis of extracts by: (1) thin layer chromatography (TLC), (2) phenolics content, (3) reduction of surface tension of water, (4) gas chromatography (GC–MS), (5) electrospray ionization mass spectrometry (ESI–MS) and (6) antiviral activity. The overall extraction yield reached 45% and TLC analysis showed extracts with different composition. extract obtained from CO₂/ethanol mixture (SCEE) exhibited the greatest ability to reduce surface tension of water from 72.4 mN m⁻¹ [1] of pure water to 26.9 mN m⁻¹ of an aqueous solution of 40 g L⁻¹. The highest phenolics contents were observed in both the hydroalcoholic extract and scCO₂/ethanolic extract. Volatile oils were not detected in the supercritical extracts by GC–MS. MS analyses identified the fatty acids: linoleic, palmitic and myristic acid in the supercritical extract (SCE), and the phenolics: caffeic acid and malic acid in the other extracts. In addition, SCE and SCEE extracts showed significant inhibition percentage against Herpes Simplex Virus Type 1. The extraction process proposed in the present study produced extracts with significant potential for application in food and pharmaceutical industries.     

Development of gluten-free flat bread using hydrocolloids: Xanthan and CMC

The effects of xanthan gum (XG) and (carboxymethyl cellulose (CMC) (5–20 g kg⁻¹) on the quality parameters of gluten-free flat bread, based on rice flour were investigated. Increase in CMC concentration yielded bigger gas cells, leading to better crumb porosity. Formula 3 (F3), containing 15 g kg⁻¹ XG and formula 10 (F10), containing 10 g kg⁻¹ CMC and 10 g kg⁻¹ XG resulted in the highest dough yield (P < 0.05) and bread yield, respectively, and F10 showed the lowest bread weight loss (P < 0.05). F10, followed by, F3 were the best and most acceptable (P < 0.05) formulae, compared to all the others.     

Supercritical carbon dioxide extraction of Gac oil

Supercritical carbon dioxide extraction of Gac (Momordica cochinchinensis Spreng) aril was performed at pressures ranging from 200 to 400 bar, temperatures from 313 to 343 K and specific flow rates from 50 to 90 kg h⁻¹ CO₂ kg⁻¹ Gac aril. Total oil recovery and carotenes concentration were investigated in the course of extraction. Mathematical modelling of oil solubility data was also performed. The results showed that at specific flow rate of 70 kg h⁻¹ kg⁻¹, pressure of 400 bar and temperature of 343 K, Gac oil recovery exceeded 95% after 120 min of extraction. Gac oil loading of supercritical carbon dioxide was successfully described by Chrastil's model. Carotenes concentration of extracted Gac oil was found at level of thousands of ppm.     

Extraction of jojoba seed oil using supercritical CO2+ethanol mixture in green and high-tech separation process

In this study, the extraction of jojoba seed oil obtained from jojoba seed using both supercritical CO₂ and supercritical CO₂+ethanol mixtures was investigated. The recovery of jojoba seed oil was performed in a green and high-tech separation process. The extraction operating was carried out at operating pressures of 25, 35 and 45 MPa, operating temperatures of 343 and 363 K, supercritical fluid flow rates of 3.33 × 10⁻⁸, 6.67 × 10⁻⁸ and 13.33 × 10⁻⁸ m³ s⁻¹, entrainer concentrations of 2, 4 and 8 vol.%, and average particle diameters of 4.1 × 10⁻⁴, 6.1 × 10⁻⁴, 8.6 × 10⁻⁴ and 1.2 × 10⁻³ m. It was found that a green chemical modifier such as ethanol could enhance the solubilities, initial extraction rate and extraction yield of jojoba seed oil from the seed matrix as compared to supercritical CO₂. In addition, it was found that the solubility, the initial extraction rate and the extraction yield depended on operating pressure and operating temperature, entrainer concentration, average particle size and supercritical solvent flow rate. The solubility of jojoba seed oil and initial extraction rate increased with temperature at the operating pressures of 35 and 45 MPa and decreased with increasing temperature at the operating pressure of 25 MPa. Furthermore, supercritical fluid extraction involved short extraction time and minimal usage of small amounts entrainer to the CO₂. About 80% of the total jojoba seed oil was extracted during the constant rate period at the pressure of 35 and 45 MPa.     

Sulfur-doped mesoporous carbon from surfactant-intercalated layered double hydroxide precursor as high-performance anode nanomaterials for both Li-ion and Na-ion batteries

We describe a preparation of sulfur-doped mesoporous amorphous carbon (SMAC) from a commercially available alkyl surfactant sulfonate anion-intercalated NiAl-layered double hydroxide precursor via thermal decomposition and subsequent acid leaching. The resultant amorphous carbon is endowed with the integrated advantage of featuring high reversible capacity and long cycling stability: intrinsic doping of sulfur, large specific area, and broad mesopore size distribution. Electrochemical evaluation shows that the SMAC electrode exhibits highly enhanced electrochemical performances, compared with the electrode of non-doped mesoporous and amorphous carbon prepared by using a different surfactant (sodium laurate). A high reversible capacity of 958 mA h g⁻¹ is achieved for the SMAC electrode after 110 cycles at 200 mA g⁻¹, and especially a superlong cycle life with a reversible capacity of 579 mA h g⁻¹ after 970 cycles at 500 mA g⁻¹. Moreover, the SMAC electrode can facilitate the reversible insertion/extraction of Na ion, owing to the proper specific area and mesopore size distribution, as well as the improved electronic conductivity resulted from doping of sulfur.     

Microstructural features of nanocomposite of alumina@carbon nanotubes/alumina nanoparticles synthesized by a solvothermal method

The present study focuses on the synthesis of nanocomposite gamma alumina (γ-Al₂O₃), boehmite and multi- walled carbon nanotubes (MWCNTs) via a solvothermal procedure. The method is based on the ex situ filling of opened CNTs by liquid reactants. The microstructure and morphology of the synthesized nanocomposite Al₂O₃@CNTs/Al₂O₃ was characterized by high resolution transmission electron microscopy (HRTEM), transmission electron microscopy (TEM), field emission scanning electron microscopy (FESEM), energy-dispersive X-ray spectroscopy (EDX), X-ray diffraction (XRD), Brunauer–Emmett–Teller (BET) and N₂ adsorption–desorption analysis.Based on the experimental results, it was determined that the volume ratio of γ-Al₂O₃/MWCNTs and the surface tension of the solvent both greatly influence the morphology of the nanocomposite. The resultant MWCNTs were coated and filled by homogeneous and uniform boehmite and γ-Al₂O₃ layers and nanoparticles with thicknesses of 1–3 nm and diameters of 20–40 nm, when the volume ratio of γ-Al₂O₃/MWCNT_S is 1 and the surface tension of the solvent is approximately 26 mN m^?1 at 20 °C, far below the maximum value (100–200 mN m^?1) for MWCNT filling.     

Discovery of effective solvents for platelet-type graphite nanofibers

The dispersibility of platelet-type graphite nanofibers (PGNFs), an archetype of carbon material with a surface dominated by graphitic edge planes, has been measured in 28 solvents and rationalized on the basis of solvent surface tension and Hansen solubility parameters. Successful solvents possess surface tensions of ∼25–35 mJ m⁻² and substantial values of the hydrogen-bonding Hansen parameter (δ_H ∼ 14–16 MPa^1/2), and many of them are alcohols, such as 1-butanol, ethanol or cyclohexanol. Such result is mainly attributed to the fact that the PGNF edge planes are decorated with oxygen functional groups. The dispersion behavior of the nanofibers could be changed to that typically exhibited by carbon nanotubes and graphene by means of a high temperature annealing that converted their surface edge planes to curved basal planes.     

Processing of alumina-coated clay–diatomite composite membranes for oily wastewater treatment

Crack-free alumina-coated clay–diatomite composite membranes were successfully prepared by a simple pressing and dip-coating route using inexpensive raw materials at a temperature as low as 1000 °C in air. The changes of porosity, flexural strength, pore size, flux, and oil rejection rate of the membranes were investigated while changing the diatomite content. A simple burn-out process subjected to the used membranes in air completely recovered the specific surface area, steady state flux, and oil rejection rate of the virgin membranes. The recycled membranes showed an exceptionally high oil rejection rate (99.9%) with a feed oil concentration of 600 mg/L at an applied pressure of 101 kPa. The typical porosity, pore size, flexural strength, oil rejection rate, and steady state flux of the recycled alumina-coated clay–diatomite composite membrane were 36.5%, 0.12 μm, 32 MPa, 99.9%, and 6.91×10⁻⁶ m³ m⁻² s⁻¹, respectively, at an applied pressure of 101 kPa.     

Effect of diamond surface orientation on the thermal boundary conductance between diamond and aluminum

[100] and [111] oriented diamond substrates were treated using Ar:H and Ar:O plasma treatments, and 1:1 HNO₃:H₂SO₄ heated at 200 °C. Subsequent to these treatments, an aluminum layer was either evaporated or sputteredon the substrates. The thermal boundary conductance (TBC) as well as the interfacial acoustical reflection coefficient between this layer and the diamond substrate was then measured using a Time Domain ThermoReflectance (TDTR) experiment. For the Ar:H plasma treated surfaces the [111] oriented faces exhibited conductances 40% lower than the [100] oriented ones with the lowest measured TBC at 32 ± 5 MWm^− 2 K^− 1. The treatments that led to oxygen-terminated diamond surfaces (extiti.e. acid or Ar:O plasma treatments) showed no TBC anisotropy and the highest measured value was 230 ± 25 MWm^− 2 K^− 1 for samples treated with Ar:O plasma with a sputtered Al layer on top. Sputtered layers on oxygen-terminated surfaces showed systematically higher TBC than their evaporated counterparts. The interfacial acoustic reflection coefficient correlated qualitatively with TBC when comparing samples with the same type of surface terminations (O or H) but this correlation failed when comparing H and O terminated interfaces with each other.     

Prediction of the optimum aqueous phase composition of a triglyceride microemulsion using response surface methodology

This paper presents the application of response surface methodology to predict the optimum aqueous phase composition of a triglyceride microemulsion for enhanced oil recovery. The two models capturing the relationships between interfacial tension and tertiary oil recovery data with the aqueous phase composition were validated prior to optimization. It was predicted that the optimum aqueous phase contains 3 wt% sodium chloride, 0.98 wt% alkyl polyglycosides, and 2.98 wt% glyceryl monooleate. At this composition the corresponding interfacial tension is minimum (0.000229451 mN/m) and the tertiary oil recovery is maximum (71.7865%). The predicted optimum aqueous phase composition using historical-data design is close to the experimental value.     

Characterization of vertical Mo/diamond Schottky barrier diode from non-ideal I–V and C–V measurements based on MIS model

In this study, we investigated non-ideal characteristics of a diamond Schottky barrier diode with Molybdenum (Mo) Schottky metal fabricated by Microwave Plasma Chemical Vapour Deposition (MPCVD) technique. Extraction from forward bias I–V and reverse bias C^− 2–V measurements yields ideality factor of 1.3, Schottky barrier height of 1.872 eV, and on-resistance of 32.63 mΩ·cm². The deviation of extracted Schottky barrier height from an ideal value of 2.24 eV (considering Mo workfunction of 4.53 eV) indicates Fermi level pinning at the interface. We attributed such non-ideal behavior to the existence of thin interfacial layer and interface states between metal and diamond which forms Metal-Interfacial layer-Semiconductor (MIS) structure. Oxygen surface treatment during fabrication process might have induced them. From forward bias C–V characteristics, the minimum thickness of the interfacial layer is approximately 0.248 nm. Energy distribution profile of the interface state density is then evaluated from the forward bias I–V characteristics based on the MIS model. The interface state density is found to be uniformly distributed with values around 10¹³ eV^− 1·cm^− 2.     

Low-cost and high-performance electrode materials based on BiCoO3 microspheres

Ternary metal oxides have great potential for chemical storage devices because of their outstanding synergistic effects as well as rich redox reactions. However, there are limited reports of 3D structure BiCoO₃ materials and relevant electrochemical properties. Meanwhile, the study of BiCoO₃ is reasonably important for underlying metal oxides researches. In this work, we have successfully developed a 3D urchin-like BiCoO₃ material without using any template and surfactant. For the supercapacitor application, the BiCoO₃ material showed a specific capacitance of 152 F g⁻¹ at the current density of 1 A g ⁻¹, and this value exhibited a rate capability of 82.3% at a high current density of 10 A g ⁻¹. Furthermore, the sample showed the ideal cycling stability (92.7% retention after 5000 times cycles at the current density of 1 A g ⁻¹ and nearly invariable specific capacitance during different current density cycles). These results suggest that the obtained urchin-like BiCoO₃ sample has superb electrochemical performances which suggest its promising applications as renewable and clean energy storage devices electrode materials in the future.     

Bioconversion of barley straw and corn stover to butanol (a biofuel) in integrated fermentation and simultaneous product recovery bioreactors

In these studies concentrated sugar solutions of barley straw and corn stover hydrolysates were fermented using Clostridium beijerinckii P260 with simultaneous product recovery and compared with the performance of a control glucose batch fermentation process. The control glucose batch fermentation resulted in the production of 23.25 g L⁻¹ ABE from 55.7 g L⁻¹ glucose solution resulting in an ABE productivity and yield of 0.33 g L⁻¹ h⁻¹ and 0.42, respectively. The control reactor (I) was started with 62.5 g L⁻¹ initial glucose and the culture left 6.8 g L⁻¹ unused sugar due to butanol toxicity resulting in incomplete sugar utilization. Barley straw (BS) hydrolysate sugars (90.3 g L⁻¹) resulted in the production of 47.20 g L⁻¹ ABE with a productivity of 0.60 g L⁻¹ h⁻¹ and a yield of 0.42. Fermentation of corn stover (CS) hydrolysate sugars (93.1 g L⁻¹) produced 50.14 g L⁻¹ ABE with a yield of 0.43 and a productivity of 0.70 g L⁻¹ h⁻¹. These productivities are 182–212% higher than the control run. The culture was able to use 99.4–100% sugars (CS & BS respectively) present in these hydrolysates and improve productivities which were possible due to simultaneous product removal. Use of >100 g L⁻¹ hydrolysate sugars was not considered as it would have been toxic to the culture in the integrated (simultaneous fermentation and recovery) process.     

Supercapacitors based on carbons with tuned porosity derived from paper pulp mill sludge biowaste

Hydrothermal carbonization followed by chemical activation is utilized to convert paper pulp mill sludge biowaste into high surface area (up to 2980 m² g⁻¹) carbons. This synthesis process employs an otherwise unusable byproduct of paper manufacturing that is generated in thousands of tons per year. The textural properties of the carbons are tunable by the activation process, yielding controlled levels of micro and mesoporosity. The electrochemical results for the optimized carbon are very promising. An organic electrolyte yields a maximum capacitance of 166 F g⁻¹, and a Ragone curve with 30 W h kg⁻¹ at 57 W kg⁻¹ and 20 W h kg⁻¹ at 5450 W kg⁻¹. Two ionic liquid electrolytes result in maximum capacitances of 180–190 F g⁻¹ with up to 62% retention between 2 and 200 mV s⁻¹. The ionic liquids yielded energy density–power density combinations of 51 W h kg⁻¹ at 375 W kg⁻¹ and 26–31 W h kg⁻¹ at 6760–7000 W kg⁻¹. After 5000 plus charge–discharge cycles the capacitance retention is as high at 91%. The scan rate dependence of the surface area normalized capacitance highlights the rich interplay of the electrolyte ions with pores of various sizes.     

Characterization,surface properties and biological activity of new prepared cationic surfactants

Three cationic surfactants were prepared. A condensation reaction between dimethylaminopropylamine (DMAPA) and benzaldehyde was performed. The produced Schiff base was quaternization with three fatty alkyl bromide with different carbon chain length separately to form the desired cationic surfactants. The chemical structure of synthesized cationic surfactants was confirmed by FTIR, ¹H NMR and mass spectroscopy. It was found that the chemical structure of prepared compounds has an effect on surface properties, where increasing the hydrophobic chain length decrease the values of CMC, Г_max while A_min value was increased. The thermodynamic parameters showed that adsorption and micellization processes are spontaneous. It is clear that the prepared cationic surfactants at first tend to adsorb at surface, then it aggregate to form micelle. The prepared surfactants showed good biological activity against gram positive and negative bacteria and fungi in the following order of II (C12) > I (C10) > III (C16). The serial dilution method was used to evaluate the inhibiting effect of these compounds on the sulfate reducing bacteria growth.