The Effect of Polymerization Temperature on the Properties of Polyvinyl Fluoride Polymerization in Supercritical Carbon Dioxide

The ongoing search for environmentally friendlier alternative to the organic solvents used in chemical processes has led to the development of technologies based on supercritical carbon dioxide (scCO2), which is non-flammable, non-toxic and relatively inert fluid. Polymer chemistry does not escape this trend. Fluoropolymers prepared in scCO2 have many special properties, which are different from fluoropolymers that use water as the reaction medium, this paper studies the effect of polymerization temperature on polyvinyl fluoride polymerization in supercritical carbon dioxide. The results show that as the polymerization temperature increases, the intrinsic viscosity and shear viscosity of the polymer gradually decreases; at the same time, the increasing of polymerization temperature leads to higher proportion of irregular structure of the polymer, which causes lower melting point and lower crystallinity, and the film prepared by the resin also exhibits a higher visible light transmittance. The above results show that the resin polymerized in supercritical carbon dioxide can impart better performance to conventional polymerization, which expands the potential application fields of the resin.

Enhancement of the solubility of asenapine maleate through the preparation of co-crystals

Background: Asenapine maleate, an anti-schizophrenic drug, is a class II drug with low solubility and high permeability. This exerts rate-limiting effect on drug bioavailability. Objective: Improve the solubility/dissolution rate of asenapine maleate and hence the bioavailability using cocrystal approach. Method: Co-crystals were prepared using the solvent evaporation technique. Since the drug has H-bond acceptor count of 6, and H-bond donor count of 2, several co-formers were investigated. The co-crystals were evaluated using PXRD, FTIR spectroscopy, and DSC. Additionally, in-vitro dissolution studies were conducted. Results: The preparation of the co-crystals was successful. The PXRD patterns showed that the resultant mixture was crystalline, the FTIR confirmed the formation of H-bond between the drug and the co-formers and the DSC showed that the mixture exhibited a lower melting point as compared to the components and it was followed immediately by an exothermic peak, which confirmed the formation of co-crystals. The dissolution of all the prepared co-crystals using different co-formers in different ratios was much enhanced as compared to the unprocessed drug. The dissolution of the drug in the drug-nicotinamide co-crystals was much faster than that from the other co-crystals during the first 15-20 minutes. The dissolution of the drug from the physical mixture was slower than from the co-crystals during the first 15-20 minutes but the cumulative amount released after 120 minutes was almost the same. Conclusion: Co-crystals were prepared successfully by improving the solubility/dissolution rate of asenapine maleate, and were expected to enhance the bioavailability of the drug.

Effect of Graphene Oxide on the Properties of Poly(3-Hydroxybutyrate-co-3-Hydroxyhexanoate)

The main shortcomings of polyhydroxybutyrate (PHB), which is a biodegradable and biocompatible polymer used for biomedical and food packaging applications, are its low thermal stability, poor impact resistance and lack of antibacterial activity. This issue can be improved by blending with other biodegradable polymers such as polyhydroxyhexanoate to form poly(3-hydroxybutyrate-co-3-hydroxyhexanoate) (PHBHHx), which is a copolymer with better impact strength and lower melting point. However, PHBHHx shows reduced stiffness than PHB and poorer barrier properties against moisture and gases, which is a drawback for use in the food industry. In this regard, novel biodegradable PHBHHx/graphene oxide (GO) nanocomposites have been prepared via a simple, cheap and environmentally friendly solvent casting method to enhance the mechanical properties and antimicrobial activity. The morphology, mechanical, thermal, barrier and antibacterial properties of the nanocomposites were assessed via several characterization methods to show the enhancement in the biopolymer properties. The stiffness and strength of the biopolymer were enhanced up to 40% and 28%, respectively, related to the strong matrix-nanofiller interfacial adhesion attained via hydrogen bonding interactions. Moreover, the nanocomposites showed superior thermal stability (as far as 40 °C), lower water uptake (up to 70%) and better gas and vapour barrier properties (about 45 and 35% reduction) than neat PHBHHx. They also displayed strong biocide action against Gram positive and Gram negative bacteria. These bio-based nanocomposites with antimicrobial activity offer new perspectives for the replacement of traditional petroleum-based synthetic polymers currently used for food packaging.

Cocrystal formation of loratadine-succinic acid and its improved solubility

Objectives Loratadine belongs to Class II compound of biopharmaceutics classification system (BCS) due its low solubility and high membrane permeability. Cocrystal is a system of multicomponent crystalline that mostly employed to improve solubility. Succinic acid is one of common coformer in cocrystal modification. This research aims to investigate cocrystal formation between loratadine and succinic acid and its effect on solubility property of loratadine. Methods Cocrystal of loratadine-succinic acid was prepared by solution method using methanol as the solvent. Cocrystal formation was identified under observation of polarization microscope and analysis of the binary phase diagram. The cocrystal phase was characterized by differential thermal analysis (DTA), powder X-ray diffraction (PXRD), Fourier transform infrared (FTIR), and scanning electron microscopy (SEM). Solubility study was conducted in phosphate-citrate buffer pH 7.0 ± 0.5 at 30 ± 0.5 °C. Results Loratadine is known to form cocrystal with succinic acid in 1:1 M ratio. Cocrystal phase has lower melting point at 110.9 °C. Powder diffractograms exhibited new diffraction peaks at 2θ of 5.28, 10.09, 12.06, 15.74, 21.89, and 28.59° for cocrystal phase. IR spectra showed that there was a shift in C=O and O–H vibration, indicating intermolecular hydrogen bond between loratadine and succinic acid. SEM microphotographs showed different morphology for cocrystal phase. Loratadine solubility in cocrystal phase was increased up to 2-fold compared to loratadine alone. Conclusions Cocrystal of loratadine and succinic acid is formed by stoichiometry of 1:1 via C=O and H–O interaction. Cocrystal phase shows different physicochemical properties and responding to those properties, it shows improved loratadine solubility as well.

Comparative Studies on Flotation Performance of Saturated Fatty Acids and Unsaturated Fatty Acids Separated from Hogwash Oil

Low flotation recovery, high pulp temperature, and large dosage of reagents are the typical disadvantages when using mixed fatty acids (MFA) prepared from hogwash oil for flotation directly. To determine the type of fatty acid that yields poor flotation performance, flotation performance and adsorption characteristics of saturated fatty acids (SFA) and unsaturated fatty acids (UFA) separated from the MFA were studied in our work. GC-MS, FT-IR, iodine value detection and melting point measurement showed that UFA contained –(CH=CH–CH2)n- groups and had much lower melting point. Quartz flotation tests were used to compare the flotation performance of UFA and SFA, which showed that UFA had excellent low-temperature floatability, and the flotation recovery of UFA was 35 percentage points higher than that of SFA at 20 °C and pH = 11.5. Zeta potential, FT-IR and XPS analysis indicated that UFA and SFA could adsorb onto the surface of activated quartz through chemisorption and hydrogen bonding. However, the adsorption of UFA was much stronger and more favorable; thus, the reason MFA have poor flotation performance was the presence of SFA.

Effect of Lead and Antimony on Sulfuric Acid Leaching of Copper in Speiss from Top Submerged Lance Furnaces

Cu-Pb and Cu-Sb alloys were prepared at various ratios, from 10:90 to 90:10, and leaching tests with sulfuric acid were conducted to investigate the effect of Pb and Sb on the leaching of Cu from speiss, which is obtained from the top submerged lance furnace process. The Cu leaching efficiency increased as the amount of Cu increased in both alloys, but the leaching efficiencies were lower in the Cu-Sb alloy than in the Cu-Pb alloy. For example, in alloys with 70% Pb and Sb ratio, the leaching efficiency of Cu from the Cu-Pb alloy increased to 95%. The leaching efficiency of the Cu-Sb alloy was 67% in 2 mol/L sulfuric acid solution with 1% pulp density and 1000 cc/min O2 at 90 °C, 400 rpm, and 6 hours. When the leaching residues were examined with SEM (scanning electron microscopy)-EDS (Energy-dispersive X-ray spectroscopy), it was found that in all Cu-Pb alloys, Cu and Pb exist as independent metal phases, while, in Cu-Sb alloys, Cu formed intermetallic compounds with Sb such as Cu2Sb, because the Cu-Sb alloy has a lower melting point than the Cu-Pb alloy. These results suggest that Sb may retard the leaching rate of Cu from the alloy. When the leaching residue of speiss obtained from a top submerged lance furnace, intermetallic alloys of Cu-Sb were also observed, having a net structure. The net structure contains Cu metal in the center of the speiss particle, while the intermetallic alloys of Cu-Sb were present in the outer layer of the particle, in good agreement with the results using the alloys in this study. This suggests the intermetallic alloys of Cu-Sb can prevent copper from leaching.

Polymorphs of 2,4,6-tris(4-pyridyl)-1,3,5-triazine and their mechanical properties

The second polymorph of the compound 2,4,6-tris(4-pyridyl)-1,3,5-triazine (TPT) is reported, TPT-II, which crystallizes in space group I2/a. Its higher density and more efficient space filling indicate the lower entropy of TPT-II, while its slightly lower melting point indicates its weaker intermolecular interactions. The conditions of the crystallization experiments for TPT-I and TPT-II are the dominant factors that determine the final crystalline products. The crystals of TPT-II are long needles. They exhibit bending behaviour along the crystallographic b direction when a mechanical force is imposed perpendicular to it, and regain their original shape after the external stress is removed. The elasticity of the single crystals is interpreted in terms of intermolecular interactions and an energy framework analysis.

Characterization of Lauric Acid Precipitated from Biocompatible Solvents

Water resistance of lauric acid (L) dissolved in biocompatible solvents mainly depended on the water affinity of solvent. L in DMSO (DL) was most sensitive to water and higher than L in N-methyl pyrrolidone (NL) and L in 2-pyrolidone (PL), respectively. From scanning electron microscope, differential scanning calorimetry, thermogravimetric analysis, powder x-ray diffractometry and hot stage microscope tests revealed the alteration of L crystal owing to the interference by solvent during precipitation. All L precipitates had lower melting point and degradation temperature than intact L in which L precipitated from 2-pyrrolidone exhibited the lowest melting temperature. These characteristics will be useful for modifying L in phase inversion in situ forming gel.

Mechanical Properties and Applications of Recycled Polycarbonate Particle Material Extrusion-Based Additive Manufacturing

Past work has shown that particle material extrusion (fused particle fabrication (FPF)/fused granular fabrication (FGF)) has the potential for increasing the use of recycled polymers in 3D printing. This study extends this potential to high-performance (high-mechanical-strength and heat-resistant) polymers using polycarbonate (PC). Recycled PC regrind of approximately 25 mm2 was 3D printed with an open-source Gigabot X and analyzed. A temperature and nozzle velocity matrix was used to find useful printing parameters, and a print test was used to maximize the output for a two-temperature stage extruder for PC. ASTM type 4 tensile test geometries as well as ASTM-approved compression tests were used to determine the mechanical properties of PC and were compared with filament printing and the bulk virgin material. The results showed the tensile strength of parts manufactured from the recycled PC particles (64.9 MPa) were comparable to that of the commercial filament printed on desktop (62.2 MPa) and large-format (66.3 MPa) 3D printers. Three case study applications were investigated: (i) using PC as a rapid molding technology for lower melting point thermoplastics, (ii) printed parts for high temperature applications, and (iii) printed parts for high-strength applications. The results show that recycled PC particle-based 3D printing can produce high-strength and heat-resistant products at low costs.

Eutectic Phenomenon of LiNH2-KH Composite in MH-NH3 Hydrogen Storage System

Hydrogenation of a lithium-potassium (double-cation) amide (LiK(NH2)2), which is generated as a product by ammonolysis of litium hydride and potassium hydride (LiH-KH) composite, is investigated in details. As a result, lithium amide (LiNH2) and KH are generated after hydrogenation at 160 °C as an intermediate. It is noteworthy that the mixture of LiH and KNH2 has a much lower melting point than that of the individual melting points of LiNH2 and KH, which is recognized as a eutectic phenomenon. The hydrogenation temperature of LiNH2 in the mixture is found to be significantly lower than that of LiNH2 itself. This improvement of reactivity must be due to kinetic modification, induced by the enhanced atomic mobility due to the eutectic interaction.