PRODUCTION OF MONOGLYCERIDES AND DIGLYCERIDES THROUGH LIPASE-CATALYZED GLYCEROLYSIS AND MOLECULAR DISTILLATION.

PRODUCTION OF MONOGLYCERIDES AND DIGLYCERIDES THROUGH LIPASE-CATALYZED GLYCEROLYSIS AND MOLECULAR DISTILLATION. Monoacilglycerides and diacilglycerides are produced through lipase-catalyzed glycerolysis of soybean oil using Candida antarctica B in a solvent-free system. The reaction was carried Out at a glycerol to triacylglycerol molar ratio of 8:1 with 2% of lipase. Acylglycerides, free fatty acids (FFA) and glycerol produced were separated employing the molecular distillation process. Starting from a product of enzymatic reaction 25.06% of triacylglycerols, 46.63% of diacylglycerides. 21.72% of monoacylglycerides, 5.38% of FFA and 1.21% of glycerol and after consecutively distillations. monoacylglycerides with 80% of purity was obtained and also oil with 54% of diacylglycerides to be used in human dietary.3261539154

Response surface methodology applied to optimization of distilled monoglycerides production

This work demonstrates that response surface methodology (RSM) is a powerful tool for the optimization of the production of distilled MG. Experiments with a centrifugal molecular distillator having an evaporation area of 0.0046 m(2) were carried out using RSM to identify operating conditions that can lead to higher MG purity. The independent variables studied were the evaporator temperature (TEV) and the volumetric feed flow rate (Q). The experimental range was from 100 to 300 degrees C for TEV and between 5 and 15 mL/min for Q. High-performance size exclusion chromatography was used to evaluate TG, DG, MG, FFA, and glycerol (GL) compositions. Results were presented as MG concentration surfaces. Starting from a material with 10.8% of TG, 37.7% of DG, 43.6% of MG, and 7.2% of GL, the maximum MG purity in the distillate stream with just one distillation step was 82.6% at a TEV equal to 250 degrees C and Q equal to 5 mL/min. At these conditions, the MG recovery was 61%. A strategy was developed to obtain distilled MG with 96.3% purity.82967367

Free fatty acid separation from vegetable oil deodorizer distillate using molecular distillation process

Distillates of the vegetable oil deodorization are composed of free fatty acids (FFA), sterols, tocopherols, sterol esters, hydrocarbons and breakdown products of fatty acids, aldehydes, ketones and acylglycerols. The content of free fatty acids in deodorizer distillates varies between 25 and 75%. Due to its high content, free fatty acid separation from deodorizer distillate is an important step to concentrate tocopherols to high purity. Tocopherols are valuable natural substances used in food, cosmetic and pharmaceutical industries. In this work, separation of free fatty acids from soybean oil deodorizer distillate (SODD) was investigated through molecular distillation, using different operating conditions. Evaporator temperature from 100 to 180 degrees C and feed flow rate in the range of 1.5-23.0 g min(-1) were used in the experiments. FFA and tocopherols contents were monitored in each stream generated by the molecular distillation process (distillate and residue streams). The intention is to determine the best operating conditions to produce a material with minimum FFA content and to minimize tocopherol losses during the process. Removal of FFA in the distillate stream resulted in a preliminary concentration of tocopherols, which is removed in the residue stream of the molecular distillation. The results showed that an efficient FFA separation from SODD with the lowest loss of tocopherols requires specific operating conditions. It was possible to obtain a material with 6.4% of FFA and 18.3% of tocopherols from a raw material composed by 57.8% of FFA and 8.97% of tocopherols, using 160 degrees C of evaporator temperature and 10.4 g min(-1) of feed flow rate. These results represent FFA elimination of 96.16% and tocopherol recovery of 81.23%. (C) 2005 Elsevier B.V. All rights reserved.481788

Optimization of distilled monoglycerides production

Monoglycerides (MG) are emulsifiers widely used in food and pharmaceutical industries. Current industrial processes for MG production consist of the interesterification of triglycerides with glycerol (GL), in the presence of inorganic catalysts at high temperatures (> 200 degrees C). This reaction is known as glycerolysis and produces a mixture of approx 50% of MG. This level of concentration is suitable for many applications, although, for some specific uses like margarine, shortening, icing, and cream filling, require distilled MGs, which are purified MG (min. 90%) obtained by the molecular distillation process. Therefore, in this work, a 2(3) factorial design was employed to evaluate the effects of reaction parameters in the MG content after the interesterification reaction of refined soybean oil with GL in the presence of sodium hydroxide as catalyst. After that, the MG content in the reaction product was enhanced through the molecular distillation process in order to obtain distilled MG.1314169968069

Comparison of two different strategies for tocopherols enrichment using a molecular distillation process

The objective of this study is to compare two different strategies for enriching tocopherols in soybean oil deodorizer distillate (SODD) using a molecular distillation process. The first strategy is to submit crude SODD to a sequence of molecular distillations using different temperatures without any preparation of the raw material. The second strategy is to modify chemically the raw material and submit it to a sequence of distillations. In SODD chemical modification, acylglycerol species are converted into free fatty acids (FFAs) and glycerol through a saponification reaction at 65 degrees C followed by an acidulation step. Crude and chemically modified SODD were submitted to five stages of molecular distillation to evaluate and compare the performance of both sequences of distillations. It was observed that the enrichment of tocopherols was 4.1 and 5.8 times higher than the original feed concentration for crude and chemically modified SODD, respectively.45275375

Natural compounds obtained through centrifugal molecular distillation

Soybean oil deodorized distillate (SODD) is a byproduct from refining edible soybean oil; however, the deodorization process removes unsaponifiable materials, such as sterols and tocopherols. Tocopherols are highly added value materials. Molecular distillation has large potential to be used in order to concentrate tocopherols, because it uses very low levels of temperatures because of the high vacuum and short operating time for separation and, also, it does not use solvents. However, nowadays, the conventional way to recover tocopherols is carrying out chemical reactions prior to molecular distillation, making the process not so suitable to deal with natural products. The purpose of this work is to use only molecular distillation in order to recover tocopherols from SODD. Experiments were performed in the range of 140-220 degrees C. The feed flow rate varied from 5 to 15 g/min. The objective of this study was to remove the maximum amount of free fatty acids (FFA) and, so, to increase the tocopherol concentration without add any extra component to the system. The percentage of FFA in the distillate stream of the molecular still is larger at low feed flow rates and low evaporator temperatures, avoiding thermal decomposition effects.1314169971672

Biodiesel Production from Integration Between Reaction and Separation System: Reactive Distillation Process

Biodiesel is a clean burning fuel derived from a renewable feedstock such as vegetable oil or animal fat. It is biodegradable, non-inflammable, non-toxic, and produces lesser carbon monoxide, sulfur dioxide, and unburned hydrocarbons than petroleum-based fuel. The purpose of the present work is to present an efficient process using reactive distillation columns applied to biodiesel production. Reactive distillation is the simultaneous implementation of reaction and separation within a single unit of column. Nowadays, it is appropriately called "Intensified Process". This combined operation is especially suited for the chemical reaction limited by equilibrium constraints, since one or more of the products of the reaction are continuously separated from the reactants. This work presents the biodiesel production from soybean oil and bioethanol by reactive distillation. Different variables affect the conventional biodiesel production process such as: catalyst concentration, reaction temperature, level of agitation, ethanol/soybean oil molar ratio, reaction time, and raw material type. In this study, the experimental design was used to optimize the following process variables: the catalyst concentration (from 0.5 wt.% to 1.5 wt.%), the ethanol/soybean oil molar ratio (from 3:1 to 9:1). The reactive column reflux rate was 83 ml/min, and the reaction time was 6 min.1614185224525

Optimization of biodiesel production from castor oil

The transesterification of castor oil with ethanol in the presence of sodium ethoxide as catalyst is an exceptional option for the Brazilian biodiesel production, because the castor nut is quite available in the country. Chemically, its oil contains about 90% of ricinoleic acid that gives to the oil some beneficial characteristics such as its alcohol solubility at 30 C. The transesterification variables studied in this work were reaction temperature, catalyst concentration and alcohol oil molar ratio. Through a star configuration experimental design with central points, this study shows that it is possible to achieve the same conversion of esters carrying out the transesterification reaction with a smaller alcohol quantity, and a new methodology was developed to obtain high purity biodiesel.1304169940541

Short-Path-Distillation Process of Lemongrass Essential Oil: Physicochemical Characterization and Assessment Quality of the Distillate and the Residue Products

Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Short-path distillation (SPD), a special high-tech thermal separation technique operating at high vacuum, was used in order to increase the citral concentration in lemongrass essential oil, without adding any extra components to the system, causing minimal thermal impact and reaching high quality for the essential oil extracted at the distillate stream. Experiments were carried out using a centrifugal molecular distillation unit with an evaporator temperature (EVT) from 60 to 120 degrees C and a feed flow rate (Q) from 1.5 to 4.5 mL . min(-1). Experimental protocols for oil and fat analysis were used to characterize the materials extracted. Results (obtained using GC-MS) showed that bSPD was successful in the separation and purification of essential oil. High-quality essential oil was confirmed because of citral concentration increases from 19.816 mg(citral) . mL(-1) (initial sample) to 40.963 mg(citral) . mL(-1) (at 120 degrees C and 4.5 mL . min(-1)), reaching a concentration of the bioactive compound (citral) in the distillate stream of 2.1 times the concentration in the original sample. The density, dynamic viscosity, and free fatty acids were 0.901 g . cm(-3), 2.069 mPa.s(-1), and 1.26 wt % (oleic acid), respectively, satisfying the oil quality criterion and avoiding thermal degradation.501381858194Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)Fundação de Amparo à Pesquisa do Estado de São Paulo (FAPESP)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq

Kinetic study on catalytic cracking of Brazilian high-boiling-point petroleum fractions

Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)This work proposed a technique to estimate the kinetic parameters of cracking reaction. High-boiling-point petroleum fractions (> 623.15 K) were analyzed. The experiments were performed using a thermal analysis system with a differential scanning calorimetry module at different linear heating rates (15, 20, 25, and 30 K min(-1)) in the temperature range from 303.15 to 823.15 K. The Arrhenius, Kissinger, and Flynn-Ozawa-Wall methods were used to determine the kinetic parameters. The compensation effect and the dependence on the activation energy of the conversion degree were evaluated. The catalyst used was a typical FCC regenerated catalyst containing 48.3 mass% of alumina, and particle size of 67 mu m. The effect of catalyst loading was studied using 3, 5, and 10 mass%. Analysis of the DSC curves showed a major transitional stage between 693.15 and 723.15 K, identified as an endothermic region of high temperature oxidation (HTO). Empirical kinetic models were produced and data were obtained from the kinetic analysis of the HTO region. Under non-isothermal heating conditions higher activation energies were found as the API gravity of the high-boiling-point petroleum fraction decreased. On the other hand, the results showed consistent effects for the dependence of the activation energy on the extent of cracking conversion under non-isothermal conditions, showing a decrease with the extent of conversion. The catalytic loading effect is remarkable, and provides an alternative route for the cracking with lower activation energy with increasing catalyst weight. The kinetic parameters formulated will be used in the mathematical modeling of the reactive molecular distillation process for upgrading high-boiling-point petroleum fractions.110312671281Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq)National Plan for the Science and Technology of Petroleum and Natural Gas (CTPETRO)Conselho Nacional de Desenvolvimento Científico e Tecnológico (CNPq