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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.
Effect of Ethylene and Propylene on Performance of Ziegler - Natta Catalyst in Stopped - Flow Polymerization
Hoza, Adam ; Kosek, Juraj (referee) ; Petrůj, Jaroslav (referee) ; Kratochvíla, Jan (advisor)
Výzkum v této práci byl zaměřen na přípravu a charakterizaci blokových kopolymerů typu polypropylen-blok-poly(propylenu-co-ethylenu) (dále jen PP-blok-EPR). Tyto materiály jsou považovány za účinné kompatibilizátory mezi semi-krystalickou polypropylenovou (PP) matricí a amorfními doménami statistického kopolymeru propylenu a etylenu (EPR) v rázuvzdorném sekvenčním kopolymeru (ICP) a proto byl výzkum zaměřen na zkoumání vlivu přídavku blokového kopolymeru PP-blok-EPR na vlastnosti komerčního ICP. Blokové kopolymery byly připraveny za použití techniky „stopped-flow“. Pro tento účel byla zkonstruována vysokotlaká polymerační „stopped-flow“ aparatura, která umožňuje syntézu kopolymerů PP-blok-EPR za podmínek blízkých podmínkám v průmyslových reaktorech pro výrobu komerčních ICP materiálů. Aparatura umožňuje vyrábět PP-blok-EPR polymer v množství dostačující na jeho charakterizaci a následnou přípravu směsí s komerčním ICP. Velmi krátké polymerační časy (obvykle kolem 0.2 s) kterých bylo dosaženo v kapilárním reaktoru aparatury „stopped-flow“ zajišťuje, že aktivní centra Ziglorova-Nattova katalyzátoru produkují polymer řetězce skládající se z bloku semikrystalického polypropylenu a bloku amorfního EPR kopolymeru. Takovéto molekuly jsou v literatuře popsány jako „skutečné blokové kopolymery PP-blok-EPR“. Kopolymery syntetizované v aparatuře „stopped-flow“ byly frakcionovány preparativní TREF (Temperature Rising Elution Fractionation) metodou a získané frakce byly následně analyzovány pomocí DSC, 13C-NMR a GPC/SEC. Tyto analýzy odhalily přítomnost amorfního EPR ve vysoce krystalické frakci (100-140 °C). Toto zjištění potvrdilo, že významná část polymerních řetězců, připravených v aparatuře „stopped-flow“ jsou blokové kopolymery skládající se z bloku semikrystalického PP homopolymeru a bloku amorfního EPR kopolymeru v jednom polymerním řetězci. Kopolymery získané metodou „stopped-flow" byly v tavenině smíchány s komerčním rázuvdorným kopolymerem ICP. U takto připravených směsí byly vyhodnoceny mechanické vlastnosti, DTMA a reologické vlastnosti a výsledky byly srovnány s vlastmi původního komerčního ICP kopolymeru. Dále byly studovány rozdíly v morfologii a umístění EPR domén v matrici PP prostřednictvím SEM. Zřetelný vliv kopolymeru PP-blok-EPR na vlastnosti ICP byl pozorován zejména v morfologických změnách EPR domén dispergovaných v PP matrici. Tyto změny mají pozitivní vliv na rovnováhu mezi modulem v ohybu a rázovou pevností ICP materiálu. Vliv kopolymeru PP-blok-EPR na reologické vlastnosti ICP byl nevýznamný. Podobně také v případě DTMA nebyl pozorován významný vliv kopolymeru PP-blok-EPR na vlastnosti ICP.
Research of Coatings of Hydrodynamically Lubricated Sliding Bearings for Combustion Engines
Repka, Martin ; Čermák, Roman (referee) ; Petrůj, Jaroslav (referee) ; Havlica, Jaromír (advisor)
Hlavní náplní této dizertační práce je výzkum a vývoj nové povrchové vrstvy pro kluzná ložiska na bázi pevných lubrikantů v polyamid-imidové polymerní matrici se zlepšenými tribologckými vlastnostmi. Podklady pro materiálovou kompozici vzešly z expertízy komerčně dostupného povlaku, respektive jeho povrchovou analýzou v mezných operačních podmínkách. Charakterizace mazného oleje před a po tribotestování společně s detailní povrchovou analýzou dala podmínky pro vznik materiálové formulace. Další část práce se zabývá studiem přípravy a vývojem aplikačního nanášení s přípravou polymerní směsi. Nakonec je popsána studie vlivu sulfidu molybdeničitého a grafitu, jakožto pevných lubrikantů pro zlepšení třecích vlastností a hydroxidu vápenatého pro potenciální zpepšení otěruvzdornosti výsledného povrchu pro palikaci kluzných ložisek.
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.
Functionalization of Polypropylene by Grafting
Kelíšek, Petr ; Sadílek, Jiří (referee) ; Petrůj, Jaroslav (advisor)
This bachelor thesis deals with the study of functionalization of polypropylene by grafting. The theoretical part summarizes current knowledge about the properties of polypropylene, polylactic acid, radical grafting, factors influencing the properties of such functionalized polymer and modification of immiscible polymers by the aid of compatibilizer. In the experimental part, samples of polypropylene grafted with polylactic acid, and blends of polypropylene with polylactic acid were prepared on an internal mixer under different conditions. Temperature and torque were monitored during the mixing. Created materials were evaluated by comparing their base properties (tensile strength, melt flox index).
Study of conditions influence on the rate of crack propagation in HDPE
Patzelt, Petr ; Kučera, Jaroslav (referee) ; Petrůj, Jaroslav (advisor)
Theoretical part of the thesis is aimed on the summary of material and testing parameters that influence SCG process and also the duration of FNCT test. The experimental part deals with the comparison of time to crack between two used surfactants – 2% Arkopal N110 and 10% sodium dodecylbenzenesulfonate. The temperature during the experiments was 80 °C. The acceleration of the process influenced by solution of sodium dodcelbenzenesulfonate was many times higher against solution of Arkopal. There were tested several HDPE and PP specimens to prove this phenomenon. HDPE specimens used – VB85, VL 20N, PL 10 that were made in UNIPETROL RPA and some other competitive materials were used. PP specimens were developed in labs of Polymer Institute Brno. In additional, another experimental part focuses on evolving the math definition of curves measured within FNCT tests and it is still in progress.
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.
Functionalization of polyolefins by grafting
Paulenka, Igor ; Petruš, Josef (referee) ; Petrůj, Jaroslav (advisor)
The theoretical part of the diploma thesis is focused on the funcionalization of polyolefins in order to accelerate their degradation and to increase their carbon content from renewable resources with focus on hydroxyacids. The experimental part is focused on preparing samples and studying the properties of the polypropylene and polyethylene blends with the polylactide with different contents of the initiator and the maleic anhydride. Samples were evaluated by determining the degree of conversion maleic anhydride, differential scanning calorimetry, infrared spectroscopy, melt flow index and mechanical properties.
Polymerization of Lactides in the Melt
Horkel, Ondřej ; Tomala, Libor (referee) ; Petrůj, Jaroslav (advisor)
This bachelor thesis deals with the problematics of Lactide polymerization in the melt. Theoretical part summarizes properties of lactic acid, lactides and polylactides as well as currently used methods of their preparation. In experimental part, a set of three experiments was designed, namely dependance of viscosity average molecular weight on catalyst concentration, polymerisation temperature and polymerisation time. This was achieved by measuring cinematic viscosity using Ubbelohde viscosimeter. As a result of these experiments, it was found that one of posssible combinations of conditions resulting in high molecular weight polymers is the following: concentration ratio of catalyst towards lactide 110–4, polymerisation teperature 160 °C and polymerisation time 3 hours.
PLA Synthesis in Solution
Svítil, Jan ; Zdeněk, Přikryl (referee) ; Petrůj, Jaroslav (advisor)
This thesis is studying PLA syntheses using polymerization of lactides in solution. Theoretical part deals with properties and production of lactic acid, lactides and polylactides. In the experimental part, possibilities of lactides polymerization in solution has been summerised and verified. Syntheses were performed via “solvothermal” method using 7 solvents (toluene, chloroforme, 1,2-chlorobenzene, acetone, tetrahydrofurane, cyclohexane and hexane). Using hexane as solvent, at concentration ratio catalyzer/lactide 1 : 1 000, polymerization temperature 160 °C and reaction time 20 h, polylactide of viscosity average molecular weight 179 000 gmol–1 was synthetized from the lactide.

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See also: similar author names
1 Petrůj, Jakub
2 Petrůj, Jan
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