The free radical copolymerization of tung oil, divinylbenzene, and n-butyl methacrylate results in bio-based thermosetting polymers with tunable properties. Biocomposites have been obtained by the reinforcement of such bio-based resins with a-cellulose. Asolectin from soybeans consists of a mixture of natural, polyunsaturated phospholipids. Because of its long, unsaturated fatty acid chains, and the presence of phosphate and ammonium groups, asolectin from soybeans is a good candidate for acting as a natural compatibilizer between the hydrophobic matrix and the hydrophilic reinforcement. In the current work, we investigate the changes in properties resulting from the addition of asolectin to a tung oil-based polymer reinforced with a-cellulose. An evaluation of the curekinetics of the tung oil-based resin has been conducted by dielectric analysis (DEA), and the final biocomposites have been thoroughly characterized by differential scanning calorimetry (DSC), thermogravimetric analysis (TGA), dynamic mechanical analysis (DMA), Soxhlet extraction, and scanning electron microscopy (SEM).
Tung oil is uniquely reactive among plant-based natural oils due to the series of conjugated carbon-carbon double bonds in its fatty acid chains. These conjugated carbon-carbon double bonds impart a high reactivity towards cationic polymerization in the presence of other reactive co-monomers, such as divinylbenzene and styrene. An impressive decrease in the cure time of tung oil-based thermosets has been achieved when the resins investigated were microwaved in the presence of carbon nanotubes (CNTs). However, the fast cure compromised the overall thermo-mechanical properties of the materials investigated. Microwave power, exposure time, and CNT loading effects have been assessed by means of dielectric analysis (DEA), thermogravimetric analysis (TGA), differential scanning calorimetry (DSC), dynamic mechanical analysis (DMA), and proton nuclear magnetic resonance ( 1 H NMR) spectroscopy of extracts obtained by Soxhlet extraction. Possible reasons were proposed to explain the overall inferior properties observed whenever faster cure rates were achieved.
AbstractA model anti-cancer/tumor drug cis-diammineplatinum (II) dichloride (cisplatin) was loaded into micro- and nanofibers of cellulose, cellulose acetate (CA) and poly(ethylene oxide) (PEO), using various electrospinning techniques. Single-nozzle electrospinning was used to fabricate neat fibers of each category. Drug loading in cellulose fibers was performed using single-nozzle electrospinning. Encapsulation of cisplatin in CA and PEO-based fibers was performed using coaxial electrospinning. Morphological analysis of the fibers was performed using scanning electron microscopy (SEM) and energy dispersive X-ray spectroscopy (EDS). The various categories of fibers exhibited diverse morphological features depending on the material compositions and applied process parameters. The drug-loaded cellulose nanofibers showed attached particles on the surface. These particles were composed of both the polymer and the drug. The CA-cisplatin fibers exhibited drug encapsulation within various diverse morphological conformations: hierarchical structures such as straw-sheaf-shaped particles, dendritic branched nanofibers and swollen fibers with large beads. However, in the case of PEO fibers, drug encapsulation was observed inside repeating dumbbell-shaped structures. Morphological development of the fibers and corresponding mode of drug encapsulation were correlated with process parameters such as applied voltage, concentrations and relative feed rates of the solutions and conductivities of the solvents.
Cellulosic nanofibers have been electrospun with an antitumor agent Cisplatin. Cellulose acetate (CA) and Cisplatin were co-electrospun using a coaxial electrospinning system. For the outer sheath, a solution of 7.5wt% CA in Acetone and DMAc (2:1) was used. The inner core consisted of Cisplatin dissolved in DMF at a concentration of 5mg/ml. Drug-loaded nanofibers from Cellulose pulp (2wt%) dissolved in NMMO. H2O were also produced. The solutions were electrospun in a high voltage electric field of 25–30 kV. Characterization of neat and drug-loaded nanofibers was performed using Scanning electron microscopy (SEM) and Energy Dispersive X-Ray Spectroscopy (EDS). The characterization studies have shown the formation of nanofibers having both sporadic beads with internal agglomeration and conjugation of Cisplatin on the nanofiber surfaces.
Bio-based vesicles, with potential application in drug delivery and/or catalyst encapsulation, have been prepared by the free radical emulsion co-polymerization of tung oil, divinylbenzene (DVB), n-butyl methacrylate (BMA), and asolectin in a xylene/water mixture. The free radical polymerization was initiated by di-tert-butyl peroxide (DTBP) at 100 • C in a convection oven. Molecular weights of approximately 11,000 Da were measured by Matrix-assisted Laser Desorption/Ionization-Time of Flight (Maldi-TOF) for tung oil-asolectin copolymers, verifying that significant polymerization occurs under the cure conditions employed. The cure of the co-monomer mixture employed in this work was monitored by Dielectric Analysis (DEA), while changes in the Raman spectrum of all co-monomers before and after the cure, along with differential scanning calorimetry (DSC) analysis, have been used to verify the need of a post-cure step and completion of the polymerization reaction. Scanning Transmission Electron Microscopy (STEM) images of the emulsion after polymerization indicate that vesicles were formed, and vesicle size distribution of samples prepared with different amounts of tung oil were determined using a Zetasizer.
Crystalline particles known as Metal Organic Frameworks (MOF’s) are known for their large surface area and high adsorption and storage capacity for CO2 gas. Electrospun nanofibers are considered as ideal substrates for synthesizing the MOF particles on the fiber surface. In this project, Polyacrylonitrile (PAN) and a Cu-based MOF known as HKUST-1 were selected as substrate fibers and adsorbent particles respectively. A precursor solution of PAN polymer hybridized with HKUST-1 particles dissolved in Dimehtylformamide (DMF) is used as the primary component solution for electrospinning. SEM images of the electrospun fibers showed small MOF particles formation into the fiber structure. A secondary solvothermal process of MOF particles growing on the fibers was then executed to increase the amount of MOF particles for effectual gas adsorption. The secondary process consists of multiple growth cycles and SEM images showed uniform distribution of porous MOF particles of 2–3μm in size on the fiber surface. EDS report of the fiber confirmed the presence of MOF particles through identification of characteristic Copper elemental peaks of HKUST-1. Thermogravitmetric analysis (TGA) of HKUST-1 doped PAN fiber displayed 32% of total weight loss between 180°C and 350°C thus proving the as-synthesized MOF particles are thermally stable within the mentioned temperature range. A comparative IR spectroscopic result between the gas-treated and gas-untreated fiber samples showed the presence of characteristic peak in the vicinity of 2300 and 2400cm−1 which corroborates the assertion of adsorption of CO2 on the system. Further step involved is to investigate the gas adsorption capacity of the filter system in an experimental test bench. Non-dispersive Infrared (NDIR) CO2 sensors will be used at the gas inlet and outlet parts to measure the concentration of CO2 and determine the amount of gas uptake by the filter system.
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