|
|
Solubility of polypropylene in hydrocarbon solvents
Urbánková, Radka ; Kučera, Jaroslav (referee) ; Kratochvíla, Jan (advisor)
Polypropylene, on a mass-scale produced polyolefin, shows an excellent combination of end-use properties, eco-friendliness, easy recyclability, and a good processability by different technologies. Key structural parameters of polypropylene are its stereoregularity, molecular weight, and its distribution. A theoretical part of this work compiles a bibliographic search and an experimental part deals with extraction and solubility of polypropylene powder prepared on a highly active Ziegler-Natta polymerization catalyst. Extractions at a boiling point temperature of solvents (pentane - hexane - cyclohexane - hex-1-ene - benzene - heptane - octane - ethylbenzene) resulted in a progressive increase of extracted portions with temperature of extraction. Solvents used within this work were characterised by their physical properties, and steric and electronic parameters such as molecular weight, density, boiling point temperature, dipole moment, refractive index, and Hildebrand´s solubility parameter. Extraction PP at a constant temperature 36°C (boiling point of pentane) at a saturated vapour pressure in a series of hydrocarbon solvents (pentane – hexane – heptane – octane) resulted in practically the same results. Boiling octane extractable fraction at a temperature 36°C was nearly 100 % higher than fractions extracted by the other solvents. The origin of this phenomenon has not been revealed. Polypropylene solubility was determined by a complete dissolving the sample at 140°C in a series of aliphatic and aromatic solvents (pentane - hexane - cyclohexane - hex-1-ene - benzene - heptane - octane - toluene - ethylbenzene - o-xylene - m-xylene - p-xylene - decalin - chlorbenzene - 1,2-dichlorbenzene), followed by cooling the solution down to a laboratory temperature, and separating a soluble fraction, and an insoluble one. The stereoregularity of soluble fractions was characterised by a 13C NMR method, the crystallinity by a DSC method, and a molecular weight distribution by a GPC method. As a result, polypropylene solubility decreases with increasing the Hildebrand solubility parameter of the solvent that corresponds with theoretical expectations. Moreover, PP solubility correlates strongly with a refractive index, and a density of solvent.
|
|
|
Development of method thermoporosimetry polymer powders
Urbánková, Radka ; Salajka,, Zdeněk (referee) ; Kratochvíla, Jan (advisor)
Thermoporosimetry is a technique to determine small pore sizes based on melting and crystallization point depression. The temperature shift was measured by Differential Scanning Calorimetry (DSC). Development of thermoporosimetry was carried out on silica with a well-characterized narrow pore size distribution. Several parameters were studied, which a have a direct influence on melting and crystallization point depression (for example: a quality of the solvent, filling the pores with the solvent, time and frequency of centrifuging, superfluous solvent removal conditions, etc.). The optimum conditions for the thermoporosimetry method were developed using high porosity silica. The optimized experimental conditions found for silica were applied to polypropylene powder with much lower porosity. Several polypropylene powders were synthesized using different polymerization catalysts and their porosity determined. Polymer powder morphology and structure was characterized by standard methods. Powder porosity obtained by thermoporometry, gas sorption, and BET methods was compared.
|
|
|
Development of method thermoporosimetry polymer powders
Urbánková, Radka ; Salajka,, Zdeněk (referee) ; Kratochvíla, Jan (advisor)
Thermoporosimetry is a technique to determine small pore sizes based on melting and crystallization point depression. The temperature shift was measured by Differential Scanning Calorimetry (DSC). Development of thermoporosimetry was carried out on silica with a well-characterized narrow pore size distribution. Several parameters were studied, which a have a direct influence on melting and crystallization point depression (for example: a quality of the solvent, filling the pores with the solvent, time and frequency of centrifuging, superfluous solvent removal conditions, etc.). The optimum conditions for the thermoporosimetry method were developed using high porosity silica. The optimized experimental conditions found for silica were applied to polypropylene powder with much lower porosity. Several polypropylene powders were synthesized using different polymerization catalysts and their porosity determined. Polymer powder morphology and structure was characterized by standard methods. Powder porosity obtained by thermoporometry, gas sorption, and BET methods was compared.
|
|
|
Solubility of polypropylene in hydrocarbon solvents
Urbánková, Radka ; Kučera, Jaroslav (referee) ; Kratochvíla, Jan (advisor)
Polypropylene, on a mass-scale produced polyolefin, shows an excellent combination of end-use properties, eco-friendliness, easy recyclability, and a good processability by different technologies. Key structural parameters of polypropylene are its stereoregularity, molecular weight, and its distribution. A theoretical part of this work compiles a bibliographic search and an experimental part deals with extraction and solubility of polypropylene powder prepared on a highly active Ziegler-Natta polymerization catalyst. Extractions at a boiling point temperature of solvents (pentane - hexane - cyclohexane - hex-1-ene - benzene - heptane - octane - ethylbenzene) resulted in a progressive increase of extracted portions with temperature of extraction. Solvents used within this work were characterised by their physical properties, and steric and electronic parameters such as molecular weight, density, boiling point temperature, dipole moment, refractive index, and Hildebrand´s solubility parameter. Extraction PP at a constant temperature 36°C (boiling point of pentane) at a saturated vapour pressure in a series of hydrocarbon solvents (pentane – hexane – heptane – octane) resulted in practically the same results. Boiling octane extractable fraction at a temperature 36°C was nearly 100 % higher than fractions extracted by the other solvents. The origin of this phenomenon has not been revealed. Polypropylene solubility was determined by a complete dissolving the sample at 140°C in a series of aliphatic and aromatic solvents (pentane - hexane - cyclohexane - hex-1-ene - benzene - heptane - octane - toluene - ethylbenzene - o-xylene - m-xylene - p-xylene - decalin - chlorbenzene - 1,2-dichlorbenzene), followed by cooling the solution down to a laboratory temperature, and separating a soluble fraction, and an insoluble one. The stereoregularity of soluble fractions was characterised by a 13C NMR method, the crystallinity by a DSC method, and a molecular weight distribution by a GPC method. As a result, polypropylene solubility decreases with increasing the Hildebrand solubility parameter of the solvent that corresponds with theoretical expectations. Moreover, PP solubility correlates strongly with a refractive index, and a density of solvent.
|
guest ::
RSS feed.