EDTI Process Improvement

Brazil

EDTI Process Improvement

Brazil

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Carvalho P.I.N.,University of Campinas | Osorio-Tobon J.F.,University of Campinas | Rostagno M.A.,University of Campinas | Petenate A.J.,EDTI Process Improvement | Meireles M.A.A.,University of Campinas
Journal of Supercritical Fluids | Year: 2015

Extracting volatile compounds using supercritical carbon dioxide (scCO2) is one of the most interesting applications of supercritical technology because of the high solubility of these substances in CO2. Supercritical carbon dioxide extraction (SFE) has been applied for obtaining extracts from several vegetable matrices, including turmeric (Curcuma longa L.), due to its valuable volatile oil. However, a techno-economic evaluation of turmeric oil and ar-turmerone extraction has not yet been performed. Therefore, the effects of temperature, pressure and process time on the extract yield, relative ar-turmerone yield and manufacturing cost were evaluated in this work. Turmeric rhizomes were ground, sieved and placed in contact with scCO2 flowing at 8.4×10-3 kg/min in a laboratory scale SFE unit. Major compounds in the extracts were identified and quantified by gas chromatography. The manufacturing cost (COM) of the extracts was estimated using a model cost developed in the simulator SuperPro Designer 8.5®. Using SFE led to high yields of extract and ar-turmerone. Fast extraction combined with relatively low solvent consumption were observed. Yields of 6.4% and 1.02% of extract and ar-turmerone, respectively, were obtained at 333K and 25MPa for a solvent mass to feed mass ratio of 1.31. For these conditions, the lowest manufacturing cost (COM=US$ 178.8/kg extract) was estimated for a unit containing two 0.005-m3 extractors. © 2015 Elsevier B.V.


Zabot G.L.,University of Campinas | Moraes M.N.,University of Campinas | Petenate A.J.,EDTI Process Improvement | Meireles M.A.A.,University of Campinas
Journal of Supercritical Fluids | Year: 2014

There is a need for scientific research that evaluates the influence of important process variables on the scale up of supercritical technology. For supercritical fluid extraction (SFE), one of these variables is the extractor's bed geometry, which can be defined by the ratio of the bed height (HB) to the bed diameter (DB). A systematic study is needed to select suitable criteria that can be used to obtain similar extraction curves among beds with different geometries. In this study, maintaining a constant ratio of solvent mass to feed mass for two beds with 1-L volumes but different geometries (E-1: HB/DB = 7.1; E-2: HB/DB = 2.7) was confirmed as a successful scale up criterion. For constant values of the temperature, pressure and bed porosity, there is experimental evidence that the mass transfer rate is equal in the two beds when the solvent flow rate is high. When 0.6 kg of clove buds was packed in the beds, the extraction rates were 2.10 ± 0.08 and 2.3 ± 0.1 g extract/min for beds E-1 and E-2, respectively. However, when the solvent flow rate was lower, the extraction rates were 0.93 ± 0.06 and 1.12 ± 0.02 g extract/min for beds E-1 and E-2, respectively. This difference in behavior between the extraction beds is associated with the axial dispersion of the fluid, which is more pronounced when the HB/DB ratio is increased. Thin particles tend to compact in the beds with high HB/DB ratios, which shorten the solvent passage. Non-isothermal profiles and differences in chemical composition of the extracts were also observed: 17% more α-humulene and 9% more eugenol were extracted in E-1 and E-2, respectively. ©2014 Elsevier B.V. All rights reserved.


Osorio-Tobon J.F.,University of Campinas | Carvalho P.I.N.,University of Campinas | Rostagno M.A.,University of Campinas | Petenate A.J.,EDTI Process Improvement | Meireles M.A.A.,University of Campinas
Journal of Supercritical Fluids | Year: 2014

Pressurized liquid extraction (PLE) of curcuminoids from deflavored turmeric rhizomes was optimized. The rhizomes were initially deflavored by extraction with supercritical CO2. Immediately after SFE, PLE process was performed using ethanol as the solvent and a static extraction time of 20 min, and the independent variables were the temperature (333-353 K) and pressure (10-35 MPa). The results indicate that the optimum extraction temperature and pressure were 333 K and 10 MPa, respectively. PLE required three and six times less extraction time than low-pressure solvent extraction and Soxhlet extraction, respectively, to produce similar extraction yields. The cost of manufacturing (COM) decreased from US$ 94.92 kg-1 to US$ 88.26 kg-1 when the capacity of the two-extractor system increased from 0.05 m3 to 0.5 m3 and from US$ 94.92 kg-1 to US$ 17.86 kg-1 when the cost of the raw materials decreased from US$ 7.91 kg-1 to US$ 0.85 kg-1 for a two 0.05 m3 extractor system. © 2014 Elsevier B.V. All rights reserved.


Osorio-Tobon J.F.,University of Campinas | Carvalho P.I.N.,University of Campinas | Rostagno M.A.,University of Campinas | Petenate A.J.,EDTI Process Improvement | Meireles M.A.A.,University of Campinas
Journal of Supercritical Fluids | Year: 2016

This study examined the precipitation of curcuminoids from an ethanolic extract using a supercritical antisolvent process (SAS). The ethanolic extract was obtained from deflavored turmeric using pressurized liquid extraction (PLE). A Split-Plot experimental design was used to evaluate the effects of process parameters, such as nozzle type (T-mixer and coaxial), temperature (313 and 333 K), pressure (10 and 12 MPa) and CO2 flow (500 and 800 g/h), on the curcuminoids precipitation process. The results indicate that the T-mixer nozzle obtained a higher yield and a lower particle size than the coaxial nozzle. Particles of curcuminoids were precipitated with a global yield of solids of 69% and a curcuminoid content of 554 mg/g. This corresponds to a precipitation efficiency of 97%. The particles precipitated via SAS contained a curcuminoid content 2 and 31 times higher than the extracts obtained by rotary evaporation and the ethanolic extract, respectively, obtained by PLE. Depending on experimental conditions, the particles were characterized as polydispersed and agglomerated into larger structures (by up to 100 μm) with different morphologies. © 2015 Elsevier B.V. All rights reserved.


Rodrigues L.M.,University of Campinas | Alcazar-Alay S.C.,University of Campinas | Petenate A.J.,EDTI Process Improvement | Meireles M.A.A.,University of Campinas
Comptes Rendus Chimie | Year: 2014

Bixin is the major carotenoid in the seed of the Annatto plant (Bixa orellana L.). The aim of this study was to obtain extracts containing bixin from seeds that had been partially defatted by supercritical fluid extraction. Pressurized liquid extraction (PLE) and low-pressure solvent extraction (LPSE) methods were used, and the effects of the solvent, temperature, pressure, solvent mass to feed mass (S/F) ratio and ultrasonication were evaluated for the global yield (X0(%)) and the bixin yield (BY(%)). Extraction conditions producing high yields of bixin were established for both the PLE and LPSE methods. Analysis of variance was used to examine the influence of the individual extraction variables in LPSE and PLE. For LPSE; significant effects were found for solvent, temperature, and the interactions of temperature with solvent and temperature with S/F. Solvent was the only variable that significantly affected X0(%) and BY(%), for PLE. While ultrasonication did not significantly affect X0(%) or BY(%), scanning electron microscopy analysis revealed structural changes in the vegetal matrix following this treatment. © 2013 Académie des sciences.

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