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Biodegradable polyurethanes based on poly(ethylene glycol)
Kupka, Vojtěch ; Žídek, Jan (oponent) ; Vojtová, Lucy (vedoucí práce)
Presented diploma thesis deals with synthesis of biodegradable polyurethanes (bio-PUs) based on poly(ethylene glycol) (PEG) and poly(e-caprolactone) (PCL) with potential use in medicine. The aim of the work was to develop the methodology for synthesis of elastomeric polyurethane that could be formed into scaffold applicable in tissue engineering for regenerative human medicine. The theoretical part summarizes the knowledge of various kinds of materials which are possible to use for intended application. Scaffold forming techniques, their biocompatibility and characterization of properties of resulting materials are involved. The experimental part is focused on the development of suitable methodology to prepare functional samples based on PEG, PCL, hexamethylene diisocyanate (HMDI) and stannous octoate as the catalyst. Effect of bio-PUs composition (mainly different amount and molecular weight of PEG) on the swelling and hydrolytic stability was investigated together with testing mechanical properties, monitoring the net formation and the degree of conversion. The morphology of prepared samples was analyzed by optical microscopy, chemical composition was confirmed by infrared spectroscopy and the thermal properties were measured by differential scanning calorimetry. As for methodology development, it was found that it is necessary to degas all feedstocks before synthesis, otherwise non-well polymerized samples with different pore size have been obtained. Synthesis of bio-PU was realized under the nitrogen atmosphere in two steps. First, both polyols (PEG and PCL) were homogenized on the vacuum line at 130 °C followed by the addition of HMDI in the second step at 65 °C in glove-bag to obtain bio-PU samples. Finally samples were cured at the mould for 48 hours at 65 °C in oven. Based on the physical conditions of samples preparations, flexible bio-PU from white films through cloudy (with visible phase separation) to transparent films (clear) were obtained. Phase separation was confirmed by optical microscopy showing typical spherulite structure of crystalline phase (PCL) in amorphous matrix of PEG. The monitoring of net formation confirmed maximal conversion of polymerization (96 %) already after 4 hours of curing in the oven. Mechanical properties testing showed that important influence to rupture strength has isocyanate index (NCO/OH ratio). Different molecular weight of PEG showed influence to tensile properties as the specimens were completely cross-linked. Characterization of swelling exhibited increase the water uptake of samples with growing molecular weight of PEG (from 28 up to 58 wt.%). As well as, the bio- PU samples having higher molecular weight of PEG degraded faster in water at 37 °C. In presented diploma thesis was confirmed that it is possible to control the hydrolytic stability of obtained biodegradable polyurethane elastomers by the amount and the molecular weight of PEG.
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Biodegradable polyurethanes based on poly(ethylene glycol)
Kupka, Vojtěch ; Žídek, Jan (oponent) ; Vojtová, Lucy (vedoucí práce)
Presented diploma thesis deals with synthesis of biodegradable polyurethanes (bio-PUs) based on poly(ethylene glycol) (PEG) and poly(e-caprolactone) (PCL) with potential use in medicine. The aim of the work was to develop the methodology for synthesis of elastomeric polyurethane that could be formed into scaffold applicable in tissue engineering for regenerative human medicine. The theoretical part summarizes the knowledge of various kinds of materials which are possible to use for intended application. Scaffold forming techniques, their biocompatibility and characterization of properties of resulting materials are involved. The experimental part is focused on the development of suitable methodology to prepare functional samples based on PEG, PCL, hexamethylene diisocyanate (HMDI) and stannous octoate as the catalyst. Effect of bio-PUs composition (mainly different amount and molecular weight of PEG) on the swelling and hydrolytic stability was investigated together with testing mechanical properties, monitoring the net formation and the degree of conversion. The morphology of prepared samples was analyzed by optical microscopy, chemical composition was confirmed by infrared spectroscopy and the thermal properties were measured by differential scanning calorimetry. As for methodology development, it was found that it is necessary to degas all feedstocks before synthesis, otherwise non-well polymerized samples with different pore size have been obtained. Synthesis of bio-PU was realized under the nitrogen atmosphere in two steps. First, both polyols (PEG and PCL) were homogenized on the vacuum line at 130 °C followed by the addition of HMDI in the second step at 65 °C in glove-bag to obtain bio-PU samples. Finally samples were cured at the mould for 48 hours at 65 °C in oven. Based on the physical conditions of samples preparations, flexible bio-PU from white films through cloudy (with visible phase separation) to transparent films (clear) were obtained. Phase separation was confirmed by optical microscopy showing typical spherulite structure of crystalline phase (PCL) in amorphous matrix of PEG. The monitoring of net formation confirmed maximal conversion of polymerization (96 %) already after 4 hours of curing in the oven. Mechanical properties testing showed that important influence to rupture strength has isocyanate index (NCO/OH ratio). Different molecular weight of PEG showed influence to tensile properties as the specimens were completely cross-linked. Characterization of swelling exhibited increase the water uptake of samples with growing molecular weight of PEG (from 28 up to 58 wt.%). As well as, the bio- PU samples having higher molecular weight of PEG degraded faster in water at 37 °C. In presented diploma thesis was confirmed that it is possible to control the hydrolytic stability of obtained biodegradable polyurethane elastomers by the amount and the molecular weight of PEG.
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