Differential Scanning Calorimetry Research Articles

The effect of polycaprolactone polyol molecular weight and chain extender type on the physico-mechanical properties and gas permeability of polyurethane thermoplastic elastomer membranes

ABSTRACT In this study, polyurethane thermoplastic elastomers (TPU) were synthesized using isophorone diisocyanate (IPDI), 1,4-butanediol (BDO), and 1,6-hexanediol (HDO) as the chain extenders, and polycaprolactone diol (PCL-diol) with three different molecular weights (2000, 4000, and 10,000 g/mol) as polyols. Fourier transform infrared (FTIR) spectroscopy, X-ray diffraction (XRD) patterns, and differential scanning calorimetry (DSC) were conducted to analyze the chemical microstructure and phase morphology of the prepared samples. The results showed that the change in the chain extender’s type (BDO and HDO) leads to a decrease in the hydrogen bonding index (HBI). Increasing the molecular weight of PCL-diol in BDO-based TPUs has led to an increase in their crystallinity, Young’s modulus, melting temperature, tensile strength, and a decrease in glass transition temperature and elongation at break. Moreover, the increase in the molecular weight of PCL-diol in HDO-based TPUs demonstrated an increase in the crystallinity and elongation at break and tensile strength up to the molecular weight 4000 in PCL-diol, after that, there was a decrease in those properties due to the increase of the soft segments content and change in the chain extender type. Permeability on TPU membranes was performed for N2 and CO2 at three different pressures 3, 6, and 9 atm at room temperature. An increase in pressure led to an increase in membrane permeability due to the increase in gas solubility in TPU based on Henry’s law. The permeability of CO2 is higher than N2 due to the proper interactions of CO2 gas with the polar carbonyl groups of polyurethane. It is observed that the permeability increases in BDO-based samples with an increase in the molecular weight of PCL-diol, while the increase in permeability of HDO-based TPU is up to PCL-diol molecular weight 4000 and after that is decreased. The selectivity of CO2 has decreased with increasing pressure due to the higher rate of dissolution of N2 at higher pressures.

Effect of Oligoricinoleic Acid on Degradation of Polylactic Acid

ABSTRACT The objective of this research is to explore the impact of oligoricinoleic acid (ORA) on the degradation of polylactic acid (PLA). ORA was synthesized from ricinoleic acid using tin (II) 2-ethylhexanoate as a catalyst. The chemical structures of the obtained ORA were confirmed by Fourier-transform infrared spectrometer (FT-IR) and proton nuclear magnetic resonance spectroscopy (1H-NMR). PLA/ORA films were prepared through the casting method by varying ORA concentrations as 0.1%wt, 0.3%wt, 0.5%wt, 1.0 wt%, and 3.0%wt. Degradation of the films via hydrolysis was studied by soaking the films in deionized water and stirring at 120 rpm in an incubator at 37°C. Alterations in the structure and properties of the films were investigated after soaking for 7, 14, 21, and 28 days using ultraviolet-visible spectroscopy (UV-Vis), Fourier-transform infrared spectrometer (FTIR), scanning electron microscope (SEM), X-ray diffraction (XRD), differential scanning calorimeter (DSC), thermogravimetric analysis (TGA), and universal testing machine (UTM). Gel permeation chromatography (GPC) was performed to confirm the decrease in molecular weight (MW). The presence of 3%wt ORA could promote both ductility and degradation of PLA films. ORA further enhances thermal stability, indicating potential for prevention of thermal degradation during melt processing.

Zein/fucoidan-coated phytol nanoliposome: preparation, characterization, physicochemical stability, in vitro release, and antioxidant activity.

To improve phytol bioavailability, a novel method of magnetic stirring and high-pressure homogenization (HPH) combination was used to prepare zein/fucoidan-coated phytol nanoliposomes (P-NL-ZF). The characterization, the simulated in vitro digestion, and the antioxidant activity of these phytol nanoliposomes from the different processes have been studied. Based on the results of dynamic light scattering (DLS) and gas chromatography-mass spectrometer (GC-MS) analysis, P-NL-ZF prepared through the combination of magnetic stirring and HPH exhibited superior encapsulation efficiency at 76.19% and demonstrated exceptional physicochemical stability under a series of conditions, including storage, pH, and ionic in comparison to single method. It was further confirmed that P-NL-ZF by magnetic stirring and HPH displayed a uniform distribution and regular shape through transmission electron microscopy (TEM). Fourier-transform infrared (FTIR) spectroscopy and differential scanning calorimetry (DSC) analysis showed that electrostatic interactions and hydrogen bonding were the primary driving forces for the formation of composite nanoliposomes. Additionally, an in vitro digestion study revealed that multilayer composite nanoliposomes displayed significant and favorable slow-release properties (58.21%) under gastrointestinal conditions compared with traditional nanoliposomes (82.36%) and free phytol (89.73%). The assessments of chemical and cell-based antioxidant activities demonstrated that the coating of zein/fucoidan on phytol nanoliposomes resulted in enhanced effectiveness in scavenging activity of ABTS free radical and hydroxyl radical and mitigating oxidative damage to HepG2 cells. Based on our studies, the promising delivery carrier of zein/fucoidan-coated nanoliposomes is contributed to the encapsulation of hydrophobic natural products and enhancement of their biological activity. © 2024 Society of Chemical Industry.

Non-Isochronal Behavior of Charge Transport at Liquid-Liquid and Liquid-Glass Transition in Aprotic Ionic Liquids.

A reversible, first-order transition separating two liquid phases of a single-component material is a fascinating yet poorly understood phenomenon. Here, we investigate the liquid-liquid transition (LLT) ability of two tetraalkylphosphonium ionic liquids (ILs), [P666,14]Cl and [P666,14][1,2,4-triazolide], using differential scanning calorimetry and dielectric spectroscopy. The latter technique also allowed us to study the LLT at elevated pressure. We found that cooling below 205 K transforms [P666,14]Cl and [P666,14][Trz] from one liquid state (liquid 1) to another (the self-assembled liquid 2), while the latter facilitates the charge transport decoupled from structural dynamics. In contrast to temperature, pressure was found to play an essential role in the self-organization of a liquid 2 phase, resulting in different time scales of charge transport for rapidly and slowly compressed samples. Furthermore, τσ(PLL) was found to be much shorter than τσ(TLL, P=atm), which constitutes the first example of non-isochronal behavior of charge transport at LLT. In turn, dielectric studies through the liquid-glass transition revealed the non-monotonic behavior of τσ at elevated pressure for [P666,14]Cl, while for [P666,14][Trz] τσ(Pg) was almost constant. These results highlight the diversity of liquid-liquid transition features within the class of phosphonium ionic liquids.

Supertoughened Polylactic Acid/Polybutylene Adipate Terephthalate Blends Compatibilized with Ethylene-Methyl Acrylate-Glycidyl Methacrylate: Morphology and Mechanical Properties by the Response Surface Methodology.

Optimized extrusion melt-blending of polylactic acid (PLA) polymer with a minor biopolymeric phase, polybutylene adipate terephthalate (PBAT), and compatibilized with random ethylene-methyl acrylate-glycidyl methacrylate terpolymer (EMA-GMA, Trademark: Lotader AX-8900) led to an outstanding improvement in mechanical properties. At the noncompatibilized PLA-PBAT (80-20) blend point, significant enhancement (∼4500%) in toughness and elongation-at-break was already obtained without compromising any elastic properties. The effect of the compatibilizer content on the mechanical properties of the PLA-PBAT (80-20) blend was investigated by an optimal custom response surface methodology. Thus, 2 wt % Lotader content was determined to be optimal by a numerical optimization methodology with a desirability value, D, of 0.882 to maximize toughness and elongation-at-break. The compatibilization and thermal behavior of the Lotader-modified blends were analyzed by scanning electron microscopy (SEM), differential scanning calorimetry (DSC), and thermogravimetric analysis (TGA). Upon adding the compatibilizer, the original phase-separated morphology of the blends changed from PBAT quasi-spherical domains to nearly elongated elliptical ones. It was also found that the interfacial boundary line of the domains faded away, which revealed that interfacial compatibility was achieved. The thermostability of the blends remained largely unaltered following the incorporation of PBAT and Lotader. Moreover, while PBAT exhibited a minor influence on the crystallinity of PLA, Lotader had no discernible impact on crystallinity, as evidenced by the DSC thermograms. Thus, the compatibilizer at the optimal point in the optimized blend ratio led to the formation of a phase-separated morphology that combined internal cavitation, interfacial cavitation, and strong adhesion features at the right proportions in the microstructure which underlies the micromechanisms driving the remarkable enhancement of as much as 7100% in toughness and ductility.

Mechanical and thermal characterization of elastomer modified polypropylene hybrid composites reinforced with hazelnut shell and wollastonite fillers

AbstractThe demand for sustainable and recyclable materials in industrial applications has led to a surge in interest in green composites, particularly those incorporating natural fillers derived from agro‐food industry waste. This study investigates the mechanical and thermal properties of polypropylene (PP) hybrid composites filled with hazelnut shell and wollastonite, along with the effect of styrene‐ethylene/butylene‐styrene (SEBS) and SEBS‐g‐maleic anhydride (SEBS‐g‐MA) compatibilizers. Various characterization techniques, including tensile, flexural, and impact tests, as well as differential scanning calorimetry (DSC), thermogravimetry (TGA), and scanning electron microscopy (SEM) analyses, were employed to evaluate the composites. Results demonstrate that the addition of wollastonite significantly improves mechanical properties, while hazelnut shell filler affects thermal behavior and stability. SEBS and SEBS‐g‐MA compatibilizers enhance impact resistance; however, they lead to a decrease in other mechanical properties. DSC and TGA analyses demonstrate changes in crystallization behavior and thermal stability due to filler and compatibilizer incorporation. SEM microstructure images show the distribution of SEBS and SEBS‐g‐MA within the composite structure, affecting mechanical and thermal properties. Overall, this study highlights the importance of filler selection, compatibilizer addition, and their distribution in attaining desired properties for industrial applications. Future research should focus on optimizing formulations for specific uses and assessing long‐term performance under real‐world conditions.

Characterization of fly ash reinforced wood polypropylene composites

In this study, fly ash, which is released as waste from thermal power plants and has negative effects on the environment, was evaluated as a filler in wood-plastic composite materials (WPC). For this purpose, inorganic fly ash from thermal power plants was mixed with polypropylene (PP) thermoplastic polymer at 10%, 20%, 30%, 40%, and 50% by extrusion method instead of wood flour used in wood plastic composite materials. Maleic anhydride-treated polypropylene (MAPP) was used to strengthen the bonding during WPC production. The material mixed in extrusion was passed through a crusher and turned into pellets. Test samples were prepared using injection molding of pelletized WPC material. Density, thickness swelling, water absorption, modulus of rupture, impact strength, modulus of elasticity in bending, tensile strength, janka hardness, differential scanning calorimetry (DSC), and thermogravimetric analyses (TGA) were performed on the prepared test samples. The results indicated that as the amount of fly ash used in the wood-plastic composite material increases, the density increases but the thermal degradation temperature of the material, water uptake, the swelling ratio to its thickness, tensile strength, impact strength, janka hardness, modulus of rupture, and modulus of elasticity decrease.

Effect of copper in the stabilization of Al/CuO energetic semiconductor bridge

The long-term storage performance of energetic multilayer nanofilms is of great significance for their applications. In this paper, it is proposed to add a 10 nm Cu barrier layer between Al/CuO composite films to increase their storage stability. The Al/CuO composite film and Al/Cu/CuO composite film were aged for 14 days in an environment with a relative humidity of 40% and a temperature of 71 °C. Scanning electron microscopy and differential scanning calorimetry were used to analyze the microstructure and thermodynamic properties of the energetic films before and after aging, and the electrical detonation performance and ignition ability of energy-containing semiconductor bridges were studied. The results indicate that after aging for 14 days in an environment with a relative humidity of 40% and a temperature of 71 °C, the Al layer of the Al/CuO composite film becomes thinner, the Al2O3 interface layer increases, and the heat release decreases. The interlayer microstructure of the Al/Cu/CuO energetic multilayer nanofilms did not change significantly, and the addition of a 10 nm Cu layer formed a low-temperature Al–Cu alloy, reducing the reaction initiation temperature from 626 to 570 °C. The critical ignition time and critical ignition energy of the Al/CuO-energetic semiconductor bridge (ESCB) increased, the flame duration shortened from 440 to 300 μs, the flame size decreased by 50%, the plasma temperature decreased, and aging had no significant effect on the electrical explosion performance of Al/Cu/CuO-ESCB. After aging for 14 days in an environment with a relative humidity of 40% and a temperature of 71 °C, the maximum ignition gap of B/KNO3 for Al/CuO-ESCB decreased from 1.4 to 1.2 mm, while the maximum ignition gap for Al/Cu/CuO-ESCB remained at 1.6 mm, which significantly improved the ignition performance and long storage performance of the energetic semiconductor bridge.

"Dissolve-on-Demand" 3D Printed Materials: Polymerizable Eutectics for Generating High Modulus, Thermoresponsive and Photoswitchable Eutectogels.

Solvent-free photopolymerization of vinyl monomers to produce high modulus materials with applications in 3D printing and photoswitchable materials is demonstrated. Polymerizable eutectic (PE) mixtures are prepared by simply heating and stirring various molar ratios of N-isopropylacrylamide (NIPAM), acrylamide (AAm) and 2-hydroxyethyl methacrylate (HEMA). The structural and thermal properties of the resulting mixtures are evaluated by 1D and 2D NMR spectroscopy as well as differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA). UV photocuring kinetics of the PE mixtures are evaluated via in situ photo-DSC and photorheology measurements. The PE mixtures cure rapidly and display storage moduli that are orders of magnitude greater than equivalent copolymers cured in an aqueous medium. The versatility of these PE systems is demonstrated through the addition of a photoswitchable spiropyran acrylate monomer, as well as applying the PE formulation as a stereolithography (SLA)-based 3D printing resin. Due to the hydrogen-bonding network in PE systems, 3D printing of the eutectic resin is possible in the absence of crosslinkers. The addition of a RAFT agent to reduce average polymer chain length enables 3D printing of materials which retain their shape and can be dissolved on demand in appropriate solvents. This article is protected by copyright. All rights reserved.

Investigating the effect of electromagnetic field and Eucalyptus oil Citriodora on polymorphism of PVDF film

AbstractPolyvinylidene fluoride (PVDF) films were prepared for evaluating the effect of electromagnetic field and Eucalyptus oil Citriodora as an additive on the polymorphism. The values of PVDF crystalline phases were determined by attenuated total reflection‐Fourier transform infrared spectroscopy. Differential scanning calorimetry was performed to achieve the crystallinity degree of the PVDF films. To evaluate the impact of the electromagnetic field on the PVDF crystalline phases, the polymeric solution was placed in 1 tesla electromagnetic field for different times. The proper time for dominating the β phase was determined 10 min. Additionally, the sum of β and γ phases percentages augmented from 28.8 for the sample without the additive of Eucalyptus oil Citriodora to 65.2 for the sample containing 8% additive.

Dynamic covalent polymer network enabled bio‐based vitrimers with excellent substrate bonding

AbstractIn this article, we report the synthesis of dynamic covalent polymer network (DCPN)‐enabled vitrimers derived from gum rosin—a pine tree extract. The concept of Diels Alder (DA) thermo‐reversibility has been used to introduce self‐healing/dynamic covalent ability into the polymer systems. For this purpose, the diene moieties were incorporated in the gum rosin‐based polymer network, and the bismaleimides served as the dienophiles. The thermo‐reversible crosslinks formed between the diene and dienophile moieties can enhance the service life of the materials by improving the durability, mechanical as well as chemical properties of the materials. Upon damage, the thermo‐reversible DA bonds de‐crosslink resulting in smaller chain segments, enabling the material to flow to the site of damage and seal the fractured edges. The formation of DA crosslinks has been confirmed by using Fourier transform‐infrared spectroscopic technique. Scanning electron microscopy analysis was used to verify the self‐healing ability of the resin matrix. The healing process was studied after manual scratches were made. The polymers' ability to heal multiple times is investigated using differential scanning calorimetry. The adhesion strength of the self‐healing material has been examined on variety of substrates such as glass, steel, and concrete. The materials exhibited superior adhesion strength on glass substrate.

(Thermo)mechanical and chemical characteristics of photochemically crosslinked acrylates from bio‐ and fossil‐based origin

AbstractThe acrylates with oligomers and monomers from (partially) bio‐based feedstock become available at (semi‐)industrial scale, which can be processed through photochemical crosslinking for applications in coatings, additive manufacturing, electronics, or inks. Although fossil‐ and bio‐based acrylates may have a similar chemical composition, it requires good understanding of processing and structure–property relationships as minor changes in microstructure may strongly alter the performance. A comparative study on mechanical properties and chemical structure of bio‐ and fossil‐based acrylates with different functionalities and backbone structures reveals higher ductility of bio‐based acrylates, in relation with a more complex organization of the intrinsic molecular structure. The latter is confirmed by mechanical testing and visco‐elastic characteristics (dynamic mechanical analysis) yielding lower stiffness and higher dampening of bio‐based acrylates, in parallel with a lower glass transition temperature (differential scanning calorimetry). The complex molecular arrangements include a nanoscale morphology with ordered structure (X‐ray diffraction), conformational changes (infrared spectroscopy), and a residual high‐molecular weight fraction (size exclusion chromatography). The visco‐elastic calculations indicate only 4% to 5% lower crosslinking density and around 10% higher mean molar mass of the polymer chains segments between chemical crosslinks and trapped chain entanglements, which explain the unique structure and performance of bio‐based acrylates.

Effects of molecular interactions on the release of small molecules from silicone rubber

AbstractSilicone rubber is a good candidate as a carrier of small molecules in such applications as drug, fragrance and semiochemical delivery. When one matrix is loaded, the molecular interactions between the molecules and the matrix may affect their release rates. For this reason, it is important to investigate the effects of molecular interactions on release to better develop delivery systems with desirable release rates. In this study, the mass transfer and diffusion coefficients of three model molecules (i.e., octanol, octyl acetate, and octyl butyrate) were determined by monitoring their release from silicone rubber sheets loaded using headspace gas chromatography–mass spectrometry. Differential scanning calorimetry was used to characterize the plasticizing effects and Fourier transform infrared spectroscopy was used to characterize the molecular interactions. It was found that the release of octanol conformed to the Fickian diffusion pattern at 1 wt% initial concentration but deviated as the concentration increased due to hydrogen bonding between octanol and the silanol group of the silica filler. When two small molecules were released simultaneously, the effects of one molecule on the diffusion coefficient of the other differed, a result explained by the competing effects of plasticizing and hydrogen bonding.

Understanding the Impact of Chain Mobility on Conformational Evolution and Kinetics of Mesophase Formation in Poly(ʟ-lactide) under Low-Pressure CO2

Although the mesomorphic phase as an intermediate state has been introduced to understand polymer crystallization, the understanding of the mesomorphic phase is far from complete. Here, the effect of chain mobility on the mesophase structuring in melt-quenched poly(ʟ-lactide) (PLLA) treated in low-pressure CO2 at 1.6–2.0 MPa and 0 °C was investigated using infrared (IR) spectroscopy, differential scanning calorimetry (DSC), and atomic force microscopy (AFM). The IR and AFM results demonstrated that the final degree of order and the kinetics of structural evolution during the CO2-induced mesophase formation were critically dependent on the CO2 pressure. This was attributed to the distinct dynamics of conformational evolution (gg to gt conformer transition) due to the different CO2 pressures. The thermal behavior from the DSC results showed that CO2 pressure dominated both the scale and dynamics of the chain motion of PLLA. At a lower CO2 pressure of 1.6 MPa, smaller-scale segmental motion was not replaced by the larger-scale cooperative motion that occurred at a relatively higher CO2 pressure of 2 MPa, which was favorable for faster mesophase formation. Consequently, by inhibiting direct crystallization under limited mobility conditions, it was demonstrated that varying the chain mobility controlled by CO2 pressure and thus CO2 solubility impacted the dynamics of the mesophase formation of PLLA. The present results have implications for understanding the role of chain mobility in determining the intermediate structural phases in semicrystalline polymers.

Thermal behavior of Sicilian clay-based geopolymers

AbstractGeopolymers have been recently proposed for restoration of built heritage to substitute traditional mortars. Local materials and industrial wastes from the Italian region Sicily showed their potential as low-cost aluminosilicate sources for the preparation of geopolymers. Here, a set of Sicilian clays was studied by Thermogravimetry (TG) and Differential Scanning Calorimetry (DSC), and its mineralogical composition was evaluated by X-ray diffraction (XRD). The raw materials were used to prepare geopolymers by alkaline activation with or without the addition of silicate. The thermal degradation profile of the final materials was studied by TGA and compared with that of the precursors, and the energetics of dehydration were investigated by DSC. Two statistical analyses (made by Principal Component Analysis) were performed on the TG data of raw materials and geopolymers and on the TG data of geopolymers and their mineralogical composition, respectively. The last analysis in particular showed a correlation between the mineralogical composition of the materials and the samples' thermal properties. Additional studies of samples subject to accelerated aging by UV irradiation and exposure to acetic acid vapors highlighted the different effects of these two agents on the samples’ stability. Graphical abstract

Comparison of Sucrose and Trehalose for Protein Stabilization Using Differential Scanning Calorimetry.

The disaccharide trehalose is generally acknowledged as a superior stabilizer of proteins and other biomolecules in aqueous environments. Despite many theories aiming to explain this, the stabilization mechanism is still far from being fully understood. This study compares the stabilizing properties of trehalose with those of the structurally similar disaccharide sucrose. The stability has been evaluated for the two proteins, lysozyme and myoglobin, at both low and high temperatures by determining the glass transition temperature, Tg, and the denaturation temperature, Tden. The results show that the sucrose-containing samples exhibit higher Tden than the corresponding trehalose-containing samples, particularly at low water contents. The better stabilizing effect of sucrose at high temperatures may be explained by the fact that sucrose, to a greater extent, binds directly to the protein surface compared to trehalose. Both sugars show Tden elevation with an increasing sugar-to-protein ratio, which allows for a more complete sugar shell around the protein molecules. Finally, no synergistic effects were found by combining trehalose and sucrose. Conclusively, the exact mechanism of protein stabilization may vary with the temperature, as influenced by temperature-dependent interactions between the protein, sugar, and water. This variability can make trehalose to a superior stabilizer under some conditions and sucrose under others.

Symmetrical liquid crystalline dimers containing azo and azomethine linkages: synthesis, characterisation, mesomorphic study and DFT studies

ABSTRACT In the current study, one new series of symmetrical liquid crystalline homologous series of dimers with a rigid aromatic core with azo and azomethine group were synthesized using an ether-linking group. Several spectroscopic methods, including FT-IR, 1H-NMR, 13C-NMR and elemental analysis, were used to describe the synthesised dimers. The differential scanning calorimetry (DSC) and polarised optical microscopy (POM) were used to assess their mesomorphic properties. The results showed that the number of methylene spacers significantly affected the thermal properties of the synthesized dimers. To ascertain photophysical behaviour, UV-visible spectroscopy was employed. All the dimers of the present series show excellent enantiotropic nematic mesophase. The relationships between structure and its mesogenic property, the effects of various flexible spacers, the mesophase ranges, and the photo-isomerization of liquid crystalline dimers were all investigated. DFT study was carried out to gain a better understanding of structural features.

Thermosensitive and mucoadhesive gels containing solid lipid nanoparticles loaded with fluconazole and niosomes loaded with clindamycin for the treatment of periodontal diseases: a laboratory experiment

BackgroundPeriodontal diseases may benefit more from topical treatments with nanoparticles rather than systemic treatments due to advantages such as higher stability and controlled release profile. This study investigated the preparation and characterization of thermosensitive gel formulations containing clindamycin-loaded niosomes and solid lipid nanoparticles (SLNs) loaded with fluconazole (FLZ), as well as their in vitro antibacterial and antifungal effects in the treatment of common microorganisms that cause periodontal diseases.MethodsThis study loaded niosomes and SLNs with clindamycin and FLZ, respectively, and assessed their loading efficiency, particle size, and zeta potential. The particles were characterized using a variety of methods such as differential scanning calorimetry (DSC), dynamic light scattering (DLS), and Transmission Electron Microscopy (TEM). Thermosensitive gels were formulated by combining these particles and their viscosity, gelation temperature, in-vitro release profile, as well as antibacterial and antifungal effects were evaluated.ResultsBoth types of these nanoparticles were found to be spherical (TEM) with a mean particle size of 243.03 nm in niosomes and 171.97 nm in SLNs (DLS), and respective zeta potentials of -23.3 and -15. The loading rate was 98% in niosomes and 51% in SLNs. The release profiles of niosomal formulations were slower than those of the SLNs. Both formulations allowed the release of the drug by first-order kinetic. Additionally, the gel formulation presented a slower release of both drugs compared to niosomes and SLNs suspensions.ConclusionThermosensitive gels containing clindamycin-loaded niosomes and/or FLZ-SLNs were found to effectively fight the periodontitis-causing bacteria and fungi.

Synergistic Effect of PBz/Epoxy/PCLA Composite Films with Improved Thermal Properties

Polybenzoxazines (PBzs) are advanced forms of phenolic resins that possess many attractive properties, including thermally induced self-curing polymerization, which produces void-free polymer products without any by-product formation. They also possess a high Tg (glass transition temperature) and thermal stability, but the produced materials are brittle in nature, due to which the final form of their application is very difficult. Hence, in this paper, an attempt has been made to overcome the brittleness of PBz by blending it with epoxy and ε-caprolactam (CPLA) to produce free-standing PBz/Epoxy/PCLA (polycaprolactam) films. The curing process between the three components (i.e., Bzo, epoxy, and caprolactam) was monitored using differential scanning calorimetric (DSC) analysis. The results show that there is no appreciable shift in curing the exotherm observed, except a slight shift in the curing process. However, the heat liberated during the exotherm (ΔH) decreases drastically from 121 to 84 J/g, indicating that the content of benzoxazine is very important as it is involved in the polymerization process through oxazine ring-opening. The morphological studies analyzed using SEM and AFM analyses indicate that there was no observable phase separation up to 30 wt.% of CPLA loading, whereas a higher CPLA content of 50 wt.% causes agglomeration and leads to distinctive phase separation. Moreover, the thermal stability of the composite film, PBz/Epoxy/PCLA30, is also increased with a 10% degradation temperature, T10, of 438 °C, when compared with an PBz/Epoxy film. From the obtained results, it is evident that the formation of a composite film through the melt blending process could produce a tough and thermally stable film without sacrificing individual properties.

Design and fabrication of 3D-printed gastric floating tablets of captopril: effect of geometry and thermal crosslinking of polymer on floating behavior and drug release

The present study aims to investigate the potential of the 3D printing technique to design gastroretentive floating tablets (GFTs) for modifying the drug release profile of an immediate-release tablet. A 3D-printed floating shell enclosing a captopril tablet was designed having varying number of drug-release windows. The impact of geometrical changes in the design of delivery system and thermal cross-linking of polymers were evaluated to observe the influence on floating ability and drug release. Water uptake, water insolubilization, Differential Scanning Calorimetry (DSC), and Attenuated Total Reflection-Fourier Transform Infrared Spectroscopy (ATR-FTIR) were performed to assess the degree of thermal cross-linking of polyvinyl alcohol (PVA) filament. The 3D-printed GFT9 was considered the optimized gastric floating tablet that exhibited >12 h of total floating time with zero floating lag time and successfully accomplished modified-drug release by exhibiting >80% of drug release in 8 h. The zero-order release model, with an r2 value of 0.9923, best fitted the drug release kinetic data of the GFT9, which followed a super case II drug transport mechanism with an n value of 0.95. The optimized gastric floating device (GFT9) also exhibited the highest MDT values (238.55), representing slow drug release from the system due to thermal crosslinking and the presence of a single drug-releasing window in the device.