Recyclability of elastomer toughened recycled poly(ethylene terephthalate): The effect of grinding-extrusion-injection moulding on the mechanical and morphological properties of the blend.

Reprocessing potential of recycled poly(ethylene-terephthalate) (RPET)/ethylene-butyl-acrylate-glycidyl methacrylate (EBA-GMA) blends was investigated. PET flakes from food packaging were compounded with 0, 5, 10, 15 and 20 % EBA-GMA. Injection moulded specimens were produced, and some of the specimens were grinded, and reproduced to simulate real reprocessing. It was revealed by scanning electron microscopy that the distribution and particle size of the elastomer did not change notably after recycling. Noticeable degradation of the polymer matrix was observable after every processing step. Such deterioration of PET resulted in higher crystallinity and rigid amorphous fraction, as found by differential scanning calorimetry, which ultimately led to higher storage modulus, while the notched impact strength and elongation at break decreased. Nevertheless, the mechanical performance of the reprocessed RPET/EBA-GMA blends still significantly outperforms that of the neat PET recyclate. The degree of chain breakage was found to be the primary factor determining the recyclability of RPET/EBA-GMA blends.

Development of Bioepoxy Resin Microencapsulated Ammonium-Polyphosphate for Flame Retardancy of Polylactic Acid.

Ammonium-polyphosphate (APP) was modified by microencapsulation with a bio-based sorbitol polyglycidyl ether (SPE)-type epoxy resin and used as a flame retardant additive in polylactic acid (PLA) matrix. The bioresin-encapsulated APP (MCAPP) particles were characterized using Fourier transform infrared (FTIR) spectroscopy and Raman mapping, particle size distribution was determined by processing of scanning electron microscopic (SEM) images. Interaction between the APP core and the bioresin shell was revealed by combined thermogravimetric analysis (TGA)­FTIR spectroscopy. The APP to SPE mass ratio of 10 to 2 was found to be optimal in terms of thermal, flammability, and mechanical properties of 15 wt% additive containing biocomposites. The bioresin shell effectively promotes the charring of the APP-loaded PLA composites, as found using TGA and cone calorimetry, and eliminates the flammable dripping of the specimens during the UL-94 vertical burning tests. Thus, the V-0 rating, the increased limiting oxygen index, and the 20% reduced peak of the heat release rate was reached compared to the effects of neat APP. Furthermore, better interfacial interaction of the MCAPP with PLA was indicated by differential scanning calorimetry and SEM observation. The stiff interphase resulted in increased modulus of these composites. Besides, microencapsulation provided improved water resistance to the flame retardant biopolymer system.

Development of Flame-Retarded Nanocomposites from Recycled PET Bottles for the Electronics Industry.

Recycled polyethylene-terephthalate (rPET) nanocomposites of reduced flammability were prepared by combining aluminum-alkylphosphinate (AlPi) flame retardant (FR) and natural montmorillonite (MMT), in order to demonstrate that durable, technical products can be produced from recycled materials. During the development of the material, by varying the FR content, the ratio and the type of MMTs, rheological, morphological, mechanical and flammability properties of the nanocomposites were comprehensively investigated. Related to the differences between the dispersion and nucleation effect of MMT and organo-modified MMT (oMMT) in rPET matrix, analyzed by Scanning Electron Microscopy (SEM), Energy Dispersive X-Ray Spectroscopy (EDS) and Differential Scanning Calorimetry (DSC), mechanical properties of the nanocomposites changed differently. The flexural strength and modulus were increased more significantly by adding untreated MMT than by the oMMT, however the impact strength was decreased by both types of nanofillers. The use of different type of MMTs resulted in contradictory flammability test result; time-to-ignition (TTI) during cone calorimeter tests decreased when oMMT was added to the rPET, however MMT addition resulted in an increase of the TTI also when combined with 4% FR. The limiting oxygen index (LOI) of the oMMT containing composites decreased independently from the FR content, however, the MMT increased it noticeably. V0 classification according to the UL-94 standard was achieved with as low as 4% FR and 1% MMT content. The applicability of the upgraded recycled material was proved by a pilot experiment, where large-scale electronic parts were produced by injection molding and characterized with respect to the commercially available counterparts.

Application of Melt-Blown Poly(lactic acid) Fibres in Self-Reinforced Composites.

The aim of our research was to produce poly(lactic acid) (PLA) fibres with diameters in the micrometer size range, serving as the reinforcing phase in self-reinforced (SR) PLA composites. Nonwoven PLA mats were manufactured by solvent-free melt-blowing technology. Three types of PLA differing in d-lactide content were processed with a productivity as high as 36 g/h. The crystallinity of the PLA microfibres was enhanced by thermal annealing. A 2⁻3-fold increase in the degree of crystallinity was obtained, as measured by differential scanning calorimetry (DSC). Fibre diameters between 2⁻14 µm were revealed by scanning electron microscopy (SEM). Static tensile tests were performed on the nonwoven mats, showing the reduced moduli of the annealed fibres due the amorphous relaxation. The PLA mats were processed via the hot compaction technique and formed into SR⁻PLA composites. The morphological and mechanical properties of the obtained microstructural composites were comprehensively studied. Composites prepared from annealed, thermally more stable PLA nonwoven mats showed superior mechanical properties; the tensile strength improved by 47% due to the higher residual fibre content.

Key Role of Reinforcing Structures in the Flame Retardant Performance of Self-Reinforced Polypropylene Composites.

The flame retardant synergism between highly stretched polymer fibres and intumescent flame retardant systems was investigated in self-reinforced polypropylene composites. It was found that the structure of reinforcement, such as degree of molecular orientation, fibre alignment and weave type, has a particular effect on the fire performance of the intumescent system. As little as 7.2 wt % additive content, one third of the amount needed in non-reinforced polypropylene matrix, was sufficient to reach a UL-94 V-0 rating. The best result was found in self-reinforced polypropylene composites reinforced with unidirectional fibres. In addition to the fire retardant performance, the mechanical properties were also evaluated. The maximum was found at optimal consolidation temperature, while the flame retardant additive in the matrix did not influence the mechanical performance up to the investigated 13 wt % concentration.

Flame Retardancy of Sorbitol Based Bioepoxy via Combined Solid and Gas Phase Action.

Flame-retarded bioepoxy resins were prepared with the application of commercially available sorbitol polyglycidyl ether (SPE). The additive-type flame retardancy of the cycloaliphatic amine-cured SPE was investigated. Three-percent phosphorus (P)-containing samples were prepared with the application of the liquid resorcinol bis(diphenyl phosphate) (RDP), the solid ammonium polyphosphate (APP), and by combining them. Synergistic effect was found between the inorganic APP and the organophosphorus RDP, when applied in combination: formulations applying RDP or APP alone showed increased limiting oxygen index (LOI) values, however, their UL-94 standard ratings remained HB. When the same amount of P originated from the two additives, V-0, self-extinguishing rating and LOI value of 34% (v/v) was reached. By the combined approach the heat release rate of SPE could be lowered by approximately 60%. The assumed balanced solid and gas phase mechanism was confirmed by thermogravimetric analysis, Fourier transform infrared spectrometry (FTIR) analysis (of the gases formed during laser pyrolysis), attenuated total reflection-infrared spectrometry (ATR-IR) analysis (of the charred residues), as well as by mechanical testing (of the char obtained after combustion).

Comparison of spray drying, electroblowing and electrospinning for preparation of Eudragit E and itraconazole solid dispersions.

Three solvent based methods: spray drying (SD), electrospinning (ES) and air-assisted electrospinning (electroblowing; EB) were used to prepare solid dispersions of itraconazole and Eudragit E. Samples with the same API/polymer ratios were prepared in order to make the three technologies comparable. The structure and morphology of solid dispersions were identified by scanning electron microscopy and solid phase analytical methods such as, X-ray powder diffraction (XRPD), differential scanning calorimetry (DSC) and Raman chemical mapping. Moreover, the residual organic solvents of the solid products were determined by static headspace-gas chromatography/mass spectroscopy measurements and the wettability of samples was characterized by contact angle measurement. The pharmaceutical performance of the three dispersion type, evaluated by dissolution tests, proved to be very similar. According to XRPD and DSC analyses, made after the production, all the solid dispersions were free of any API crystal clusters but about 10 wt% drug crystallinity was observed after three months of storage in the case of the SD samples in contrast to the samples produced by ES and EB in which the polymer matrix preserved the API in amorphous state.

In vitro dissolution-permeation evaluation of an electrospun cyclodextrin-based formulation of aripiprazole using µFlux™.

Since it is a well-known fact that among the newly discovered active pharmaceutical ingredients the number of poorly water soluble candidates is continually increasing, dissolution enhancement of poorly water soluble drugs has become one of the central challenges of pharmaceutical studies. So far the preclinical studies have been mainly focused on formulation methods to enhance the dissolution of active compounds, in many cases disregarding the fact that the formulation matrix not only affects dissolution but also has an effect on the transport through biological membranes, changing permeation of the drug molecules. The aim of this study was to test an electrospun cyclodextrin-based formulation of aripiprazole with the novel µFlux apparatus, which monitors permeation together with dissolution, and by this means better in vitro-in vivo correlation is achieved. It was evinced that a cyclodextrin-based electrospun formulation of aripiprazole has the potential to ensure fast drug delivery through the oral mucosa owing to the ultrafast dissolution of the drug from the formulation and the enhanced flux across membranes as shown by the result of the novel in vitro dissolution and permeation test.