Solvent-free Method Research Articles

Paper-based flexible photodetector functionalized by WS2/Ti3C2Tx 2D-2D heterostructures

Paper-based photodetectors are gaining attention in the field of optoelectronics due to their low cost, flexibility, and eco-friendliness. The paper-based devices have applications in areas like wearable devices, environmental monitoring, and point-of-care diagnostics, where these photodetectors exhibit significant potential. In the present work, we fabricated paper-based photodetectors functionalized by WS2/Ti3C2Tx heterostructures. These materials were characterized by X-ray diffractometer, UV–visible spectroscopy, X-ray photoelectron spectroscopy, Raman spectroscopy, Energy dispersive spectroscopy, and Scanning electron microscopy. We fabricated a paper-based flexible device from this WS2/Ti3C2Tx composite using a solvent-free, easily available, and cost-effective Hand-print method. We studied the I–V & I-t response of this device. The as-synthesized device shows excellent photodetection properties with a responsivity value of 3.06 mA/W, and 5.93 × 108 Jones specific detectivity. We further investigated the flexibility and durability of these devices. Finally, the current study supports a substantial advancement in the design of reliable, flexible, and large-area optoelectronic devices.

Fabrication of 2D TiO2/α-Fe2O3/Fe-g-C3N4 heterogeneous from metallurgical solid waste for Photo-Fenton catalysis of levofloxacin/Cr(VI): Electron transfer pathway and DFT calculation

Herein, the 2D Nano α-Fe2O3 were prepared by solvent-free method from rolling iron scale (RIS) - a by-product of metallurgical industry. 2D TiO2/α-Fe2O3 nanostructures were prepared using the obtained nanocrystals. Fe-doped g-C3N4 (Fe-g-C3N4) was synthesized using RIS as the raw material. A Composite of TiO2/α-Fe2O3 and Fe-g-C3N4 was combined to prepare a TiO2/α-Fe2O3/Fe-g-C3N4 heterojunction with high catalytic performance. This heterojunction was employed as a photo-Fenton catalyst to synergistically remove Cr(VI) and levofloxacin (LEV). The TiO2/α-Fe2O3/Fe-g-C3N4 heterojunction enhanced the intensity of the visible light response and suppressed the recombination of photogenerated electrons and holes. The N-Fe-O bridge, formed by synergistic coordination effects, enhanced the charge lifetime by decreasing the impedance of the catalyst and increasing the electron transfer rate. Additionally, the Fermi level and work function of the sample were calculated, providing further evidence for the electron transfer. Direct electron transfer between TiO2/α-Fe2O3/Fe-g-C3N4 and LEV/Cr(VI) was observed, indicating its importance in the removal of pollutants. To determine the potential degradation pathways, the energy orbitals of LEV derived from DFT calculations were analyzed. Overall, the study presents an excellent strategy for the sustainable use of RIS and the preparation of highly active catalysts. In conclusion, TiO2/α-Fe2O3/Fe-g-C3N4 is predicted to considerably contribute to studies on treating heavy metal and organic pollutant-contaminated wastewater.

High-Loading Lithium-Sulfur Batteries with Solvent-Free Dry-Electrode Processing.

Lithium-sulfur (Li-S) batteries, with their high energy density, nontoxicity, and the natural abundance of sulfur, hold immense potential as the next-generation energy storage technology. To maximize the actual energy density of the Li-S batteries for practical applications, it is crucial to escalate the areal capacity of the sulfur cathode by fabricating an electrode with high sulfur loading. Herein, ultra-high sulfur loading (up to 12mgcm-2) cathodes are fabricated through an industrially viable and sustainable solvent-free dry-processing method that utilizes a polytetrafluoroethylene binder fibrillation. Due to its low porosity cathode architecture formed by the binder fibrillation process, the dry-processed electrodes exhibit a relatively lower initial capacity compared to the slurry-processed electrode. However, its mechanical stability is well maintained throughout the cycling without the formation of electrode cracking, demonstrating significantly superior cycling stability. Additionally, through the optimization of the dry-processing, a single-layer pouch cell with a loading of 9mgcm-2 and a novel multi-layer pouch cell that uses an aluminum mesh as its current collector with a total loading of 14mgcm-2 are introduced. To address the reduced initial capacity of dry-processed electrodes, strategies such as incorporating electrocatalysts or employing prelithiated active materials are suggested.

Hot-Pressing Enhances Mechanical Strength of PEO Solid Polymer Electrolyte for All-Solid-State Sodium Metal Batteries.

Poly(ethylene oxide) (PEO)-based solid polymer electrolytes (SPEs) are widely utilized in all-solid-state sodium metal batteries (ASSSMBs) due to their excellent flexibility and safety. However, poor ionic conductivity and mechanical strength limit its development. In this work, an emerging solvent-free hot-pressing method is used to prepare mechanically robust PEO-based SPE, while sodium superionic conductors Na3Zr2Si2PO12 (NZSP) and NaClO4 are introduced to improve ionic conductivity. The as-prepared electrolyte exhibits a high ionic conductivity of 4.42×10-4 S cm-1 and a suitable electrochemical stability window (4.5V vs Na/Na+). Furthermore, the SPE enables intimate contact with the electrode. The Na||Na3V2(PO4)3@C ASSSMB delivers a high-capacity retention of 97.1% after 100 cycles at 0.5 C and 60°C, and exhibits excellent Coulombic efficiency (CE) (close to 100%). The ASSSMB with the 20µm thick electrolyte also demonstrates excellent cyclic stability. This study provides a promising strategy for designing stable polymer-ceramic composite electrolyte membranes through hot-pressing to realize high-energy-density sodium metal batteries.

Catalytic One-pot Solvent Free Synthesis, Biological Activity, and Docking Study of New Series of 1, 3-thiazolidine-4-one Derivatives Derived from 2- (P-tolyl) Benzoxazol-5-amine.

In this study, a simple triethylammonium salt of phosphoric acid (triethylammonium dihydrogen phosphate) (4) in the liquid state was utilized as an inexpensive, efficient one-pot three components, solvent-free synthesis of thiazolidine-4-one derivatives, with good to excellent yields. Techniques such as FT-IR, 1H-NMR, 13C-NMR, 13C-NMR-DEPT-135, and MS. were used for the structural elucidation. The high biotic efficiency of the newly obtained compounds was confirmed by in vitro antimicrobial action against Gram-positive (S. Aureus), Gram-negative bacteria (P. Aeruginosa and E. Coli) and antifungal activity (C. Albicans) via microplate titer dilution technique. Finally, a molecular docking study was performed with a resolved crystal structure of S. Aureus D-alanine alanyl carrier protein ligase (PDB ID: 7VHV). This investigation aimed to synthesize a new series of thiazolidine-4-one derivatives combined with benzoxazole moiety. Ionic liquid assistance one-pot solvent-free synthesis method used to synthesize a new series of thiazolidine-4-one derivative 10(a-e). Structural identification of new synthesis and biological evaluation via techniques of (IR, 1H-NMR, 13C-NMR, 13C-NMR-DEPT-135, and MS). Ionic liquid is utilized as an inexpensive, efficient one-pot three-component solvent-free synthesis of thiazolidine-4-one derivatives with good to excellent yields. Most of the synthesized compounds showed high biological and anti-fungal activity, in line with the docking study against mentioned microorganism and crystal structure of PDB (ID: 7VHV), respectively.

Preparation of environmental-benign castor oil-derived polyurethane thermal conductive structural adhesives with superior strength

Thermal conductive structural adhesives offer a robust solution for injection into the battery core of power battery packs in new energy vehicles, effectively providing filling, protecting, and facilitating timely heat dissipation. In this work, a series of castor oil (CO)-based polyurethane prepolymers with different isocyanate (NCO) contents were synthesized by a solvent-free method, which designated as Component B (curing agent) for the CO-based polyurethane (CIPU) adhesives. Polyaspartic acid ester (PAE) resin compounded with poly (tetramethylene ether glycol) (PTMG) of different molecular weights, constituted Component A of the CIPU adhesives. The effect of mass ratio of PAE to PTMG (M value) on mechanical performance of the CIPU adhesives under different curing agent conditions was investigated. The results indicated optimal overall performance for the CIPU adhesive with an M value of 3, exhibiting a tensile strength of 10.25 MPa, an elongation at break of 107.14%, and a steel-steel tensile shear strength of 4.7 MPa. Subsequently, a series of CIPU thermal conductive structural adhesives were prepared by introducing thermal conductive fillers into the optimized CIPU adhesive formula. The introduction of a 35% Boron nitride content yielded a CIPU thermal conductive structural adhesive with a thermal conductivity of 0.64 W/m·K, and a steel-steel tensile shear strength of 6.97 MPa. These innovative CIPU thermal conductive structural adhesives prepared herein are expected to be applied in the new energy automotive and electronics industries.

Solvent-free preparation of high synthetic yield carbon dots from sodium ligninsulfonate for on-site detection of formaldehyde in the environment

Formaldehyde (FA), as a widespread toxic pollutant in cars, furniture and construction materials, has been implicated in hazardous health effects on the human body. This paper presents a green and large-scale preparation of carbon dots (CDs) using sodium ligninsulfonate and o-phenylenediamine through a solvent-free reaction method. The prepared CDs exhibit a synthetic yield of 43 % and show green fluorescence. In addition, the CDs can be employed as an ideal fluorescent FA probe, exhibiting excellent linearity within the range of 0–50 μM (R2 = 0.998, limit of detection (LOD) = 79 nM). By taking advantage of the obvious color changes in detection, the droplet detection system is investigated for on-site visual detection of indoor FA gas. This work not only contributes to the efficient utilization of agricultural waste but also represents a significant process in the development of FA on-site detection.

PFAS-free superhydrophobic chitosan coating for fabrics

In view of health and environmental concerns, together with the upcoming restrictive regulations on per- and polyfluoroalkyl substances (PFAS), less impactful materials must be explored for the hydrophobization of surfaces. Polysaccharides, and especially chitosan, are being explored for their desirable properties of film formation and ease of modification. We present a PFAS-free chitosan superhydrophobic coating for textiles deposited through a solvent-free method. By contact angle analysis and drop impact, we observe that the coating imparts hydrophobicity to the fabrics, reaching superhydrophobicty (θA = 151°, θR = 136°) with increased amount of coating (from 1.6 g/cm2). This effect is obtained by the combination of chemical water repellency of the modified chitosan and the nano- and micro-roughness, assessed by SEM analysis. We perform a comprehensive study on the durability of the coatings, showing good results especially for acidic soaking where the hydrophobicity is maintained until the 8th cycle of washing. We assess the degradation of the coating by a TGA-IR investigation to define the compounds released with thermal degradation, and we confirm the coating's biodegradability by biochemical oxygen consumption. Finally, we demonstrate its biocompatibility on keratinocytes (HaCaT cell line) and fibroblasts (HFF-1 cell line), confirming that the coating is safe for human skin cells.

Boosting the Interfacial Stability of the Li6PS5Cl Electrolyte with a Li Anode via In Situ Formation of a LiF-Rich SEI Layer and a Ductile Sulfide Composite Solid Electrolyte.

Due to its good mechanical properties and high ionic conductivity, the sulfide-type solid electrolyte (SE) can potentially realize all-solid-state batteries (ASSBs). Nevertheless, challenges, including limited electrochemical stability, insufficient solid-solid contact with the electrode, and reactivity with lithium, must be addressed. These challenges contribute to dendrite growth and electrolyte reduction. Herein, a straightforward and solvent-free method was devised to generate a robust artificial interphase between lithium metal and a SE. It is achieved through the incorporation of a composite electrolyte composed of Li6PS5Cl (LPSC), polyethylene glycol (PEG), and lithium bis(fluorosulfonyl)imide (LiFSI), resulting in the in situ creation of a LiF-rich interfacial layer. This interphase effectively mitigates electrolyte reduction and promotes lithium-ion diffusion. Interestingly, including PEG as an additive increases mechanical strength by enhancing adhesion between sulfide particles and improves the physical contact between the LPSC SE and the lithium anode by enhancing the ductility of the LPSC SE. Moreover, it acts as a protective barrier, preventing direct contact between the SE and the Li anode, thereby inhibiting electrolyte decomposition and reducing the electronic conductivity of the composite SE, thus mitigating the dendrite growth. The Li|Li symmetric cells demonstrated remarkable cycling stability, maintaining consistent performance for over 3000 h at a current density of 0.1 mA cm-2, and the critical current density of the composite solid electrolyte (CSE) reaches 4.75 mA cm-2. Moreover, the all-solid-state lithium metal battery (ASSLMB) cell with the CSEs exhibits remarkable cycling stability and rate performance. This study highlights the synergistic combination of the in-situ-generated artificial SE interphase layer and CSEs, enabling high-performance ASSLMBs.

Mild and Efficient Preparation of N-Heterocyclic Organic Molecules by Catalyst-free and Solvent-free Methods.

The small organic molecular compounds with biological activity containing C-C and C-N or C-O bonding were efficiently prepared without catalyst and solvent in the hydrothermal synthesis reactor. Our goal was to explore new applications for the more environmentally friendly and efficient synthesis of bis(indolyl)methyl, xanthene, quinazolinone, and N-heterocyclic derivatives in hydrothermal synthesis reactors under solvent-free and catalyst-free conditions. A greener and more efficient method was successfully developed for the synthesis of bis(indolyl)methyl, heteroanthracene, quinazolinone, and N-heterocyclic derivatives using a hydrothermal synthesis reactor in a solvent- and catalyst-free manner. In a hydrothermal synthesis reactor, bis(indoyl)methyl, xanthene, quinazolinone, and N-heterocyclic derivatives were synthesized without catalysts and solvents. Overall, it is proved once again that the catalyst-free and solvent-free synthesis method has universal value and is a more ideal and environmentally friendly new method, especially the hydrothermal reactor for synthesis.

Strong microwave absorption performance of simply grinding FAPbI3/CNTs composite absorbers

The distinctive physical and chemical characteristics of organic-inorganic lead halide perovskite make it a promising candidate for microwave absorption applications. However, the high-efficiency microwave absorption of halide perovskite-based composites is concentrated at high frequencies, while electronic equipment operates at low-frequency bands. Exploring simple and efficient methods to achieve optimal microwave absorption efficiency at low frequencies continues to pose a considerable challenge. Here, FAPbI3 was synthesized by a simple solvent-free hand grinding method and mixed with carbon nanotubes (CNTs) to obtain a series of FAPbI3/CNTs (FC) composites. By modulating the mass ratio of the components, FAPbI3 modulates the absorption bands, CNTs can effectively establish a conductive network to enhance both polarization loss and conductive loss and regulate impedance matching. The lower permittivity of FAPbI3 gives FC an advantage in terms of low-frequency microwave absorption. The FC-4 composite exhibits a minimum reflection loss (RLmin) of −55.67 dB at a low frequency of 6.88 GHz with a thickness of 3.5 mm. Meanwhile, microwave absorption performance can reach 99 % covering almost the entire C band when utilizing a thickness ranging from 3 to 5 mm. Additionally, according to adjusting the load of FAPbI3 in the mixture, the FC-3 composite displays the highest microwave absorption value among the composites based on halide perovskites. With a thickness of 1.4 mm, the reflection loss at 17.4 GHz reaches an impressive minimum value of −71.89 dB. This study represents the first research specifically focused on FAPbI3 perovskite in the domain of microwave absorption. FC composites display remarkable capabilities in absorbing microwaves, indicating their promising prospects for advancement within the realm of microwave absorption. This research may provide valuable insights for the design of low-frequency and high-efficiency microwave absorbers.

Solvent-Free Reaction for Unsymmetrical Organodisulfides with High Purity and Application as Cathode-Active Materials.

Unsymmetrical disulfides, in which different organic groups are bonded to disulfide bonds, have been synthesized by cross-coupling reactions using thiols as substrates. However, due to the low-binding energy of unsymmetrical disulfides, its disproportionation occurs based on the side reactions with nucleophilic thiols, resulting in the impurity of symmetric disulfides. In this study, we developed a solvent-free synthesis method for unsymmetrical disulfides using thiosulfonates, thiols, and a base. This synthetic method enabled us to obtain highly pure diaryl-substituted unsymmetrical disulfides with particularly low-binding energy without control over the nucleophilicity and elimination properties of the substrate. Furthermore, it was observed that the disproportionation of unsymmetrical disulfides occurred in the solvent. This means that solvent-free condition is one of the factors to obtain unsymmetrical disulfides. As a new application of unsymmetrical disulfides, we applied unsymmetrical disulfides to cathode active materials of lithium batteries based on the reversible multi-electron redox activity of S-S bonds. The batteries using unsymmetrical disulfide cathode-active materials with a carbon nanotube exhibited initial capacities of 127 and 158 Ah/kg, equal to 42 and 53% of their theoretical ones. We demonstrated that unsymmetrical disulfides could be used as cathode-active materials for rechargeable batteries.

Solvent-free synthesis of foam board-like CoSe2 alloy to selectively generate singlet oxygen via peroxymonosulfate activation for sulfadiazine degradation

Singlet oxygen (1O2) is a highly effective reactive species in selectively oxidizing organic pollutants. However, it is still challenging to rationally design robust catalysts for the selective generation of 1O2. Herein, the coordination and engineering architecture of the foam board-like CoSe2 alloy were facilely constructed through a green solvent-free method and displayed almost 100% 1O2 production selectivity. The CoSe2 alloy showed excellent catalytic ability for the efficient and fast removal of organic pollutants via peroxymonosulfate (PMS) activation compared with previously reported cobalt-based catalysts. The CoSe2/PMS system exhibited strong resistance for a broad pH range (3.0–11.0) and various coexisting inorganic ions owing to the advantage of the strong bonding of Co-Se in CoSe2 alloy. Mechanism studies revealed that 1O2 was the only reactive oxygen species in the CoSe2/PMS system. Theoretical calculations demonstrated that Co was the dominant adsorption site for PMS in CoSe2, and the production pathway of 1O2 was PMS* → *OH → *O → 1O2. In addition, it was proved that *OH and *O served as the rate-determining steps for the formation of 1O2 by PMS activation on CoSe2 alloy. These findings provide a rational strategy for preparing a series of low-cost transition metal-based alloy catalysts for PMS activation to achieve high-efficiency 1O2 production in the elimination of organic pollutants.

Comparative assessment of phenolic composition profile and biological activities of green extract and conventional extracts of Salvia sclarea

In recent years, there have been an attempt to develop safe and environmental friendly solvents to replace conventional solvents, and use for extraction bioactive compounds from natural sources. A current investigation involved the preparation of green, methanolic, and ultrasonic extracts of S. sclarea, and compared their phenolic profiling using HPLC–DAD, antibacterial, antioxidant, and enzyme inhibition activities. The HPLC–DAD analysis revealed that Rosmarinic acid was the main content in all extracts, with Ellagic acid only present in the green extract. The green extract exhibited superior anti-biofilm activity against S. Aureus and E. Faecalis compared to the other extracts at MIC concentration. Furthermore, the green extract also displayed the highest inhibition of swarming motility in P. Aeruginosa with inhibition range 68.0 ± 2.1 (MIC) to 19.5 ± 0.6 (MIC/4). and better enzyme inhibitory activity against BChE (with IC50 = 131.6 ± 0.98 µg/mL) and AChE (with inhibition 47.00 ± 1.50%) compared to the other extracts; while, the ultrasonic extract showed strong inhibition of violacein production by C. Violaceum with a inhibition range 05.5 ± 0.1 (MIC/32) to 100 ± 0.00 (MIC), followed by the green extract with a inhibition range 15.0 ± 0.5 (MIC/8) to 100 ± 0.00 (MIC), additionally, the ultrasonic and methanoic extracts showed significant activity against urease enzyme with (IC50 = 171.6 ± 0.95 µg/mL and IC5 0 = 187.5 ± 1.32 µg/mL) respectively. Both the green and methanolic extracts showed considerable antioxidant activities, as β-carotene-linoleic acid (IC50 = 5.61 ± 0.47 µg/mL and 5.37 ± 0.27 µg/mL), DPPH· (IC50 = 19.20 ± 0.70 µg/mL and 16.31 ± 0.23 µg/mL), ABTS·+(IC50 = 8.64 ± 0.63 µg/mL and 6.50 ± 0.45 µg/mL) and CUPRAC (A0.5 = 17.22 ± 0.36 µg/mL and 12.28 ± 0.12 µg/mL) respectively, likewise the green extract performing better in metal chelating compared to the other extracts. The green extraction is reported as a cost effective and solvent free method for extracting natural products that produces compounds free of toxic chemicals. This could be the method to be used in the industries as a renewable method.

Construction of MoS42− intercalated NiAl-layered double hydroxide by solvent-free method for promoting photocatalytic degradation of antibiotics: Synergistic effect of oxygen vacancies and electron-rich groups

MoS42− intercalated NiAl-layered double hydroxides (LDH) were prepared by solvent-free techniques, which possessed oxygen vacancies and efficient electron transfer channels. Oxygen vacancies were increased with increasing of the MoS42− intercalation amount. Through X-ray Photoelectron Spectroscopy (XPS), Electron Paramagnetic Resonance (EPR), Kelvin Probe Force Microscopy (KPFM), and Density Functional Theory (DFT), the presence of oxygen vacancies and electron transfer channels were confirmed. In the meantime, the formation mechanisms of electron transfer channels and the synergistic mechanisms involving oxygen vacancies and electron transfer channels were illustrated. Electrochemical characterization revealed that compared with LDH, the electron lifetime of LDH-WM-0.5 increased from 1.70 ns to 2.88 ns, and the recombination efficiency of electron holes was reduced by about 6 times. Degradation experiments demonstrated that the degradation rate of tetracycline by LDH-WM-0.5 increased from 19.0 % to 90.0 % in 3 h, representing a 4.5-fold improvement compared to LDH photocatalysts. This study contributed novel insights into developing advanced photocatalysts by strategically manipulating the presence of oxygen vacancies and constructing the electron transfer channels.

Sequential-Dispersion PGSS process applied to lutein encapsulation at moderate temperatures: A solvent-free method for thermosensitive compound encapsulation

Sequential-Dispersion Particles from Gas Saturated Solutions (SD-PGSS) process was applied to encapsulate lutein with biocompatible polymer excipients to elaborate drug-delivery particles for oral uptake at mild temperatures (38 and 45 °C) under 25 MPa. Polycaprolactone and a polycaprolactone/polyethyleneglycol mixture (1:1 w/w) were selected to modulate in-vitro release. An experimental setup was designed in-house to limit the challenging plugging issues often encountered with the PGSS process. In this study, process yields up to 94% were obtained. The drug precipitation yields varied from 43 to 61% and the homogeneity of lutein dispersion was demonstrated for all conditions. In-vitro release kinetics were performed in phosphate-buffered saline solutions for 8 h. A higher release of lutein was obtained from PCL/PEG blends (∼ 90% in 5 h), whereas only 56% were released from pure PCL formulations. This study highlights the potential of the SD-PGSS process in encapsulating thermosensitive compounds at moderate temperatures.

A facile method to prepare biobased flexible polydimethylsiloxane − Benzoxazine resin: Dielectric properties and high heat resistance

For the benefit of meet the industrial demand of integrated circuits for low dielectric constant (k) and the environmental requirements of sustainable development, it is important to prepare biobased benzoxazine resin with low k and high heat resistance by solvent-free method. In this paper, the biobased monomer V-fa containing aldehyde group was synthesized by biobased raw materials furfurylamine and vanillin, and then reacted with amino-terminated polydimethylsiloxane (PDMS) to prepare benzoxazine monomer V-fa-pdms containing schiff base structure by a solvent-free method. Then, the monomer was cured to obtain biobased benzoxazine resin poly(V-fa-pdms), and the heat resistance, mechanical and dielectric properties of poly(V-fa-pdms) were studied. The results indicate that the resin exhibits excellent thermal stability and toughness by combining benzoxazine and PDMS reasonably. The initial thermal decomposition temperature (Tdi, 5% thermogravimetric loss) is 387 °C, and the material also exhibits excellent dielectric properties. When the frequency increases from 1 Hz to 1 MHz, the k of the material decreases from 2.71 to 2.60, and the fluctuation range of dielectric loss is 0.0051–0.0049. With the increase of frequency, both k and dielectric loss show a downward trend. At the same time, the material shows good corrosion resistance in commonly used solvents. These excellent properties of poly(V-fa-pdms) are due to the existence of a high cross-linked network structure formed by multiple cross-linking sites in the polymer network and the combined effect of low k and high heat-resistant PDMS components.

Bridging solvent-free polyamic acid and epoxy resin by Si-O-C hyperbranched polymer for enhanced compatibility, toughness and self-lubrication performance

Despite the great application potential of epoxy resin (EP) modified with polyamic acid (PAA), the large amount of high-boiling-point non-protonic polar solvents used to promote their compatibility cannot be completely eliminated, which affects the fabrication and application of epoxy composites in practical engineering. Herein, PAA was prepared by solvent-free ball milling method, and then the primary amine hyperbranched polysiloxane (HSiNH2) was prepared by “one-pot” method as the “bridging structure” to improve the compatibility between PAA and EP. Compared to neat EP, the flexural, impact and tensile shear strength of the epoxy composite are increased by 22.2 %, 30.0 % and 23.2 %, while the average friction coefficient and volume wear rate are reduced by 26.5% and 20.6% under the contents of PAA and HSiNH2 are 1.50 wt% and 2.0 wt%, respectively. Moreover, the material exhibits excellent thermal properties. By comprehensively analyzing the structure and properties of the epoxy composite, it is mainly ascribed to the fact that HSiNH2 with a large number of reactive groups acted as a “bridging structure” to enhance the compatibility of PAA and EP, which results in the epoxy composite having excellent mechanical, tribological and thermal properties. This research also lays the theoretical foundation for the development of high-performance epoxy composites in aerospace.

Highly efficient DES-based catalytic systems for carbon dioxide utilization via cycloaddition with epoxide substrates

The accumulation of greenhouse gases (GHG) in the atmosphere, with carbon dioxide being the most significant contributor, is a major environmental problem as it impacts significantly on climate change. The development of new catalysts and chemical reactions that incorporate CO2 are needed to reduce its further emission significantly. Deep eutectic solvents (DES) have garnered increasing attention as environmentally friendly catalysts in the cycloaddition of carbon dioxide (CO2) with epoxide substrates to produce cyclic carbonates. Their appeal stems from their facile synthesis, cost-effectiveness, low vapour pressure, and thermal stability. In this study, we present a convenient solvent-free synthesis method for nine deep eutectic solvents (DES), utilizing varying compositions of quaternary amine salts (N,N,N-triethyldodecan-1-aminium hydroxide, [TEA-12][OH]) and quinaldic acid [Q-COOH]. These deep eutectic solvents were thoroughly characterized using several techniques, including FTIR, NMR, DSC, and TGA. Moreover, their efficacy for the solvent-free fixation of CO2 to cyclic carbonates were evaluated. Among the tested compositions, [TEA-12]:[Q-COOH] (0.9:0.1) exhibited the lowest melting point (100.17 °C) and highest catalytic activity, showcasing an optimized Turn-Over Frequency (TOF) of 1466 h−1. This remarkable result represents a significant advancement in the application of DES for CO2 fixation, exceeding the previous highest catalytic activity observed with TBAB:Citric acid (2.5:1) by more than tenfold.

Solvent-Free Method for Masking the Bitter Taste of Azithromycin Dihydrate Using Supercritical Fluid Technology

ABSTRACT Introduction and purpose The unpleasant extremely bitter taste of the orally administered broad-spectrum antibiotic azithromycin decreases patient compliance, especially in pediatrics. This issue can be overcome by decreasing drug interaction with the tasting buds using insoluble polymers at salivary pH (6.8 -7.4), like the cationic polymer Eudragit EPO. Supercritical fluid technology is a green synthesis method for preparing pharmaceutical preparations that replace organic solvents with safe supercritical CO2. This study aimed to mask the bitter taste of azithromycin using the supercritical fluid method and a pH-sensitive Eudragit EPO polymer. Methods: A foaming process was investigated for preparing a formulation (TEST), which comprises treating the polymer with supercritical carbon dioxide (CO2) fluid to prepare a taste-masked dosage form without employing organic solvents or flavors. Results: The use of the supercritical technique at 40 °C and 10 MPa for two hours allowed the manufacturing of solvent-free polymeric foam with azithromycin dispersions; the average calculated percentage of apparent volume change was 62.5 ± 5.9% with an average pore diameter of 34.879 Å. The formulated sample showed low drug release in simulated salivary fluid while keeping its crystalline nature. Moreover, clinical studies on healthy subjects showed that the formula successfully masked azithromycin's bitter taste. Conclusions: Overall, it has been shown herein that the supercritical fluid technology foaming method is promising in masking the bitter taste of bitter ingredients.