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We report a mathematical model of the supercritical fluid foaming (SCF) from the poly(e-caprolactone) (PCL) + CO2 system based on the Laws of Conservation of Momentum and Conservation of Mass. The ...

Supercritical fluid extraction assisted by cold pressing (SFEAP) is presented for obtaining volatile oil from clove buds at 150 bar, 40 °C, and using two torques (40 and 80 N.m). As the best condition, SFEAP with 40 N.m provided an oil yield of 22.19 g/100 g buds containing Eugenol (57.7 wt.%), Eugenyl Acetate (12.6 wt.%), β-caryophyllene (8.3 wt.%), and α-humulene (0.9 wt.%). This paper also presented, for the first time, the economic evaluation of using SFEAP instead of SFE. In the economic approach, 24 scenarios were tested in the terms of cost of manufacturing (COM), which consisted of evaluating the scale of the plant, capital financing, purchasing cost of clove, solvent to feed mass ratio and the extraction techniques. The best scenario indicated a COM of only US$ 13.42/kg oil, whereas approximately 87% of the COM is dependent on the purchase cost of clove and other materials.

Supercritical fluid extraction assisted by pressing (SFEAP) and supercritical fluid extraction (SFE) were compared in terms of extraction kinetics and extract fractionation using fennel. Extraction was performed at a pressure of 200 bar, a temperature of 40 °C, and a solvent-to-feed ratio of 95, using torques of 0, 40, and 70 N m. The overall extraction yield increased by 24.5%, from 9.8 g extract/100 g fennel for SFE to 12.2 g extract/100 g fennel for SFEAP with a torque meter reading of 40 N m, while overall extraction yield increased by only 2.5% after increasing the torque from 40 N m to 70 N m. In the second part of this study, fennel oils extracted with SFE and SFEAP were successfully fractionated into fatty oil rich product and essential oil rich product using two serial, equal-sized separators.

The present study evaluated the effect of supercritical fluid extraction (SFE) assisted by cold pressing (SFEAP) on the overall yield, extraction kinetics, composition of baru seed oil and manufacturing cost (COM). The best extraction conditions were determined in extraction assays combining different pressures (150–350 bar) and temperatures (35 and 45 °C). The extraction yield by SFEAP (28.6 g oil/100 g baru seed) was approximately 31% higher than that obtained by SFE (21.9 g oil/100 g baru seed), according to the kinetic study with the best extraction conditions (350 bar and 45 °C). The extraction yield observed under this condition allowed us to obtain a lower COM for both techniques (SFE was US$ 118.32/kg baru oil and SFEAP was US$ 87.03/kg baru oil) compared to lower pressures and temperatures. The oil obtained under all extraction conditions was rich in unsaturated fatty acids and other bioactive compounds. The extraction of baru seed oil by SFEAP resulted in a higher yield and lower manufacturing cost than SFE., Economic evaluation; Supercritical fluid extraction assisted by pressing; baru seed oil; supercritical CO2.

Supercritical CO2 extraction of sucupira branca (SB) seeds was studied under different conditions of pressure (20-40 MPa) and temperature (40 and 60°C). Operational conditions were assessed on laboratory and pilot scales, and their influences on manufacturing cost (COM) and productivity were discussed. At 40°C and 30 MPa for 65 min, 40 g oil/100 g SB seeds were obtained. In the economic and technical approaches, a plant with two extractors (2×15 L) is more convenient to implement than a plant with one extractor (1×30 L), obtaining a COM of 49.21 US$/kg SB oil and productivity of 20,083 kg oil/year. This COM and productivity were reached at the kinetic point where the S/F was 13.5 g CO2/g SB seeds. In this period, the mass transfer is controlled by diffusion and convection (FER period). The oil obtained under these conditions presented phytochemicals, such as alpha-humulene, beta-caryophyllene, alpha-copaene, (-)-beta-elemene, (E)-germacrene D(-)-gamma-elemene, and spathulenol.

This paper presents the techno-economic influence of grinding time (GT) (10 s–90 s) and CO2 flow rate (FR) (1.08 × 10−4–2.17 × 10−4 kg/s) on the supercritical fluid extraction (SFE) performance of oil from pequi (Caryocar brasiliense) under 60 °C and 40 MPa. Then, in the economic approach, the best extraction curves were described in terms of Cost of Manufacturing (COM) in the laboratory scale for each combination of GT and FR for selecting the suitable mass to feed mass ratio (S/F) that yielded the lowest COM and the highest productivity. Thereafter, with this S/F, eight scenarios were tested in pilot (100 L) and industrial (500 L) scales with CO2 recycle, which included the purchase cost of pequi and acquisition cost of equipment. Within these eight scenarios tested, the most promising one indicated a COM of only US$ 37.03/kg pequi oil, whereas approximately 85% of the COM is dependent on the purchase cost of pequi and other raw materials (e. g., CO2).

Introduction: The effects of the grinding procedure on the supercritical fluid extraction (SFE) yields of eugenol, β-caryophyllene, α-humulene, and eugenyl acetate from clove are discussed in detail in this paper. Methods: For this purpose, five grinding procedures were employed: 1) continuous 1-min grinding, 2) continuous 2-min grinding, 3) two 1-min grinding periods with 6-min stop in between 4) continuous 4-min grinding, and 5) four 1-min grinding periods with 6-min stops in between. After that, the extractor was filled with 12 g of milled clove obtained using one of the grinding procedures while the other SFE parameters were kept constant (pressure of 150 bar, temperature of 40 °C, supercritical CO2 flow rate of 1.03×10−4 kg/s, static time of 20 min, and dynamic extraction time of 15 min). Then, the composition of the extract was evaluated by gas chromatography (GC). Conclusion: It was found that the grinding procedure has considerable effects on the recoveries of eugenol, β-caryophyllene, α-humulene, and eugenyl acetate from clove, and employing four 1-min grinding periods with 6-min stops in between as the grinding procedure gave the highest content of the aforementioned components in the extract.

Extraction processes that employ supercritical fluid technology has been extensively applied for the obtaining of high-quality extracts from turmeric rhizomes. Nevertheless, these processes generate high quantities of wastes, which are potential sources of antioxidant constituents and carbohydrates. In this work, mixed biopolymers composed of starch and curcuminoids were recovered from supercritical fluid and pressurized liquid extraction processes. The quality of these materials was investigated in terms of experimental and economic approaches. The application of supercritical fluid and pressurized liquid extraction resulted on products with relevant quality in terms of curcuminoids and modified polymer matrix, which can attribute inclusion in industry as a colorant agent, and in human diet as a resistant starch source. Economic evaluation reports that recovery of biopolymers from turmeric wastes is a feasible alternative considering 80% yield and capacities of 50 L and 500 L.

The effects of several operational parameters (pressure, temperature, CO2 flow rate, solution flow rate, injector type, and concentration of solute in the ethanol solution) during Supercritical AntiSolvent (SAS) precipitation process on the energy consumption cost per unit of manufactured product were investigated using experimental design technique. In this work, two different injectors were used. A completely randomized experiment would eventually require a modification of the apparatus after each experimental run. To avoid this, the experimental runs were done accordingly with a split-plot experimental design. For this study, Ibuprofen sodium salt was used as a model solute, ethanol was used as solvent, and CO2 was used as antisolvent. This supercritical fluid-based has been used successfully for several food and pharmaceutical applications since the production of small micro- and nanometer-sized particles have attracted growing interest in these industries. Focusing on energy saving, an SAS precipitation process was simulated using the SuperPro Designer simulation platform. The effect of temperature versus concentration of ethanolic solution and pressure versus solution flow rate interactions on the energy consumption cost per unit of manufactured product was demonstrated. The lowest estimated energy cost per unit of manufactured product was obtained using an ethanolic solution of 0.04 g mL−1 at 12 MPa of pressure and a solution flow rate of 1 mL min−1. This result was independent of the temperature. Thus, the present work reports a systematic energetic-economic study of the supercritical antisolvent micronization process, aiming increase knowledge about this process and its further incorporation by the food and pharmaceutical industries.

This work consists of the steps for the assembly of a Supercritical Antisolvent Precipitation laboratory equipment and evaluation of the parts acquisition costs. A flow diagram with all components was developed, a complete list of all necessary components was presented, and an estimate of the acquisition of these parts in Brazil was reported. The stages of construction along with the importance of each component in the equipment were discussed. An equipment designs were presented as a result of the current work that serve as a basis for consulting future work on the development of new equipment.

A supercritical particle formation equipment, designed and constructed by our research group, was validated in this study using supercritical CO2 as an antisolvent. Ibuprofen sodium salt was successfully micronized by supercritical antisolvent (SAS) precipitation. Ethanol and CO2 was used as solvent and antisolvent, respectively, and the effect of the operating conditions on the precipitation yield, residual organic solvent content and particle morphology were evaluated using a split-plot experimental design and the analysis of variance (ANOVA) method. This study showed that when selecting appropriate process conditions, it is possible to produce a sheet-like morphology, which is the best for tableting purposes, with high precipitation yield (70%) and low residual solvent content (4.7 mg kg−1).

Efficient encapsulation techniques and development of special delivery systems enhance the stability of target compounds, enabling their processing and application. Supercritical fluid extraction of emulsions (SFEE) is a promising alternative to process natural target compounds, due to its suitability to encapsulate poorly water-soluble compounds in an aqueous suspension, providing products with controlled particle size, stability and without toxicity. This chapter provides technological aspects and recent data (2016–2018) on the application of SFEE delivery systems to encapsulate compounds of great interest to the food and non-food industry.

High Turbulence Extraction Assisted by Ultrasound combined with Supercritical Antisolvent Fractionation (SAF) was done to intensify the recovery of bixin and phenolic compounds from semi-defatted annatto seeds. Annatto seeds are extensively used due to its colorant properties and bioactive potential in human health. Modifications were performed in the SAF experimental apparatus in order to prevent losses of product. Results show that supercritical fractionation resulted in particle yields between 72.2–80.5%, 20–50% phenolics, and 66% bixin.

Surfactants are widely used in the food industry to form and stabilize emulsion-based food and beverage products. The use of natural surfactant to replace the synthetic ones is a recent demand in industries. In this work, first it was evaluated the influence of hydrostatic pressure levels (up to 10 bars applying nitrogen), oily phase type and surfactant type. In addition, we propose a novel surfactant for the formulation of emulsions constituted of concentration of saponin-enriched extract. The extract containing saponins was obtained from pressurized hot water extraction of Brazilian Ginseng (Pfaffia glomerata) roots. The emulsions containing saponin extract were used for further processing by Supercritical Fluid Extraction of Emulsions (SFEE), using an oily bixin-rich extract from annatto seeds (Bixa orellana L.) as core material (extracting solution from hot ethyl acetate pressurized extraction). Since, the final product of SFEE achieved a low residual ethyl acetate concentration (9.4 ppm). Regarding droplet size similar results were obtained for the emulsion (549 nm) and the produced suspension (569 nm), which were 24.74% lower than the droplet size obtained in process not assisted with pressurized nitrogen atmosphere (730 nm). This work proposed the use of this alternative biosurfactant and the process that we named Ultrasound Emulsification Assisted by Nitrogen Hydrostatic Pressure (UEANHP), during the emulsification preparation step of the SFEE process.

Phytochemicals extracted from natural sources are widely studied for many applications, including the prevention of diseases and functional foods. In this context, passion fruit by-products (PFBP) can play an important role in obtaining these compounds. This work aimed to concentrate PFBP extracts from supercritical fluid extraction (SFE) (fixed at 40 °C and 35 MPa) in δ-tocotrienol, β/γ-tocotrienol, squalene, and carotenoids using a homemade fractionation system with two separator vessels. Integrated extraction and fractionation (SFE-SFF) were performed at 17−25 MPa and 50−80 °C. An economic evaluation simulated a pilot-scale process, resulting in a cost of US$ 277–384/kg extract for the most concentrated fraction (F2). Two SFE-SFF conditions were able to concentrate squalene in about 5.2 times in the last fraction of the process (F3). In contrast, the proposed integrated process did not seem promising to concentrate carotenoids, thus other fractionation methods should be investigated.

The effect of grinding time (GT) from 15 s to 20 min on the dynamic yield of supercritical fluid extraction (SFE(from fennel was investigated. The extractor was subjected to a pressure of 200 bar, a temperature of 313 K, and a supercritical CO2 flow rate of 2.0 × 10−4 kg/s over 80 min. It was found that the overall SFE yield was increased from 6.4 g/100 g fennel when GT = 15 s to 9.8 g/100 g fennel when GT =6 min, while it changed by only 1.5 g/100 g fennel after increasing GT from 6 min to 20 min. The process was then modeled based on the mass conservation law, and the model was solved using Galerkin’s method on finite element method (FEM). It was demonstrated that considering the whole bed as one single element can acceptably solve the PDEs and reduces the computation cost significantly.

The present work describes setting up a laboratory unit for supercritical fluid extraction. In addition to its construction, a survey of cost was done to compare the cost of the homemade unit with that of commercial units. The equipment was validated using an extraction of annatto seeds’ oil, and the extraction and fractionation of fennel oil were used to validate the two separators; for both systems, the solvent was carbon dioxide. The chemical profiles of annatto and fennel extracts were assessed using thin layer chromatography; the images of the chromatographic plates were processed using the free ImageJ software. The cost survey showed that the homemade equipment has a very low cost (~US$ 16,000) compared to commercial equipment. The extraction curves of annatto were similar to those obtained in the literature (yield of 3.8% oil). The separators were validated, producing both a 2.5% fraction of fennel seed extract rich in essential oils and another extract fraction composed mainly of oleoresins. The ImageJ software proved to be a low-cost tool for obtaining an initial evaluation of the chemical profile of the extracts.