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Síntese e caracterização de membranas de acetato de celulose, obtido do bagaço de cana-de-açúcar, e blendas de acetato de celulose com poliestireno de copos plásticos descartadosMeireles, Carla da Silva 23 February 2007 (has links)
Coordenação de Aperfeiçoamento de Pessoal de Nível Superior / In the present dissertation, the synthesis and characterization of cellulose acetate
membranes as well as cellulose acetate and polystyrene blends, were studied. Recycled materials
were used to produce the blends. Cellulose acetate (CA) was produced from sugarcane bagasse,
and waste plastic cups were used as polystyrene (PS) source. Blends, produced with different
CA/PS ratios, were characterized regarding the miscibility of their components. The techniques
utilized for membrane characterization were Fourier Transform Infrared Spectrometry (FTIR),
Differential Scanning Calorimetry (DSC), Thermogravimetric Analysis (TGA), Scanning
Electron Microscopy (SEM) and measurements of water diffusion through the membranes. The
results confirmed the existence of miscibility microregions in the blends and indicated a region of
transition when 30% PS was used, indicating a limit for a possible phase inversion between the
matrix and the disperse phase. The membranes were also characterized regarding their properties
of water flux, PEG rejection (utilizing an aqueous solution 1% w/v of polyethylene glycol, PEG,
45 kDa and 80 kDa) and ion diffusion by dialysis. The experiment of ion diffusion by dialysis
showed that the coefficients of ion diffusion of both the pure CA and the CA/PS blends were
comparable to previously reported values for commercial cellulose triacetate membrane. These
results showed that the membrane produced from recycled materials, sugarcane bagasse and
polystyrene cups, behaves likewise the commercial material. Regarding permeation driven by
difference of pressure, 12% w/w membrane showed the best performance and rejected 27% PEG
80 kDa. These preliminary results showed that this membrane should be better evaluated in the
range of application comprehending ultrafiltration or microfiltration processes. / Nesta dissertação estudou-se a síntese e caracterização de membranas de acetato de
celulose e blendas de acetato de celulose com poliestireno. Foram utilizados materiais reciclados,
sendo o acetato de celulose (AC) obtido pela reciclagem do bagaço de cana-de-açúcar, e o
poliestireno (PS) de copos plásticos descartados. As blendas, produzidas com diferentes
proporções de AC/PS, foram caracterizadas quanto a miscibilidade dos seus componentes. As
técnicas utilizadas foram a Espectrometria de Infravermelho com Transformada de Fourrier
(FTIR), Calorimetria Diferencial Exploratória (DSC), Análise Termogravimétrica (TGA),
Microscopia Eletrônica de Varredura (MEV) e medidas de difusão de água através das
membranas. Os resultados confirmaram a existência de microrregiões de miscibilidade nas
blendas, e também evidenciaram uma região de transição na proporção de 30% de PS, indicando
um limite para uma possível inversão de fases entre a matriz e a fase dispersa. As membranas
também foram caracterizadas por fluxo de água, rejeição ao PEG (de diferentes massas molares)
e difusão de íons por diálise, visando apontá-las para possíveis processos de separação. Os
experimentos de difusão de íons por diálise mostraram que o coeficiente de difusão de íons, tanto
das membranas de AC puro quanto das blendas AC/PS, foram comparáveis ao valor encontrado
na literatura para uma membrana de triacetato de celulose comercial. Estes resultados
demonstram que as membranas produzidas a partir de materiais reciclados, bagaço de cana-deaçúcar
e copos de poliestireno, apresentaram performance comparável àquela produzida de um
material comercial. Com relação ao experimento por diferença de pressão, a membrana de AC
12% mostrou a melhor performance e rejeitou 27 % do PEG 80 kDa. Estes resultados
preliminares mostram que esta membrana pode ser indicada para uma melhor avaliação em uma
faixa de aplicação que compreende os processos de ultrafiltração e microfiltração. / Mestre em Química
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Aplicações analíticas do eletrodo híbrido modificado acetato de celulose/grafite/azul da prússiaNectoux, Aline da Silveira January 2015 (has links)
Neste trabalho foram estudadas as potencialidades eletroanalíticas de um material híbrido condutor baseado em acetato de celulose e grafite com eletrodeposição de filme condutor de Azul da Prússia (CA/G/PB) como sensor para espécies com importância biológica. O material híbrido foi preparado pelo processo de inversão de fase e caracterizado pelas técnicas de microscopia eletrônica de varredura acoplada com espectroscopia de energia dispersiva (SEM-EDS) e voltametria cíclica. O composto Azul da Prússia (PB) foi imobilizado na superfície do material por eletropolimerização, aplicando-se um potencial fixo de 20 mV em uma janela de -0,3 V a 1,2 V. Os estudos eletroquímicos do eletrodo modificado CA/G/PB foram realizados em solução de KCl 0,1 mol.L-1, sendo obtidos dois pares redox para a espécie eletroativa imobilizada com potenciais médios (E0) em 0,204 V e 0,842 V, indicando um comportamento quase-reversível. O eletrodo demonstrou alta estabilidade após 500 ciclos redox, não sendo observada lixiviação da espécie eletroativa da superfície da matriz modificada. Os dois pares redox do material híbrido CA/G/PB permaneceram praticamente constantes entre os pH 5,0 e 8,0, indicando que as intensidades de pico não são significativamente afetadas nessa faixa de pH. A correlação linear entre as intensidades de pico e a raiz quadrada da velocidade de varredura, indicou que o sistema possui um comportamento similar aqueles em que o processo é controlado por difusão das espécies eletroativas à superfície do eletrodo. O azul da Prússia imobilizado foi aplicado na determinação de dopamina (DP), ácido úrico (AU), ácido ascórbico (AA) e Paracetamol (PCT) através da técnica de voltametria cíclica, voltametria de pulso diferencial e cronoamperometria. / In this work, we studied the electroanalytical potential of a conductive hybrid material based on cellulose acetate and graphite with electrodeposition Blue conductor film of Prussia (CA / G / PB) as a sensor for species with biological importance. The hybrid material was prepared by phase inversion process and characterized by the techniques of scanning electron microscopy coupled with energy dispersive spectroscopy (SEM-EDS) and cyclic voltammetry. The dye of Prussian blue (PB) was immobilized on the surface of the material by electropolymerization applying a fixed potential of 20 mV in a interval from -0.3 V to 1.2 V. The electrochemical behavior of the modified electrode CA / G / PB were performed in solution of 0.1 mol L-1 KCl being obtained two redox couples for the electroactive species immobilized with midpoint potentials (E0) in 0.204 V and 0.842 V, indicating a quasi-reversible behavior. The electrode showed high stability after 500 redox cycles with no observed leaching of electroactive species to the surface of the modified electrode. The two redox pair of the CA / G / PB electrode was kept practically constant within pH 5.0 and 8.0, indicating that the peak intensities are not significantly affected in this pH range. The linear correlation between peak intensities and the square root of scan rate, indicated that the system has a similar behavior those in which the process is controlled by diffusion of electroactive species to the electrode surface. The immobilized Prussian blue was applied to determine dopamine (DP), uric acid (UA), ascorbic acid (AA) and paracetamol (PCT) by analytical techniques of cyclic voltammetry, differential pulse voltammetry and chronoamperometry.
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Aplicações analíticas do eletrodo híbrido modificado acetato de celulose/grafite/azul da prússiaNectoux, Aline da Silveira January 2015 (has links)
Neste trabalho foram estudadas as potencialidades eletroanalíticas de um material híbrido condutor baseado em acetato de celulose e grafite com eletrodeposição de filme condutor de Azul da Prússia (CA/G/PB) como sensor para espécies com importância biológica. O material híbrido foi preparado pelo processo de inversão de fase e caracterizado pelas técnicas de microscopia eletrônica de varredura acoplada com espectroscopia de energia dispersiva (SEM-EDS) e voltametria cíclica. O composto Azul da Prússia (PB) foi imobilizado na superfície do material por eletropolimerização, aplicando-se um potencial fixo de 20 mV em uma janela de -0,3 V a 1,2 V. Os estudos eletroquímicos do eletrodo modificado CA/G/PB foram realizados em solução de KCl 0,1 mol.L-1, sendo obtidos dois pares redox para a espécie eletroativa imobilizada com potenciais médios (E0) em 0,204 V e 0,842 V, indicando um comportamento quase-reversível. O eletrodo demonstrou alta estabilidade após 500 ciclos redox, não sendo observada lixiviação da espécie eletroativa da superfície da matriz modificada. Os dois pares redox do material híbrido CA/G/PB permaneceram praticamente constantes entre os pH 5,0 e 8,0, indicando que as intensidades de pico não são significativamente afetadas nessa faixa de pH. A correlação linear entre as intensidades de pico e a raiz quadrada da velocidade de varredura, indicou que o sistema possui um comportamento similar aqueles em que o processo é controlado por difusão das espécies eletroativas à superfície do eletrodo. O azul da Prússia imobilizado foi aplicado na determinação de dopamina (DP), ácido úrico (AU), ácido ascórbico (AA) e Paracetamol (PCT) através da técnica de voltametria cíclica, voltametria de pulso diferencial e cronoamperometria. / In this work, we studied the electroanalytical potential of a conductive hybrid material based on cellulose acetate and graphite with electrodeposition Blue conductor film of Prussia (CA / G / PB) as a sensor for species with biological importance. The hybrid material was prepared by phase inversion process and characterized by the techniques of scanning electron microscopy coupled with energy dispersive spectroscopy (SEM-EDS) and cyclic voltammetry. The dye of Prussian blue (PB) was immobilized on the surface of the material by electropolymerization applying a fixed potential of 20 mV in a interval from -0.3 V to 1.2 V. The electrochemical behavior of the modified electrode CA / G / PB were performed in solution of 0.1 mol L-1 KCl being obtained two redox couples for the electroactive species immobilized with midpoint potentials (E0) in 0.204 V and 0.842 V, indicating a quasi-reversible behavior. The electrode showed high stability after 500 redox cycles with no observed leaching of electroactive species to the surface of the modified electrode. The two redox pair of the CA / G / PB electrode was kept practically constant within pH 5.0 and 8.0, indicating that the peak intensities are not significantly affected in this pH range. The linear correlation between peak intensities and the square root of scan rate, indicated that the system has a similar behavior those in which the process is controlled by diffusion of electroactive species to the electrode surface. The immobilized Prussian blue was applied to determine dopamine (DP), uric acid (UA), ascorbic acid (AA) and paracetamol (PCT) by analytical techniques of cyclic voltammetry, differential pulse voltammetry and chronoamperometry.
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Cellulose acetate / plasticizer systems : structure, morphology and dynamics / Systèmes d'acétate de cellulose plastifiés : structure, morphologie et dynamiqueBao, Congyu 28 April 2015 (has links)
Les polysaccharides sont l'une des principales options à retenir pour progresser dans l'utilisation ou la conception de polymères renouvelables. Depuis les années cinquante, le développement industriel de ce type de polymères s'était considérablement réduit du fait de l'avènement des polymères synthétiques. Cependant, cet intérêt a cru considérablement ces dernières années en raison de la sensibilisation du public sur la limite des ressources fossiles. Ces biopolymères sont donc devenus un sujet d'importance, tant sur le plan industriel que sur celui de la recherche fondamentale. Toutefois, les systèmes à base de polysaccharides sont le plus souvent transformés via l'utilisation d'importantes quantités de solvants (y compris l'eau), ce qui globalement pénalise le procédé associé en l'affligeant d'une charge environnementale supplémentaire. Par la voie ‘fondue', le développement de polymères thermoplastiques à base de dérivés de la cellulose est un véritable défi, qui concerne autant le mode de transformation de ces systèmes que le niveau des propriétés du matériau final. Pour exemple, la température de dégradation de l'acétate de cellulose (CA) (dont le degré de substitution 2,5 est développé par le Groupe Solvay) est si proche de sa température de fusion que son procédé de mise en oeuvre ne peut être envisagé qu'avec l'ajout d'une quantité importante de plastifiants externes (entre 20 et 30 en poids selon le type d'additif). Le comportement d'un mélange CA-plastifiant est principalement régi par un «réseau» de très fortes interactions polaires, dont la force et la densité dépendent de 3 paramètres spécifiques: le degré de substitution de CA, la typologie de plastifiant et la quantité de plastifiant. Pour expliquer les différents mécanismes de plastification, il est donc important pour nous d'étudier et de comprendre les propriétés dynamiques (en ce qui concerne les phénomènes de relaxation) de ce type de systèmes et comment les trois leviers que nous avons identifiés peuvent influencer ou moduler les différentes interactions échangées dans les mélanges / Polysaccharides are one of the main options to the on-going move towards the use of renewable polymers. The industrial interest in this type of polymers drastically shrunk by the advent of synthetic polymers in the fifties, but is currently reviving due to the public awareness on the limit of fossil resources. These biopolymers are nowadays offering a challenging and industrially profitable playground for researchers. However, current polysaccharides based materials are mostly processed with extensive use of solvents (including water) making the total process an environmental burden despite the advantage of the starting material. Development of thermoplastic cellulose-based materials is very challenging regarding both final material properties and polymer processing. The degradation temperature of Cellulose Acetate (CA) (degree of substitution 2.5) is so close to its melting temperature that it can only be processed with a significant amount of external plasticizers (between 20 et 30 wt.% depending on the type of the additive). Behavior of a CA-plasticizer blend is mainly governed by a ‘network’ of high polar interactions, the strength and the density of which clearly depend of 3 specific parameters: the CA’s degree of substitution, the typology of the plasticizer, the amount of plasticizer. In an attempt to explain the different plasticization mechanisms, it is thus of utmost importance for us to study and understand the dynamic properties (regarding the relaxation phenomena) of this kind of systems and how the three levers that we identified can influence or modulate the different interactions exchanged within the blends
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Fluide supercritique et liquide ionique comme plastifiants de polymères biosourcés : application à l'amidon et à l'acétate de cellulose / Supercritical fluid and ionic liquid as plasticizes on natural-based polymersBendaoud, Amine 13 November 2014 (has links)
Les biopolymères constituent une alternative crédible à l’utilisation des plastiques issus de ressources pétrolières. Dans cette étude, la transformation de l’amidon et de l’acétate de cellulose en présence de liquides ioniques en voie fondue (par extrusion) a été réalisée. Les caractéristiques physico-chimiques des formulations obtenues ont montré une dépendance vis-à-vis du type et de la concentration de plastifiant utilisé, mais aussi de l’humidité relative appliquée. De manière générale, les liquides ioniques ont présenté comparativement à des plastifiants usuels: une interaction plus privilégiée avec les deux polymères, une réduction beaucoup plus importante de la cristallinité, une diminution significative de la température de transition vitreuse et une plastification efficace des deux matrices polymères étudiées. Dans un deuxième temps, on s’est intéressé à associer le pouvoir de solvatation et de plastification du dioxyde de carbone supercritique (CO2Sc) sur la mise en oeuvre de l’amidon par les liquides ioniques. Les résultats les plus importants ont montré que le CO2Sc est capable d’interagir sur l’amidon et sur les liquides ioniques, de sorte qu’il peut induire une diminution de la température de la transition vitreuse de l’amidon plastifié / Biopolymers are viable alternatives to the use of conventional plastics derived from fossil fuels resources. In this study, our objective, beyond doing the melt processing ionic liquids plasticized starch and cellulose acetate in laboratory scale microcoumpounder which simulate the performance of a co-rotating twin screw extruder, are to investigate the effects and influence of ionic liquids and water on the intrinsic properties of the materials which are prepared. In general ways, processing with ionic liquids compared with conventional plasticizers, presents: a better interaction with starch and cellulose acetate, a more efficient depressor of glass transition temperature and allows the production of processed materials with efficient crystallinity destruction and plasticization. In the second step, we investigate the effects of supercritical carbon dioxide on the processing of starch with ionic liquid and the effects of the processing pressure, temperature and duration of supercritical carbon dioxide (ScCO2), which is an environmentally-friendly component, on the properties of plasticized starch. The significant results show that ScCO2 is capable of interacting with starch chains and with ionic liquids, so that it may induce a decrease in the glass transition temperature of the plasticized starch
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Antimicrobial activity and dye photodegradation of titanium dioxide nanoparticles immobilized on polyacrylonitrile-cellulose acetate polymer blended nanofibers.Nkabinde, Sibongile Chrestina January 2019 (has links)
M. Tech. (Department of Chemistry, Faculty of Applied and Computer Sciences), Vaal University of Technology. / Electrospinning is a method that has gained more attention due to its capability in spinning a wide variety of polymeric fibers and nanoparticles embedded in polymer fibers. Polymer blending has been considered the most appropriate way for creating new materials with fused properties which improve poor chemical, mechanical, thermal and dynamic mechanical properties of each polymer. Hence, in this study, electrospinning technique was used to fabricate polyacrylonitrile (PAN) nanofibers at concentrations of (10, 12 and 14 wt%) and cellulose acetate (CA) nanofibers at concentrations of (14, 16 and 18 wt%). 10wt% of PAN and 16 wt% of CA were blended together and the optimum blend ratio was found to be 80/20 PAN/CA. TiO2 nanoparticles (0.2 and 0.4 wt%) were incorporated into CA nanofibers and (1, 2 and 3 wt%) were incorporated into PAN and PAN/CA blended polymers, respectively. Applied voltages of 20, 22 and 24 kV were varied at a spinning distance of 15cm and the optimum voltage for the fabrication of composite was 22 kV. The sol-gel method was used to synthesise the TiO2 nanoparticles at different calcination temperatures of 400, 500 and 600 ºC. The fabricated composite nanofibers were tested for antibacterial and photocatalytic activities. The synthesised nanomaterials were characterized using SEM, TEM, EDX, UV-Vis, PL, FTIR spectroscopy, XRD and TGA. The absorption and emission spectra illustrated the formation of TiO2 nanoparticles and the increase in absorption band edges. TEM showed the spherical morphology of the nanoparticles with average diameter of 12.2 nm for nanoparticles calcined at 500 ºC. SEM illustrated the diameter and morphology of the nanofibers and composites with the average diameter of 220, 338, 181, 250, 538, 294 nm for PAN, CA, PAN-TiO2, CA-TiO2, PAN/CA and PAN/CA-TiO2, respectively. XRD revealed anatase phase as the dominant crystalline phase of the synthesised nanoparticles. FTIR spectroscopy and EDX signified that the formation of composite nanofibers and the presence of TiO2 nanoparticles corresponded to the Ti-O stretching and Ti-O-Ti bands on the FTIR spectra. The antimicrobial activity of the composite nanofibers were tested against E. coli, S. aureus and C. albicans microorganisms. The photocatalytic activity of the nanomaterials was tested using methyl orange dye. PAN/CA-TiO2 composite nanofibers revealed the greatest antibacterial activity against selected microorganisms as compared to the other nanocomposites. PAN/CA-TiO2 nanocomposite (44%) showed greater rate of photodegradation of methyl orange than PAN-TiO2 nanofibers (28%) and TiO2 nanoparticles (12%) under visible light irradiation.
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The effect of chloramines on diffusion controlled membrane degradationCi, Yihua 01 April 2003 (has links)
No description available.
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Otimização das colunas de absorção da recuperação de acetona na produção de Filter Tow por meio de estudos fenomenológicos e análise estatística. / Optimization of the absorption columns in the acetone recovery at the Filter Tow production by phenomenological studies and statistical analysis.Nasser Junior, Roberto 13 November 2009 (has links)
A absorção é a etapa determinante da recuperação de acetona no Filter Tow, por reduzir a emissão de acetona e trazer melhorias à economia. Por isso, ela constitui o objeto deste estudo, que inclui desde a revisão dos conceitos fenomenológicos, considerando a escolha do melhor modelo de equilíbrio líquido-vapor, passando pela execução dos balanços coerentes de massa e o estabelecimento da Fotografia da situação original, relatando um caso complexo de transposição de pratos para recheios. Contudo, a operação das colunas de absorção é influenciada por outras variáveis de caráter desconhecido, ruídos em relação à fenomenologia, o que se pretende avaliar, justificando-se desenvolver estudo para avaliar seus efeitos. Com o objetivo geral de otimizar absorção, uma análise estatística foi executada a partir do levantamento de dados operacionais, utilizando todas suas variáveis, sejam as fenomenológicas, como os ruídos, com o objetivo específico de obter modelos empíricos que complementem as simulações fenomenológicas, aumentando sua abrangência. Para a execução da análise estatística, os conjuntos de dados históricos foram levantados e validados pelos balanços coerentes de massa e pela Fotografia, o que tornou possível sua evolução, desde a seleção das variáveis, até estabelecer os modelos de regressão, com os quais pode-se obter um novo modo de controle, que estabiliza a operação, possibilitando a otimização. Em termos ambientais, a utilização destes modelos resulta em redução de até 15% das perdas de acetona para o ambiente, como também de consumo energético, com uma economia da ordem de 1 milhão de reais por ano, sem quaisquer custos adicionais. / Absorption is the key step of the acetone recovery at Filter Tow production, for reducing the acetone emission and improving economics. For this reason it is the subject of this study, including the revision of phenomenological concepts, considering the choice of the best vapor liquid equilibrium model, passing by the improvement of coherent mass balances and establishing the Photography of the original situation, detailing a complex case of transposition of sieve trays to structured packing. However, the operation of the absorption columns is influenced by other variables, with unknown impacts, noises in relation to the phenomenology, justifying the development of this study, for evaluating them. With the general objective of optimizing the absorption, a statistical analysis is performed from collecting operating data, considering all variables, phenomenological and noises, with the specific objective of getting empirical models complementing the phenomenological simulations, increasing their comprising. For performing the statistical analysis sets of historical data have been collected and validated by coherent mass balances and the Photography, making possible its evolution, from the selection of the variables till establishing the regression models, and with them getting a new control way, which stabilizes the operation, allowing the optimization. In environmental terms, the use of these models results in up to 15% decrease in acetone losses to the environment, as well as power consumption with a saving of approximately 1 million reais per year, without any additional costs.
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Preparation, characterization and carrier gas transport characteristics of inorganic and organic membranes for application in lactic acid esterification with ethanolOkon, Edidiong January 2018 (has links)
Ethyl lactate (EL) plays a major role as green solvent and also a replacement for most petrochemical solvents. The esterification process of lactic acid and ethanol to produce EL is an equilibrium-limiting reaction and the selective removal of one of the reaction products can be improved using a membrane reactor and when coupled with a heterogeneous catalyst offers an opportunity for process intensification. This thesis investigates the batch process esterification reaction involving lactic acid (LA) and ethanol (EL) in the presence of a water selective membrane using different cation-exchange resin catalysts. The product was analysed using gas chromatograph coupled with mass spectrometry detector (GC-MS). The analytical methods used for the characterisation of the cation-exchange resins and membrane include Fourier transform infrared coupled with attenuated total reflectance (FTIR-ATR), scanning electron microscopy attached to energy dispersive analyser (SEM/EDAX), Liquid nitrogen physisorption and nuclear magnetic resonance (NMR) respectively. A novel method was developed for carrying out esterification reaction in a gaseous phase system using a flat sheet polymeric membrane. Prior to the esterification reaction, different carrier gases were tested with ceramic membrane to determine the suitable carrier gases for the analysis of esterification product. The four carrier gases used for the permeation test were argon (Ar), helium (He), carbon dioxide (CO2) and nitrogen (N2). A 15nm pore size commercially available tubular ceramic support, consisting of 77%Al2O3 and 23%TiO2 with the porosity of 45% was used for the carrier gas investigation. The support was modified with silica based on the sol-gel dip-coating techniques. The dip-coated membrane exhibited a higher molar flux with He (0.046mol m-2s-1) and Ar (0.037mol m-2s-1) with a much lower flux for N2 (0.037mol m-2s-1) and CO2 (0.035 mol m-2s-1) at 0.30 bar. Helium gas with the highest permeation rate were identified as the suitable carrier gas for the analysis of esterification product with GC-MS. The esterification reaction in the presence of four cation-exchange resins to produce ethyl lactate was carried out between 60-160 oC in a batch and membrane processes to determine the effectiveness resin catalysts for LA esterification. The effect of external mass transfer diffusion limitation between the liquid components and the resin catalysts was avoided by increasing the agitation time of the esterification reaction. The percentage conversion rate of the lactic acid feed from the batch process esterification was found to be in the range of 98.6 to 99.8%. The reaction kinetics of the esterification reaction was described based on two simplified mechanisms of Langmuir Hinshelwood model to describe the adsorption components on the surface of the catalysts. The lactic acid feed gave a conversion rate of up to 100 % confirming the effectiveness of the acetate membrane impregnated resin catalysts in the selective removal of water for the separation of ethyl lactate. The significance of producing ethyl lactate through batch process intensified by a water-selective membrane processes can be recommended for industrial LA production.
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Suitability of cellulose ester derivatives in hot melt extrusion : thermal, rheological and thermodynamic approaches used in the characterization of cellulose ester derivatives for their suitability in pharmaceutical hot melt extrusionKarandikar, Hrushikesh M. January 2015 (has links)
Applications of Hot Melt Extrusion (HME) in pharmaceuticals have become increasingly popular over the years but nonetheless a few obstacles still remain before wide scale implementation. In many instances these improvements are related to both processing and product performance. It is observed that HME process optimisation is majorly focused on the active pharmaceutical ingredient's (API) properties. Characterising polymeric properties for their suitability in HME should be equally studied since the impact of excipients on both product and process performance is just as vital. In this work, two well-established cellulose ester derivatives: Hydroxy Propyl Methyl Cellulose Acetate Succinate (HPMCAS) and Hydroxy Propyl Methyl Cellulose Phthalate (HPMCP) are studied for their HME suitability. Their thermal, thermodynamic, rheological, thermo-chemical and degradation kinetic properties were evaluated with model plasticisers and APIs. It was found the thermal properties of HPMCP are severely compromised whereas HPMCAS is more stable in the processing zone of 150 to 200 °C. Thermodynamic properties revealed that both polymers share an important solubility parameter range (20-30 MPa P1/2P) where the majority of plasticisers and BCS class II APIs lie. Thus, greater miscibility/solubility can be expected. Further, the processability of these two polymers investigated by rheometric measurements showed HPMCAS possesses better flow properties than HPMCP because HPMCP forms a weak network of chain interactions at a molecular level. However, adding plasticisers such as PEG and TEC the flow properties of HPMCP can be tailored. The study also showed that plasticisers have a major influence on thermo-chemical and kinetic properties of polymers. For instance, PEG reduced polymer degradation with reversal in kinetic parameters whereas blends of CA produced detrimental effects and increased polymer degradation with reduction in onset degradation temperatures. Further, both polymers are observed to be chemically reactive with the APIs containing free -OH, -SOR2RN- and -NH2 groups. Finally, these properties prove that suitability of HPMCP is highly debated for HME and demands great care in use while that of HPMCAS is relatively better than HPMCP in many instances.
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