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The influence of nanoparticles on isothermal crystallization rate of isotactic polypropylene
Miškolci, Michal ; Jančář, Josef (referee) ; Bálková, Radka (advisor)
This diploma thesis deals with the study of isothermal crystallization of nanocomposite materials based on isotactic polypropylene (iPP) and nanosilica, depending on the volume fraction (0, 2, 4 and 6 %) and type of silica and the crystallization temperature. Fumed silica and four types of silica with different surface treatment were used as filler. The crystallization performed at temperatures 136, 138, 140 and 142 °C has been studied in-situ using polarized optical microscope and the crystallization rate was evaluated from the growing radius of spherulites. It can be stated that particles of silica have been inbuilt into the spherulites due to the linear growth of spherulites of all composite materials. The most significant increase of the crystallization rate of iPP was caused by fumed silica, the most significant decrease was caused by silica TS-720 at volume fraction 4 %. The crystallization rate (G) has been slightly increased with the increasing volume fraction of filler at 136 °C, the G slightly decreased at 138 °C and there was no trend of G for two higher temperatures. Also, it was not possible to exactly evaluate the influence of the surface treatments. The reason is the most probably uneven (non-homogenous) distribution of nanosilica as revealed thermogravimetric analysis. The crystallization kinetics was evaluated according to the Lauritzen-Hoffmann theory. The morphological part of the study showed that iPP was in ? and ß-structure and spherulites of ? phase were of the type I, II and mixed.
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Grafting of PP using itaconic anhydride and drying agent
Petruš, Josef ; Hermanová, Soňa (referee) ; Kučera, František (advisor)
The bachelor´s thesis deal with a preparation of polypropylene (PP) grafted with itaconic acid (IA) and itaconic anhydride (IAH) arising by thermic dehydration in situ from IA in presence of drying agents. Theoretical part contains actual knowledges especially about radical grafting of polypropylene with different monomers. In experimental part samples of polypropylene grafted with 0.5 wt % IA were prepared with free different drying agents: calcium oxide, aluminium oxide and calcium sulfate hemihydrate. To comparison PP grafted with 0.5 wt % IAH was prepared. Thermic behaviour of IA with drying agent and IAH samples was determined by thermogravimetric analysis (TGA) and differential scanning calorimetry (DSC) measurement. Process of grafting was realized with mixer Brabender at temperature 230 °C, speed was 30 RPM and reaction time 6 minutes. 2,5-dimethyl-2,5bis(tert-buthylperoxy)hexane (Luperox 101) was used as iniciator. Percentage of grafted carboxylic groups was provided by acid-base titration. FTIR spectroscopy was used for quantitative and qualitative analysis of characteristic groups.
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Blends of PLA with thermoplastics
Petruš, Josef ; Petrůj, Jaroslav (referee) ; Kučera, František (advisor)
Diploma thesis deals with preparation of polymer blend of polymer A and polymer B. Knowledge of polymer blends forming, thermodynamics and function of compatibilizer is contained in the theoretical part. Polymer blend A/B of weight ratios 75/25, 50/50 and 25/75 wt% were prepared by physical compatibilization. Concentration of compatibilizer was 5 wt%, in the case of A/B 50/50 wt% concentration of compatibilizer was 10 and 30 wt%, respectively. Blending was achieved with twin-screw extruder at 230 °C and 100 rpm. Second method used for A/B blending was based on reactive compatibilization which was achieved with Brabender kneader at 230 °C, 50 rpm and reaction time 10 minutes. Concentration ratios of A/B were 75/25, 50/50 and 25/75 wt%. Itaconic acid anhydride and maleic anhydride 0.5 and 5 wt% were used as monomer. 2,5-dimethyl-2,5-bis(tert-buthylperoxy)hexan was (Luperox 101) used as an initiator. Difference between compatibilized and noncompatibilized blends was characterized by scanning electron microscopy, tensile test, differential scanning calorimetry, melt flow index measuring, acid-base titration and FT-IR spectroscopy.
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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.
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Polypropylene membranes and their use
Strunga, Alan ; Bartuli, Erik (referee) ; Kůdelová, Tereza (advisor)
This Bachelor’s thesis is focused on polymeric membranes with additional focus on membranes produced from polypropylene. The main physicochemical properties of the membranes are discussed together with procedures and measuring devices suitable for their determination. Also discussed here are the most common production and modification methods, potential applications in the industry and the drawbacks that still limit widespread use. This works should provide basic information about the applications of hydrophobic membranes within the membrane technology.
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Analytical Methods of Radical Grafted Polypropylene
Zahálka, Martin ; Petruš, Josef (referee) ; Kučera, František (advisor)
The bachelor thesis deals with characterization and analyzes of radical grafted polypropylene. Analytical methods and processes used for determination of concentration of MA in grafted PP and characterization of prepared material were summarized in theoretical part. PP-g-MA samples were prepared by the homogeneous and heterogeneous technique. All the samples with unknown content of MA were analyzed by two volumetric methods. Quantitative analysis by attenuated total reflectance infrared spectroscopy (ATR–FTIR) was used. Carbonyl index was determined based on peaks of methylene (1167 cm-1) and carbonyl (1785 cm-1) groups. X-ray photoelectron spectroscopy was one of the methods used to determine concentration of MA in modified PP. Melt flow index was determined and range of -scission was discussed.
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CHARACTERIZATION OF WRAPPAGING FILMS BASED ON POLYETHYLENE AND POLYPROPYLENE
Bělašková, Marie ; Poláček, Petr (referee) ; Bálková, Radka (advisor)
By seven kinds of coextruded and blown packing polyethylene and polypropylene based films, which are supplied by Granitol were characterized in this bachelor thesis. The following methods were used for characterization: thermogravimetric analysis, differential scanning calorimetry, Fourier transform infrared spectroscopy, confocal laser scanning microscopy , and scanning electron microscopy. The methods made possible to determine the composition of the films and to evaluate the degree of crystallinity.
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Preparation of grafted PP with diferent concentration of MA and IA
Běťák, Lukáš ; Žídek, Jan (referee) ; Kučera, František (advisor)
The bachelor thesis deal with a preparation and a characterization of polypropylene grafted with anhydrides carboxylic acids in a melt. A present knowledge about radical grafting was summarized in a theoretical part. Samples of polypropylene grafted with itaconic anhydride (IA) and maleic anhydride (MA) were prepared in the experimental part. 2,5 dimethyl 2,5bis(tert-buthylperoxy)hexane (Luperox 101) was used as a radical initiator. A Brabender mixer was used for experiment, conditions for grafting were 210 °C, 30 RPM and 6 min. Weight concentration of grafted monomer was in range 0,25 wt % 1 wt %. It was found that a degree of conversion depended on concentration ratio of initiator to monomer. Attached carboxylic groups to polypropylene backbone were confirmed by FTIR spectroscopy. The percentage of grafting was determined by acid-base titration.
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Post-polymerization modification of polyolefins for the preparation of hydroxylated macroinitiators
Boldovjaková, Tatiana ; Kučera, František (referee) ; Petruš, Josef (advisor)
The diploma thesis deals with post-polymerization hydroxylation of polypropylene in solid state. Regarding the literature review, polypropylene was hydroxylated by radical grafting in aqueous solution of potassium persulfate at 100 °C, under nitrogen atmosphere for 60 minutes. Hydroxylation of polypropylene was performed at different concentrations of potassium persulfate (1; 5; 10 mol. %) and two different water/potassium persulfate molar ratios. The effects of reaction system composition and reaction conditions on reaction efficiency, extent of side reactions, thermal and rheological properties of hydroxylated polypropylene were evaluated. The presence and concentration of hydroxyl groups on polypropylene surface was determined by structural analysis (FTIR, XPS), while the highest efficiency was achieved in the presence of nonionic wetting agents, using 10 mol. % potassium persulfate and at lower water/potassium persulfate molar ratio. Based on changes in polypropylene structure, the modification took place mainly in the amorphous phase of the polymer. In addition to hydroxylation, concurrent side reactions have been reported, in particular the oxidation of wetting agents and polypropylene, which has resulted in chain cleavage, reducing the average molecular weight of the polypropylene.
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