Destilação molecular centrífuga e de filme descendente: aplicação em óleos vegetais / Centrifugal and descending film molecular distillation: application to vegetable oils

A Destilação Molecular Centrífuga (CMD) e a Destilação Molecular por Filme de Queda (FFMD) serão apresentadas como uma importante operação unitária para obter produtos de alto valor acrescentado sem a utilização de qualquer solvente. Os carotenóides foram obtidos a partir de óleo de palma por CMD. Outra aplicação envolveu o enriquecimento de diterpenos de café a partir de óleo de café verde utilizando a Destilação Molecular por Filme de Queda (FFMD). Os destilados foram enriquecidos em ésteres de ácidos gordos diterpenos e ácidos gordos livres, enquanto os resíduos foram enriquecidos em triacilgliceróis de alta massa molar. Os ésteres de ácidos gordos diterpénicos foram enriquecidos a 42% (o óleo de café verde original tinha 24,4%) num único passo. Estas aplicações mostraram a importância e a versatilidade da destilação molecular para diferentes processos

Extension of the true boiling point curve for national heavy petroleums through nolecular distillation process

Orientadores: Maria Regina Wolf Maciel, Cesar Benedito BatistellaTese (doutorado) - Universidade Estadual de Campinas, Faculdade de Engenharia QuimicaResumo: Destilação Molecular é um processo de separação que utiliza alto vácuo, temperaturas de operação reduzidas e curta exposição do material à temperatura operacional. O termo resíduo de vácuo (frações pesadas de petróleo) se refere ao fundo da destilação à vácuo, que tem uma temperatura atmosférica equivalente (TAE) acima de 540oC. A determinação da curva de Ponto de Ebulição Verdadeiro (PEV) é bem estabelecida para frações de petróleos que alcançam o PEV de aproximadamente 565oC por meio da Sociedade Americana de Testes e Materiais. Para temperaturas mais elevadas, não existe, ainda, um método padronizado. O objetivo deste trabalho foi desenvolver um método novo e apropriado para estender a curva PEV para ser utilizada na caracterização de resíduos de vácuo de petróleos pesados. Por meio de um destilador molecular de filme descendente, experimentos foram realizados usando frações pesadas de petróleos brasileiros, onde as temperaturas operacionais foram aumentadas sistematicamente. As frações obtidas em cada uma das temperaturas pré-estabelecidas foram coletadas, quantificadas e caracterizadas para ambas as correntes do destilador. Com uma melhor caracterização dos petróleos brasileiros, que são considerados pesados, será possível aumentar os rendimentos operacionais nas refinarias, além da obtenção de produtos de alto interesse comercial. De acordo com os resultados obtidos, foi possível estender a curva PEV através do processo de Destilação Molecular com boa precisão utilizando a correlação FRAMOL desenvolvida. Isto é de extrema importância, uma vez que permite definir melhores estratégias e condições operacionais para o processamento de petróleo, representando um progresso considerável na análise de frações pesadas de petróleo. Os desenvolvimentos realizados nesse trabalho são muito importantes desde que nenhuma metodologia padronizada está disponível para cálculo da curva PEV estendida e devido à grande quantidade de petróleo pesado encontrado hojeAbstract: Molecular Distillation is a separation process which explores high vacuum, operation at reduced temperatures and brief exposition of the material to the operating temperature. The term vacuum residue (heavy petroleum fractions) refers to the bottom of the vacuum distillation, which has an atmospheric equivalent temperature (AET) above 540oC. The determination of the True Boiling Point (TBP) curve is well established for petroleum fractions that reach the TBP up to 565°C by the American Society for Testing and Materials (ASTM). Even so, for higher temperatures, these does not exist a standard methodology as yet. The objective of this work is to develop a new and more appropriated method to extend the TBP curve in order to use it for characterizing vacuum residue of heavy petroleum. Through falling film molecular distillator, experiments were carried-out using heavy fractions of Brazilian petroleum, where operating temperatures were increased systematically. The fractions obtained in each one of the pre-established temperatures were collected, quantified and characterized for both streams of the distillator. With a better characterization of the Brazilian petroleum, which is considered heavy, it will be possible to increase the operational yields in refineries, besides obtaining products of greater commercial interest. Regarding the results obtained, it is possible to extend the TBP curve through Molecular Distillation process with very good precision using the FRAMOLDoutoradoDesenvolvimento de Processos QuímicosDoutor em Engenharia Químic

Thermal Characterization Of Orange, Lemongrass, And Basil Essential Oils

In this work, it was performed the thermoanalytical characterization of three essential oils (Orange, Lemongrass, and Basil) using techniques of thermogravimetry (TG/DTG) and differential scanning calorimetry (DSC). Thermogravimetry analysis provided information on essential oil thermal stability. TG/DTG data were correlated to Arrhenius equation to provide evaporation kinetic parameters, including: Activation energy (Ea), and frequency factor (A). DSC analyses were conducted over a temperature range from -150 to 300°C and showed the presence of endothermic peaks related to the process of evaporation for all these three oils. Differently from Orange and Lemongrass oils that showed only one phase change (vaporization), the DSC profile of Basil essential oil revealed three thermal events: Two endothermic peaks due to melting and vaporization, and an exothermic peak attributed probably to a change in the solid structure before melting. The importance of thermal characterization of essential oils is to drive new technological developments to supply the market demand for new products. © 2011, AIDIC Servizi S.r.l.24463468Aggarwal, P., Dollimore, D., Alexander, K., The use of thermogravimetry to follow the rate of evaporation of an ingredient used in perfumes (1997) Journal of Thermal Analysis, 49 (2), pp. 595-599Choi, M.J., Soottitantawat, A., Nuchuchua, O., Min, S.G., Ruktanonchai, U., Physical and light oxidative properties of eugenol encapsulated by molecular inclusion and emulsion-diffusion method (2009) Food Research International, 42, pp. 148-156Hazra, A., Alexander, K., Dollimore, D., Riga, A., A characterization of some essential oils and their key components (2004) Journal of Thermal Analysis and Calorimetry, 75, pp. 317-330Hazra, A., Dollimore, D., Alexander, K., Thermal analysis of the evaporation of compounds used in aromatherapy using thermogravimetry (2002) Thermochimica Acta, pp. 392-393. , 221-229Hsui-Mei, C., Hua-Hsien, C., Yen-Ming, L., Ching-Yen, C., Hung-Lung, C., Carbonyl species characteristics during the evaporation of essential oils (2010) Atmospheric Environment, 44, pp. 2240-2247Hua-Hsien, C., Hsui-Mei, C., Cho-Ching, L., Ching-Yen, C., Hung-Lung, C., Constituents of volatile organic compounds of evaporating essential oil (2009) Atmospheric Environment, 43, pp. 5743-5749Sansukcharearnpon, A., Wanichwecharungruang, S., Leepipatpaiboon, N., Kerdcharoen, T., Arayachukeat, S., High loading fragrance encapsulation based on a polymer-blend: Preparation and release behavior (2010) International Journal of Pharmaceutics, 391, pp. 267-273Zhang, X., Jong, W., Preto, F., Estimating kinetic parameters in TGA using B-spline smoothing and the friedman method (2009) Biomass and Bioenergy, 33, pp. 1435-144

Enrichment of oxyterpenes from orange oil by short path evaporation

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)The developing of processes to perform orange oil deterpenation is an important operation to guarantee the industrial application of this material. By not using organic solvents, presenting a small residence time, and operating at low pressures, short path evaporation is an alternative to deterpenate orange oil. However, the determination of its suitable operating conditions is not trivial. Therefore, in this work, the variables: evaporator temperature, condenser temperature, and feed flow rate, were studied aiming to determine the best orange oil deterpenation operating conditions by short path evaporation. In the range of study, the product obtained at 1.33 kPa, using evaporator temperature of 82.5 degrees C, condenser temperature of 0 degrees C, and feed flow rate of 10.5 ml/min presented the richest oxygenated fraction due to removing more than 95% of limonene initial content. The concentration of linalool and decanal, oxygenates representatives, were respectively 4.5 and 13 times higher than the initial raw material concentration. (c) 2013 Elsevier B.V. All rights reserved.116385390Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES

Short path evaporation for methyl chavicol enrichment from basil essential oil

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)In this work, the evaluation of methyl chavicol enrichment from basil essential oil was carried out using short path evaporation. The evaluation was performed by experimental design using response surface methodology. Evaporator temperature (from 28 to 112 degrees C), condenser temperature (from -8.4 to 8.4 degrees C), and feed flow rate (from 8.3 to 21.7 ml/min) were the studied factors. The results showed that it is possible to increase methyl chavicol concentration up to 89.79% from basil essential oil using a short path evaporator. Process analysis showed that a quadratic model is adequate to describe methyl chavicol concentration using short path evaporation and that evaporator temperature was the unique statistically significant variable of the process. Maximum methyl chavicol concentration was obtained using evaporator temperature at 70 degrees C. (C) 2011 Elsevier B.V. All rights reserved.877178Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES

Sunflower enzymatic reaction optimization: MAG and DAG formation / Otimização da reação enzimática do girassol: formação de MAG e DAG

Monoacylglycerols (MAG) and diacylglycerols (DAG) are emulsifiers widely used in food and cosmetic industries. Typical industrial processes for MAG and DAG production consist of the catalytic glycerolysis of triacylglycerols at high temperatures (>200°C). However, the inorganic catalyst and the high temperature contribute to the formation of a product often dark and with unpleasant smell. The goal of this work is the use of enzymatic glycerolysis to improve product aspect and quality, increase selectivity and decrease energy consumption. This reaction produces a mixture of approximately 20% of MAG and 50% of DAG. In order to evaluate the effects of reaction parameters in the MAG and DAG content after the enzymatic glycerolysis reactions of refined sunflower oil a 23 experimental design was employed. A surface response analysis was used to optimize this process

Enrichment of oxyterpenes from orange oil by short path evaporation

The developing of processes to perform orange oil deterpenation is an important operation to guarantee the industrial application of this material. By not using organic solvents, presenting a small residence time, and operating at low pressures, short path evaporation is an alternative to deterpenate orange oil. However, the determination of its suitable operating conditions is not trivial. Therefore, in this work, the variables: evaporator temperature, condenser temperature, and feed flow rate, were studied aiming to determine the best orange oil deterpenation operating conditions by short path evaporation. in the range of study, the product obtained at 1.33 kPa, using evaporator temperature of 82.5 degrees C, condenser temperature of 0 degrees C, and feed flow rate of 10.5 ml/min presented the richest oxygenated fraction due to removing more than 95% of limonene initial content. the concentration of linalool and decanal, oxygenates representatives, were respectively 4.5 and 13 times higher than the initial raw material concentration. (c) 2013 Elsevier B.V. All rights reserved.Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Coordenação de Aperfeiçoamento de Pessoal de Nível Superior (CAPES)Universidade Federal de São Paulo UNIFESP, Dept Ciencias Exatas & Terra, BR-09972270 Diadema, SP, BrazilUniv Campinas UNICAMP, Sch Chem Engn, BR-13083970 Campinas, SP, BrazilUniversidade Federal de São Paulo UNIFESP, Dept Ciencias Exatas & Terra, BR-09972270 Diadema, SP, BrazilWeb of Scienc