Polylaktidin sulakehruun optimointi reaaliaikaisen monitoroinnin avulla

Polylactide (PLA) is a synthetic biodegradable polyester and it is usually processed into fibres by two-step melt spinning, which comprises of (i) melting the raw material and pushing the melt through small orifices and (ii) stretching and heat treating the fibre to increase its mechanical properties. However, processing biodegradable polymers is challenging because the polymer degrades thermally which narrows the choice of the processing parameters. Real-time monitoring allows monitoring of the key properties of the material during the production of the fibre. There were two objectives for this work: (i) upscaling the production of 4-filament PLA fibre with an updated set-up with real-time monitoring and (ii) studying the hydrolytic degradation of PLA fibres manufactured with the conventional set-up. The updated set-up comprised of high-speed spinning plants and a twin-screw extruder equipped with a slit die for later real-time monitoring of parameters related to thermal degradation of the polymer. The processing conditions of polylactide melt spinning were optimised by two sets of trials; initial trials with a packaging grade PLA and a second set of trials with GMP grade poly(L/D)lactide with an L/D ratio of 96/4. The obtained fibres were characterised by tensile testing and the temperature-induced chain scission was evaluated by inherent viscosity (i.v.) measurements. Goal values were established to enable the post-processing of the fibres. Mechanically adequate fibre was produced in the initial trials regarding the material used and the filament diameters fulfilled the requirements. The packaging grade PLA did not degrade during extrusion but the i.v. of the GMP grade PLA was decreased by one third. The filament diameter and the strain values were at an acceptable level in half of the spools produced in the GMP grade trials. In the initial trials there was a problem with the fluctuation of the filament diameters but it was largely solved by a change of the feeding equipment in the GMP grade trials. There is a need for further optimisation of the mechanical properties. This should be done by increasing the draw ratio. However, the ultimate tensile strength of the fibre was close to the required value. In addition a 48-week hydrolysis study was conducted on the fibre produced with the conventional set-up. The molecular, rheological, thermal and mechanical properties of gamma irradiated and non-irradiated fibres were measured. The molecular weights and inherent viscosities of both fibres decreased steadily, but the irradiated fibre degraded more prominently. The mechanical performance of the non-irradiated fibre showed no changes but the irradiated fibre could no longer be tested after 28 weeks. In conclusion, the results of the hydrolytic degradation studies were mainly in line with earlier studies. These results can be used as a reference for the future hydrolytic degradation studies for the fibre manufactured with the upgraded set-up