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Effect of alternative agents on controlled degradation of polypropylene
Kadlecová, Zuzana ; Figalla, Silvestr (referee) ; Bílek, Vlastimil (advisor)
This bachelor’s thesis focuses on the effect of degradation agents in controlled rheology polypropylene and its efficiency. That was evaluated on several types of polypropylene with different molecular weight, the strength of stabilization and content of degradation reagents (organic peroxide and nitroxide Irgatec® CR 76). Melt flow rate, rheometry, and molecular weight distribution methods were applied. Results of each method for unstabilized, stabilized polypropylene and polypropylene containing degradation agent were compared. It was determined, that higher polymer chain degradation efficiency is provided by organic peroxide, lower by nitroxide. The molecular weight distribution of polypropylene was much narrower with peroxide than with nitroxide even though it should have been conversely according to published data. The molecular weight distribution of polypropylene (Mw/Mn) was much narrower with nitroxide than with peroxide at all process temperatures.
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New Processes of Lactid Acid Polymers Preparation
Figalla, Silvestr ; Svěrák, Tomáš (referee) ; Herink,, Tomáš (referee) ; Petrůj, Jaroslav (advisor)
The work focuses on new processes for the preparation of lactic acid derivatives. The main objective was to verify the feasibility of preparing high molecular weight polylactide using ethyl lactate as a precursor of lactide synthesis. Part of the work is devoted to the new ethyl lactate synthesis method. The experimental part of the thesis is divided into partial key steps on the way from the lactic acid to the high molecular polylactide. The preparation of anhydrous ethyl ester of lactic acid (EtLA) was solved in an innovative way using alcoholysis of the oligomeric lactic acid. A kinetic model for isothermal alcoholysis and equimolar reactants ratio was derived from this method. The ethyl lactate was oligomerized by transesterification into the low and high molecular weight oligomer with the help of newly found catalysts suitable for the reaction medium. Stannous lactate was used as catalyst for oligomerization of the low molecular weight polymer suitable for the preparation of lactide (Mn 1000 g.mol-1). Experimental polymerization of ethyl lactate into high molecular weight product in tens of kDa has been investigated with newly synthesized tetraethyllactoyl titanate, Ti(EtLA)4. The laboratory method was derived for the depolymerization of the oligomer into lactide. Optimal conditions found for lactidation are as follow: temperature 225 ° C, pressure 2 kPa, catalysis 0,05 mol% of stannous lactate (with respect to oligomer lactate units). The prepared lactide was refined to polymer grade purity by distillation and subsequent recrystallization from ethyl acetate and toluene. The method for the preparation of high molecular weight PLA through ROP polymerization of lactide has been optimized. By optimization, suitable catalyst concentration was found in combination with the polymerization temperature and the polymerization length. An equimolar mixture of Tin 2-ethylhexanoate and 1-decanol was used as the catalytic system. The optimal ROP conditions for achieving the maximum molecular weight and suppressed polymer coloration (yellowing) are: catalyst concentration 0,01 mol%, temperature 160 °C, and polymerization length 4 hours. PLA with molecular weight Mw= 447 ± 7,8 kg.mol-1 was prepared at these conditions and good repeatability of the result was achieved. The effect of naturally occurring lactide contaminants and their influence on the course and ROP result was experimentally verified on the optimized polymerization system. The purpose was to explore the effect of lactide contamination with water and ethanol as natural lactide contaminants. The results clearly confirm the orderly lower sensitivity of the polymerization system for the presence of ethanol as compared to water contamination. In the case of the presence of water, the course and the result of the polymerization in terms of both the conversion and achieved molecular weights are negatively affected, even when the water content is in the order of 0,001%. Conversely, the presence of ethanol has a positive effect on lactide conversion and polymer polydispersity. Lactides with an alcohol content of about one-tenth of a percent are suitable to reach molecular weights of PLA similar to commercially available products. This difference shoves a significant advantage in the proposed technology of preparing PLA from ethyl lactate, especially for easier purification of crude lactide into polymer grade purity.
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Functionalization of Polyethylene by Grafting
Hofmann, Jan ; Figalla, Silvestr (referee) ; Petrůj, Jaroslav (advisor)
The bachelor thesis deals with functionalization of polyethylene by grafting. The theoretical part summarizes informations about types of copolymers, free radical grafting techniques and the factors, that affect properties of modified polymers as well as their biodegradability. The experimental part deals with modification of polyethylene in kneader under various conditions. The blends are composed of polyethylene, polylactic acid and another aditives (initiator, stabilizers). The torque and the temperature were monitored during the kneading. Some mechanical properties of new materials were tested on Zwick Z010 apparatus. Rheological properties of samples were investigated with melt flow indexes.
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Bio-based composites made from lactic acid resins
Smiřický, Jan ; Černý, Miroslav (referee) ; Figalla, Silvestr (advisor)
This bachelor thesis is about the synthesis of polyurethane glue, which is capable of gluing together sawdust, and about the testing of the mechanical characteristics of the glue and sawdust compostion. This glue is biodegradable and is created from renewable resources, this is why it could be an appropriate replacement for phenol formaldehyde, melamine, and urea formaldehyde resins. Another indisputable advantage is the absence of arenes in the macromolecule structure, which can be carcinogenic. In this synthesis, the compounds polylactic acid and hexamethylene diisocyanate were chosen, the former as the polyol and the latter as the isocyanate. In the theoretical section of the thesis, the used compounds are described in terms of their characteristics, their creation and the tests of the composites as well. In the experimental section, the conducted experiments are described.
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Processing stability of polyhydroxybutyrate (PHB)
Palkovský, Radim ; Figalla, Silvestr (referee) ; Tocháček, Jiří (advisor)
The aim of this thesis was to observe and to evaluate the effects of selected additives on stabilization of two poly-3-hydroxybutyrates - Biomer and Hydal. In the experimental section of the thesis,the physical properties of pure polymers, polymers with mixture of polylactid acid, boron nitride and Citroflex 4A as well as the samples with five different additives which were added to this mixture, were meassured. Whilst processing the samples, the torque inside of the kneader was recorded. Tensile strength, Young´s modulus and relative extension were evaluated using tensile tests. Next, the differential scanning calorimetry was used to determine the melting points and their changes in comparison to the pure polymers. To evaluate the thermooxidative stability, method of induction periods was used, where the amount of time needed for degradation to make the material brittle was observed and recorded. These methods determined the the Stabilizer 9000 (Raschig) as the most suitable, owing to its better thermooxidative stability and considerable relative extension. As for DHT-4A on the other hand, it was proven that within P3HB it supports degrading processes, which devaluate the processing properties of this material even more. Amongst the other additives no significant influence on the material was observed and the changes of properties were attributed to the mixture of PLA and the other substances.
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Study of poly(lactic acid) foams preparation
Svatík, Juraj ; Petrůj, Jaroslav (referee) ; Figalla, Silvestr (advisor)
The bachelor thesis focuses on the processing of expanded poly(lactic acid) (PLA) or polylactide and on studying of some of its properties. The theoretical part deals with several ways of processing of PLA, its properties and methods of degradation. Furthermore, this part focuses on various processing methods of expanded PLA and the phenomena affecting the expansion, such as dissolving of gases in PLA. At the end of this part, it focuses on strength properties of PLA foams. The experimental part deals with specific way of processing of expanded PLA; that is dissolving of the physical blowing agent in PLA and subsequent foaming. Specific conditions within the processing of PLA foams are investigated there, such as pressure of gas needed, size of PLA particles. Further, this part focuses on distinct types of PLA foams differing in density or processing temperature. Last, it focuses on strength characteristics of PLA foams depending on their density and processing temperature.
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The Study of Ethyllactate Synthesis from Lactic Acide Salts
Hlavatá, Daniela ; Figalla, Silvestr (referee) ; Petrůj, Jaroslav (advisor)
This diploma thesis deals with senthesis of lactic acid ethyl ester from slats of lactic acid. The literature review has been processed in the theoretical part of the diploma thesis. It is focused on manufacturing technologies of lactic acid esters, mainly on ethyl lactate by conventional and non-conventional ways of producing. Also the literature review involves producing of lactic acid and slats of lactic acid by fermentation because subsequently is possible produce ethyl lactate from that two substances. The laboratory apparatus for preparation of ethyl lactate and methyl lactate has been designed, realized and verificated function of it in the experimental part. There were carried out laboratory experimnets for production ethyl lactate and methyl lactate in this apparaturs.
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The study of using lactic acid esters for preparing lactides and PLA
Vida, Mikuláš ; Figalla, Silvestr (referee) ; Petrůj, Jaroslav (advisor)
This diploma thesis deals with use of lactic acid esters for preparation of lactides and PLA. In the theoretical part, it has been processed literature review focus on manufacturing technologies and properties of lactic acid and its esters (especially ethyl ester and lactides). In the experimental part, it has been designed and realized functional laboratory apparatus for preparation of cyclic dimer of lactic acid – lactides. On this apparatus, there were carried out principal laboratory experiments leading to optimization of lactides yields using various catalysts.
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Optimization of Microwave Glycerolysis of Crosslinked Rigid PU Foams for Using Recyclate in Production
Figalla, Silvestr ; Kučera, František (referee) ; Petrůj, Jaroslav (advisor)
The theoretical part summarizes the chemical recycling processes of polyurethane and polyisocyanurate insulation foams and methods of polyols preparation from their alcoholysates. Emphasis is placed on the use of microwave heating during depolymerization, as a perspective energy source for chemolysis processes. The practical part is focused on optimization of recyclates preparation derived from polyisocyanurate foams and polyethylene terephthalate by microwave enhanced glycerolysis. Recyclates obtained were verified for their workability and applicability in blends with virgin polyols in polyisocyanurate foam manufacture process.
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Waste Recycling Possibilities of Rigid PU Foams from the Production of KingSpan CZ
Figalla, Silvestr ; Kučera, František (referee) ; Petrůj, Jaroslav (advisor)
The theoretical part of the bachelor thesis evaluates methods and trends of recycling polyurethane materials with the emphasis on rigid polyurethane foams used as thermo isolation building material. The experimental part is focused on glycerol process verification as an alcoholization agent in the regenerative process of polyol, together with perspective microwave heating of reaction mixture. The final part of the work suggests further steps in the development of above mentioned process with the aim of its transforming into technical practice.
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