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No. of bitstreams: 2 Dissertação - Anderson Almeida Dias - 2016.pdf: 2267814 bytes, checksum: ee86b1492eb772ffa46bd1de1e5e9e4b (MD5) license_rdf: 0 bytes, checksum: d41d8cd98f00b204e9800998ecf8427e (MD5) Previous issue date: 2016-06-03 / Conselho Nacional de Pesquisa e Desenvolvimento Científico e Tecnológico - CNPq / This manuscript describes development of batch injection analysis (BIA) cells using a 3D printer as well show the fabrication of pencil draw electrode on paper platform. Bia cells were employed on wall-jet configuration coupled with amperometric system. Bia systems were used to detect a product reaction obtained by paper-microreactor and determine ethanol in whiskey samples. Fabrication process using 3D printer was simple, fast (lower than four hours) and cost effectiveness (ca. $ 3.43 and 1.07 to the 1st and 2nd generation of Bia system, respectively). The 1st generation of Bia cell was production to be couple with commercial screen printed electrodes (SPEs) by DropSens (DropSens, DPR 710 model) and 2nd generation have support to put home-made electrodes. Both Bia cells, present a specific compartment to be coupled the micropipette. Paperbased microreactors (MOPs) were used with the 1st generation of Bia cell and the system was employed to measure glucose through the generation of hydrogen peroxide by the reaction of glucose with glucose oxidase and amperometric detection of H2O2 generated in the reaction at a potential of -0.25 V vs. Ag. In the same way of Bia cell, MOPs fabrication process is simpler, faster and cheaper (ca. $ 0.02 cent each). In general, the system shows a good linear response for concentration range between 1 to 10 mmo L-1. The limit of detection (LD) and quantification (LQ) found were 0.11 mmol L-1 and 0.38 mmol L-1, respectively. Besides, the measure of glucose using five different MOPs presented a good repeatability (RSD between 1.5 to 2.8%) and reproducibility (RSD = 0.66%). The 2nd generation of Bia cell was coupled with copper working electrode modified thermally and chemically. This cell was employed to determine the presence of ethanol in whisky sample using 1 mol L-1 NaOH as supporting electrolyte and potential of 0.45 V vs Ag / AgCl. The modified-electrode shows optimum stability to measure seventy minute of consecutive injection with RSD lower than 4.7%. A good linear response was obtained when concentration of ethanol ranged from 2.5 to 25% (v/v). The LD achieved was ca. 0.07% (v/v). Besides the Bia cells experiments, this work describes the fabrication process of alternative electrodes by hand drawing pencil on paper platform. Initially, the geometry of sensing electrodes was drawn using a graphic software and printed on paper surface. During printing process, toner lines were deposited on paper to delimit the electrode area. Then, the desire layout was draw using a pencil and laminated using benchtop laminator. This last step is necessary to make the electrical insulation. Fabrication process of alternative electrodes was simple, fast (~ 20 minutes) and cost effectiveness (ca. $ 0,023). Characterization of paper electrodes was made by cyclic voltammetry with potassium ferrocyanide (5 mmol L-1) in KCl solution (0.5 mol L-1). Besides, showed good peak separation (ΔEp) ca. 238 mV and excellent reproducibility. The RSD was lower than 2.25% to five different electrodes. / Esta dissertação apresenta o desenvolvimento de células para análise por injeção em batelada (BIA, do inglês “batch injection analysis”) mediante uso de uma impressora 3D assim como a fabricação de eletrodos utilizando uma técnica de escrita direta em papel. As células BIA foram utilizadas com detecção eletroquímica, visando a análise de um produto de reação realizada em microrreatores de papel e, também, de etanol em amostras de uísque. As células BIA, fabricadas no laboratório por meio de uma impressora 3D, apresentaram baixo custo (cerca de R$ 12,00 e R$ 3,75 para 1° e 2° geração respectivamente), fabricação rápida (cerca de 4 horas e 1 hora e 40 minutos para 1° e 2° geração respectivamente) e robustez. Ambas as células BIA foram utilizadas com detecção amperométrica (DA) e apresentam configuração wall-jet. A 1° geração BIA possui suporte para eletrodos serigrafados (SPEs) comerciais da DropSens e pipeta eletrônica e a 2° geração BIA possui suporte para eletrodos convencionais construídos no laboratório e pipeta eletrônica. Os microrreatores à base de papel (MOPs) foram vinculados à 1° geração da célula BIA, este sistema foi utilizado para quantificação de glicose a partir da geração de peróxido de hidrogênio mediante a reação da glicose com glicose oxidase, e detecção do H2O2 gerado com SPEs de carbono modificado com azul da prússia (DropSens, modelo DPR 710) em um potencial de -0,25 V versus Ag. A confecção dos MOPs é simples, rápida (2 horas e 30 minutos) e de baixo custo (cerca de R$ 0,06 a unidade). Para a fabricação dos microrreatores a base de papel, primeiramente foi realizada a modificação química da superfície do papel. Para, em seguida, efetuar a imobilização covalente da enzima. Os ensaios realizados utilizando os MOPs vinculados a 1° geração da célula BIA com detecção amperométrica (BIADA) apresentaram linearidade para faixa de concentração entre 1 e 10 mmol L-1 (R² = 0,990), alta repetitividade (DPR entre 1,5% e 2,8%) e elevada reprodutibilidade (DPR = 0,66%) para 5 microrreatores. Os limites de detecção e quantificação obtidos foram de 0,11 mmo L-1 e 0,38 mmol L-1 respectivamente. A 2° geração da célula BIA foi acoplada com eletrodo de trabalho (ET) de cobre modificado por tratamento químico / térmico e utilizada para verificação de adulteração em uísques através da quantificação de etanol utilizando NaOH 1 mol L-1 como eletrólito suporte e potencial de 0,45 V versus Ag/AgCl. Os ensaios utilizando a 2° geração da célula BIA-DA apresentaram linearidade para faixa de concentração entre 2,5 e 25 % v/v de etanol (R² = 0,998) e elevada estabilidade (DPR = 4,7%) para aproximadamente 70 minutos de injeções consecutivas. O limite de detecção obtido para o etanol foi de 0,07% (v/v). Os eletrodos em plataforma de papel foram produzidos através da pintura direta com lápis. Para a fabricação destes dispositivos, primeiramente o layout dos eletrodos são impressos no papel para definir a área do desenho dos eletrodos. Em seguida os eletrodos são pintados com lápis, depois os dispositivos são plastificados com polaseal com o objetivo de isolar os contatos e delimitar a área dos eletrodos. A confecção destes eletrodos é rápida (~ 20 minutos) e de baixo custo (R$ 0,082 a unidade). Os eletrodos foram caracterizados utilizando voltametria cíclica com ferrocianeto de potássio 5 mmol L-1 solubilizado em KCl 0,5 mol L-1. Estes dispositivos apresentaram elevada reprodutibilidade (DPR = 2,25%) para 5 eletrodos distintos.

L'objectif de ce travail est la synthèse et la fonctionnalisation de monolithes siliciques à porosité hiérarchique et leur utilisation en tant que microréacteur en catalyse sous flux. Une synthèse reproductible de monolithes siliciques a été mise à point. La fonctionnalisation avec une variété de fonctions a été réalisée, telle que la fonctionnalisation avec des groupements aminopropyle, avec de l'oxyde d'aluminium, par incorporation des MOFs (CuBTC) et par dépôt de nanoparticules de palladium. Les monolithes fonctionnalisés ont été testés en tant que microréacteurs catalytiques sous flux pour les réactions de Knoevenagel, de Diels-Alder et de Friedländer et montrent dans plusieurs cas une augmentation de la productivité des réactions par rapport aux réacteurs batch ou à lit fixe ainsi qu'une automatisation des procédés. La transformation pseudomorphique de monolithes siliciques en monolithes zéolithiques en phase SOD et LTA a été mise a point. Nous avons ainsi montré la première utilisation d'un monolithe macroporeux à base de zéolithes en tant que microréacteur pour la synthèse de produits de chimie fine en continu. Les monolithes zéolithiques ont aussi été analysés pour l'échange d'ions en dynamique et sont prometteurs pour une application en tant que matériaux pour la décontamination d'effluents radioactifs. / The aim of this work is the synthesis and the functionalization of silica monoliths with hierarchical porosity and their use as catalytic microreactors for flow-through chemistry. A reproducible synthesis of the silica monoliths was elaborated. The functionalization with a variety of functions has been performed, such as aminopropyl groups, aluminium oxide, MOFs (CuBTC), and palladium nanoparticles. These functionalized silica monoliths have been used for the Knoevenagel condensation, Diels-Alder reaction and Fiedländer reaction, where they show increasing productivities compared to classically used reactors (batch, packed-bed) and enable process automation. The pseudomorphic transformation of silica monoliths in zeolite monoliths in the SOD and LTA phase has been elaborated. We have preformed the first implementation of a macroporous zeolite monolith as microreactor for the fine chemical production in flow continuous conditions. The zeolite monoliths have been tested for dynamic ion exchange and are promising materials for the use as decontaminants of radioactive discharges.

We investigate a nonlinear reaction-diffusion system coupled with convection- diffusion system. This combined system corresponds to physical description of heteroge- neous catalysis when the flow of bulk-constituents is driven by a given stationary velocity field; diverse mechanisms between bulk- and surface-parts of the model-domain are de- scribed by Langmuir-Hinshelwood absorption kinetics; and the irreversible reactions on the catalytic walls meets the law of mass action with quadratic rate. The first part of the thesis is focused on analytical results; in Chapter 2 we prove existence and unique- ness of a mild solution for so-called near-by problem using nonlinear semigroup theory; in Chapter 3 we investigate the weak formulation of the problem. We prove an existence of a weak solution for little modified problem which, under an assumption, coincides with the original problem. In the second part of the thesis (Chapter 4) we numerically investigate the evolution of the bio-diesel microreactor. We compute numerical solutions using several methods and we test the results by analytical and physical conditions; with the aim to find the most efficient way to compute precise and physically correct solution. Keywords: heterogeneous catalysis, coupled reaction-diffusion/convection-diffusion system, nonlinear...

Continuous milli-scale and micro-scale structures such as FlowPlate® microreactors have emerged as a promising element of process intensification due to their inherently effective rates of mass and heat transfer. These microfluidic devices have proven to be a preferred solution in place of energy-intensive batch processes for certain pathways of fine chemical and pharmaceutical synthesis, most notably fast reactions taking place on the scale of milliseconds to seconds. Computational fluid dynamics (CFD) has become an increasingly valuable tool in the field of microreactor design and optimization for its ability to locally map complex fluid flow patterns and resolve microscopic scales of reactive mixing that are challenging to characterize experimentally. The primary objective of this research was thus to develop and validate a mathematical model for the simulation of chaotic flow and homogeneous mixing in continuous microreactors. The model needed to be versatile enough to handle transition between flow regimes within a given reactor as well as the coexistence of both chaotic and laminar flow patterns in the micromixing elements that comprise said reactors. This was successfully achieved through the implementation of a k-ω SST (shear-stress transport) turbulence model that accounts for the impact of small-scale temporal and spatial fluctuations generated in the micromixer geometries studied herein; be it a liquid-liquid mixer (LLM), a serpentine (SZ) or a tangential (TG) mixer. In a first CFD study, the computational predictions were validated based on excellent agreement with experimental pressure loss (R^2 > 0.997) and residence time distribution (RTD) data (R^2 > 0.97) in several LL microreactors at Reynolds numbers ranging from 210 to 2140. Furthermore, the local velocity distribution and streamlines were mapped across the 3D domain of these reactors and it was discovered, based on the emergence of advective recirculation zones and turbulent dispersion, that a drastic change in flow behaviour occurred in these mixing elements at a Reynolds number of about 640. The interspacing of LLM elements with straight microchannels proved to be a suitable approach to modulating pressure loss while concurrently maintaining the chaotic secondary flow patterns generated from the mixers. In a second CFD study, the impact of micromixer geometry on the local velocity fields and advective transport performance was investigated both from a macromixing and micromixing perspective. Like the LLM, the SZ and TG mixers conferred chaotic secondary flow patterns at characteristic Reynolds numbers between 500 and 1000. As such, it was concluded that it would be ideal to operate these mixers at water flow rates of at least 30 ml/min. Contour plots of the velocity magnitude coupled with the computation of RTD showed that the SZ virtually mimics a plug-flow profile over a volume of 77 mm3 or greater at 50 g/min. The RTD of the LLM and TG resembles that of a mixed flow pattern given that approximately 65-80% of their fluid volume is occupied by recirculation zones. As such, it required 65 LLMs in series (3105 mm3) and 80 TGs (1142 mm3) to approach the same pattern as 10 SZs (77 mm3) from a macromixing perspective. Micromixing time distributions (MTD) were also characterized by locally computing the decay time of small-scale segregation (t_SSS) as a function of flow rate, wherein higher flow rates generated lower characteristic mixing times. The TG and LLM conferred the broadest range of mixing times, spanning nearly four orders of magnitude in the range of [0.02 ms, 10 ms], whereas the SZ generated a much narrower MTD ranging between [0.024 ms, 0.69 ms]. Finally, the impact of geometry and flow conditions on reaction yield was assessed by characterizing the extent of a finite-rate reaction relative to an infinitely fast reaction taking place in parallel. The calculated yield for the competitive-parallel reaction scheme showed that the second Damköhler number (Dall) computed based on the mean tSSS provides useful information about whether the process will be limited by the intrinsic rate of reaction or by the rate of mass transfer, even though the reaction process is controlled by a combination of the RTD as well as loss of LSS and SSS. It was concluded that the change in MTD as a function of power dissipation should coincide with the reaction yield response, and that any deviation in that relationship is because of macroscopic blending of reactants in the entrance region.

The need for clean and renewable fuel such as hydrogen is driven by a growing worldwide population and increasing air pollution from fossil fuels. One of the major barriers for the use of hydrogen in automotive industry is the storage of hydrogen. Physisorption is the most promising storage technique due to its high storage density, reversibility and rapid sorption kinetics besides being safe and volume-efficient. A major challenge for physisorption is the need to manage the heat of adsorption at cryogenic temperatures. In this thesis, a 6061 aluminum microchannel cooling plate is designed to remove the equivalent heat flux required by the adsorption of hydrogen within an adsorption bed. Therefore, the objective of this thesis is to determine whether laser welding and heat treating strategies can be developed for a 6061 aluminum microchannel cooling plate as part of a larger hydrogen storage thermal management system. Key manufacturing process requirements include controlling the hermeticity, strength and dimensional stability of the heat-treated weld joint. A hermetic microchannel cooling plate was successfully laser welded and heat treated using free convection in air to quench the solution heat treatment. The weld strength and warpage obtained were within acceptable limits. Experimental testing of the fabricated microchannel cooling plate showed acceptable percent error with an experimental heat removal rate within 13.4% of computational fluid dynamics (CFD) analyses and an average pressure drop error of 25%. Calculations show that the cooling plate developed could support a hydrogen storage thermal management system taking up 5.0% and 10.3% of the system displacement volume and mass, respectively. / Graduation date: 2013

The continuous microreactor-assisted solution deposition (MASD) process was used for the deposition of CdS thin films on fluorine-doped tin oxide (FTO) glass. The MASD system, including a T-junction micromixer and a microchannel heat exchanger is capable of isolating the homogeneous particle precipitation from the heterogeneous surface reaction. The results show a dense nanocrystallite CdS thin films with a preferred orientation at (111) plane. Focused-ion-beam was used for TEM specimen preparation to characterize the interfacial microstructure of CdS and FTO layers. The band gap of the microreactor-assisted deposited CdS film was determined at 2.44 eV. X-ray Photon Spectroscopy show the bindings of energies of Cd 3d₃/₂, Cd 3d₅/₂, S 2p₃/₂ and S 2p₁/₂ at 411.7 eV, 404.8 eV, 162.1 eV, and 163.4 eV, respectively. The film growth kinetics was studied by measuring the film thickness deposited from 1 minute to 15 minutes in physical (FIB-TEM) and optical (reflectance spectroscopy) approaches. A growth model that accounts for the residence time in the microchannel using empirical factor (η) obtained from previous reported experimental data. Applying this factor in the proposed modified growth model gives a surface reaction rate of 1.61*10⁶ cm⁴ mole⁻¹s⁻¹, which is considerable higher than the surface reaction rates obtained from the batch CBD process. With the feature of separating homogeneous and heterogeneous surface reaction, the MASD process provides the capability to tailor the surface film growth rate and avoid the saturation growth regime in the batch process. An in situ spectroscopy technique was used to measure the UV-Vis absorption spectra of CdS nanoparticles formed within the continuous flow microreactor. The spectra were analyzed by fitting the sum of three Gaussian functions and one exponential function in order to calculate the nanoparticle size. This deconvolution analysis shows the formation of CdS nanoparticles range from 1.13 nm to 1.26 nm using a residence time from 0.26 s to 3.96 s. Barrier controlled coalescence mechanism seems to be a reasonable model to explain the experimental UV-Vis data obtained from the continuous flow microreactor, with a rate constant k' value of 2.872 s⁻¹. Using CFD, low skewness value of the RTD curve at high flow rate (short τ) suggests good radial mixing at high flow rate is responsible for the formation of smaller CdS nanoparticles with a narrower size distribution. The combination of CdS nanoparticle solution with MASD process resulted in the hindrance of CdS thin film deposition. It is hypothesized that the pre-existing sulfide (S²⁻) ions and CdS nanoparticles changes the chemical species equilibrium of thiourea hydrolysis reaction. Consequently, the lack of thiourea slows down the heterogeneous surface reaction. To test the scalability of the MASD process, a flow cell and reel-to-reel (R2R)-MASD system were setup and demonstrated for the deposition of CdS films on the FTO glass (6" x 6") substrate. The film deposition kinetics was found to be sensitive to the flow conditions within the heat exchanger and the substrate flow cell. The growth kinetics of the CdS films deposited by R2R-MASD process was investigated by with a deposition time of 2.5 min, 6.3 min, and 9 min. In comparison with the continuous MASD process, the growth rate in R2R-MASD is higher, however more difficult to obtain a linear relationship with the deposition time. / Graduation date: 2012 / Access restricted to the OSU Community at author's request from Jan. 13, 2012 - Jan. 13, 2013

Cette étude est dédiée à l'amélioration du design des microréacteurs gaz-liquide. Le terme de microréacteur correspond à des appareils composés de canaux dont les dimensions sont de l’ordre de quelques dizaines à quelques centaines de microns. Grâce à la valeur importante du ratio surface/volume, ces appareils constituent une issue prometteuse pour contrôler les réactions rapides fortement exothermiques, souvent rencontrées en chimie fine et pharmaceutique. Dans le cas des systèmes gaz-liquide, on peut citer par exemple les réactions de fluoration, d’hydrogénation ou d’oxydation. Comparés à des appareils conventionnels, les microréacteurs permettent de supprimer le risque d’apparition de points chauds, et d’envisager le fonctionnement dans des conditions plus critiques, par exemple avec des concentrations de réactifs plus élevées. En même temps, la sélectivité peut être augmentée et les coûts opératoires diminués. Ainsi, les technologies de microréacteurs s’inscrivent bien dans les nouveaux challenges auxquels l'industrie chimique est confrontée ; on peut citer en particulier la réduction de la consommation énergétique et la gestion des stocks de produits intermédiaires. Les principaux phénomènes qui doivent être étudiés lors de la conception d’un microréacteur sont le transfert de matière et le transfert thermique. Dans les systèmes diphasiques, ces transferts sont fortement influencés par la nature des écoulements, et l'hydrodynamique joue donc un rôle central. Par conséquent, nous avons focalisé notre travail sur l’hydrodynamique de l’écoulement diphasique dans les microcanaux et sur les couplages constatés avec le transfert de masse. Dans ce contexte, nous nous sommes dans un premier temps intéressés aux régimes d’écoulement et aux paramètres contrôlant la transition entre les différents régimes. Au vu des capacités de transfert de matière et à la flexibilité offerte en terme de conditions opératoires, le régime de Taylor semble le plus prometteur pour mettre en œuvre des réactions rapides fortement exothermiques et limitées par le transfert de matière. Ce régime d'écoulement est caractérisé par des bulles allongées entourées par un film liquide et séparées les unes des autres par une poche liquide. En plus du fait que ce régime est accessible à partir d’une large gamme de débits gazeux et liquide, l'aire interfaciale développée est assez élevée, et les mouvements de recirculation du liquide induits au sein de chaque poche sont supposés améliorer le transport des molécules entre la zone interfaciale et le liquide. A partir d'une étude de l’hydrodynamique locale d’un écoulement de Taylor, il s’est avéré que la perte de charge et le transfert de matière sont contrôlés par la vitesse des bulles, et la longueur des bulles et des poches. Dans l’étape suivante, nous avons étudié l'influence des paramètres de fonctionnement sur ces caractéristiques de l’écoulement. Une première phase de notre travail expérimental a porté sur la formation des bulles et des poches et la mesure des champs de vitesse de la phase liquide dans des microcanaux de section rectangulaire. Nous avons également pris en compte le phénomène de démouillage, qui joue un rôle important au niveau de la perte de charge et du transfert de matière. Des mesures du coefficient de transfert de matière (kLa) ont été réalisées tandis que l'écoulement associé était enregistré. Les vitesses de bulles, longueurs de bulles et de poches, ainsi que les caractéristiques issues de l’exploitation des champs de vitesse précédemment obtenus, ont été utilisées afin de proposer un modèle modifié pour la prédiction du kLa dans des microcanaux de section rectangulaire. En mettant en évidence l'influence du design du microcanal sur l’hydrodynamique et le transfert de matière, notre travail apporte une contribution importante dans le contrôle en microréacteur des réactions rapides fortement exothermiques et limitées par le transfert de matière. De plus, ce travail a permis d'identifier certaines lacunes en termes de connaissance, ce qui devrait pouvoir constituer l'objet de futures recherches. / The present project deals with the improvement of the design of gas-liquid microreactors. The term microreactor characterizes devices composed of channels that have dimensions in the several tens to several hundreds of microns. Due to their increased surface to volume ratios these devices are a promising way to control fast and highly exothermic reactions, often employed in the production of fine chemicals and pharmaceutical compounds. In the case of gas-liquid systems, these are for example direct fluorination, hydrogenation or oxidation reactions. Compared to conventional equipment microreactors offer the possibility to suppress hot spots and to operate hazardous reaction systems at increased reactant concentrations. Thereby selectivity may be increased and operating costs decreased. In this manner microreaction technology well fits in the challenges the chemical industry is continuously confronted to, which are amongst others the reduction of energy consumption and better feedstock utilization. The main topics which have to be considered with respect to the design of gasliquid μ-reactors are heat and mass transfer. In two phase systems both are strongly influenced by the nature of the flow and thus hydrodynamics play a central role. Consequently we focused our work on the hydrodynamics of the two-phase flow in microchannels and the description of the inter-linkage to gas-liquid mass transfer. In this context we were initially concerned with the topic of gas-liquid flow regimes and the main parameters prescribing flow pattern transitions. From a comparison of flow patterns with respect to their mass transfer capacity, as well as the flexibility offered with respect to operating conditions, the Taylor flow pattern appears to be the most promising flow characteristic for performing fast, highly exothermic and mass transfer limited reactions. This flow pattern is characterized by elongated bubbles surrounded by a liquid film and separated from each other by liquid slugs. In addition to the fact that this flow regime is accessible within a large range of gas and liquid flow rates, and has a relatively high specific interfacial area, Taylor flow features a recirculation motion within the liquid slugs, which is generally assumed to increase molecular transport between the gas-liquid interface and the bulk of the liquid phase. From a closer look on the local hydrodynamics of Taylor flow, including the fundamentals of bubble transport and the description of the recirculation flow within the liquid phase, it turned out that two-phase pressure drop and gas-liquid mass transfer are governed by the bubble velocity, bubble lengths and slug lengths. In the following step we have dealt with the prediction of these key hydrodynamic parameters. In this connection the first part of our experimental study was concerned with the investigation of the formation of bubbles and slugs and the characterization of the liquid phase velocity field in microchannels of rectangular cross-section. In addition we also addressed the phenomenon of film dewetting, which plays an important rôle concerning pressure drop and mass-transfer in Taylor flow. In the second part we focused on the prediction of gas-liquid mass transfer in Taylor flow. Measurements of the volumetric liquid side mass transfer coefficient (kLa-value) were conducted and the related two-phase flow was recorded. The measured bubble velocities, bubble lengths and slug lengths, as well as the findings previously obtained from the characterization of the velocity field were used to set-up a modified model for the prediction of kLa-values in μ-channels of rectangular cross-section. Describing the interaction of channel design hydrodynamics and mass transfer our work thus provides an important contribution towards the control of the operation of fast, highly exothermic and mass transfer limited gas-liquid reactions in microchannels. In addition it enabled us to identify gaps of knowledge, whose investigation should be items of further research.