Search results for: supercritical condition

Authors: Aarti Singh, Anees Ahmad

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Essential oil was extracted from lemon grass (Cymbopogon martini) with supercritical carbondioxide (SC-CO2) at pressure of 140 bar and temperature of 55 °C and CO2 flow rate of 8 gmin-1, and its composition and yield were compared with other conventional extraction methods of oil, HD (Hydrodistillation), SE (Solvent Extraction), UAE (Ultrasound Assisted Extraction). SC-CO2 extraction is a green and sustainable extraction technique. Each oil was analysed by GC-MS, the major constituents were neral (44%), Z-citral (43%), geranial (27%), caryophyllene (4.6%) and linalool (1%). The essential oil of lemon grass is valued for its neral and citral concentration. The oil obtained by supercritical carbon-dioxide extraction contained maximum concentration of neral (55.05%) whereas ultrasonication extracted oil contained minimum content (5.24%) and it was absent in solvent extracted oil. The antioxidant properties have been assessed by DPPH and superoxide scavenging methods.

Keywords: cymbopogon martini, essential oil, FT-IR, GC-MS, HPTLC, SC-CO2

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Authors: Yousef Bakhbakhi

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Crystallization with supercritical fluids (SCFs), as a developed technology to produce particles of micron and sub-micron size with narrow size distribution, has found appreciable importance as an environmentally friendly technology. Particle synthesis using SCFs can be achieved employing a number of special processes involving solvent and antisolvent mechanisms. In this study, the compressed antisolvent (PCA) process is utilized as a model to analyze the theoretical complexity of crystallization with supercritical fluids. The population balance approach has proven to be an effectual technique to simulate and predict the particle size and size distribution. The nucleation and growth mechanisms of the particles formation in the PCA process is investigated using the population balance equation, which describes the evolution of the particle through coalescence and breakup levels with time. The employed mathematical population balance model contains a set of the partial differential equation with algebraic constraints, which demands a rigorous numerical approach. The combined Collocation and Galerkin finite element method are proposed as a high-resolution technique to solve the dynamics of the PCA process.

Keywords: particle formation, particle size and size distribution, PCA, supercritical carbon dioxide

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Authors: Norsyamimi Hassim, Masturah Markom

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Supercritical fluid extraction (SFE) has been known as a sustainable and safe extraction technique for plant extraction due to the minimal usage of organic solvent. In this study, a scale-up process for the selected herbal plant (Phyllanthus niruri) was investigated by using supercritical carbon dioxide (SC-CO2) with food-grade (ethanol-water) cosolvent. The quantification of excess ethanol content in the final dry extracts was conducted to determine the safety of enriched extracts. The extraction yields obtained by scale-up SFE unit were not much different compared to the predicted extraction yields with an error of 2.92%. For component contents, the scale-up extracts showed comparable quality with laboratory-scale experiments. The final dry extract showed that the excess ethanol content was 1.56% g/g extract. The fish embryo toxicity test (FETT) on the zebrafish embryos showed no toxicity effects by the extract, where the LD50 value was found to be 505.71 µg/mL. Thus, it has been proven that SFE with food-grade cosolvent is a safe extraction technique for the production of bioactive compounds from P. niruri.

Keywords: scale-up, supercritical fluid extraction, enriched extract, toxicity, ethanol content

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Authors: Chun-Ying Lee, Kun-Hsien Lee, Bor-Wei Wang

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The process of post-supercritical CO₂ electroplating uses the electrolyte solution after being mixed with supercritical CO₂ and released to atmospheric pressure. It utilizes the microbubbles that form when oversaturated CO₂ in the electrolyte returns to gaseous state, which gives the similar effect of pulsed electroplating. Under atmospheric pressure, the CO₂ bubbles gradually diffuse. Therefore, the introduction of ultrasound and/or other agitation can potentially excite the CO₂ microbubbles to achieve an electroplated surface of even higher quality. In this study, during the electroplating process, three different modes of agitation: magnetic stirrer agitation, ultrasonic agitation and a combined mode (magnetic + ultrasonic) were applied, respectively, in order to obtain an optimal surface morphology and mechanical properties for the electroplated Ni coating. It is found that the combined agitation mode at a current density of 40 A/dm² achieved the smallest grain size, lower surface roughness, and produced an electroplated Ni layer that achieved hardness of 320 HV, much higher when compared with conventional method, which were usually in the range of 160 to 300 HV. However, at the same time, the electroplating with combined agitation developed a higher internal stress of 320 MPa due to the lower current efficiency of the process and finer grain in the coating. Moreover, a new control methodology for tailoring the coating’s mechanical property through its thickness was demonstrated by the timely introduction of ultrasonic agitation during the electroplating process with post supercritical CO₂ mixed electrolyte.

Keywords: nickel electroplating, micro-bubbles, supercritical carbon dioxide, ultrasonic agitation

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Authors: Shyh Ming Chern

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Cubic equations of state (EoS), popular due to their simple mathematical form, ease of use, semi-theoretical nature and, reasonable accuracy are normally fitted to vapor-liquid equilibrium P-v-T data. As a result, They often show poor accuracy in the region near and above the critical point. In this study, the performance of the renowned Peng-Robinson (PR) and Patel-Teja (PT) EoS’s around the critical area has been examined against the P-v-T data of water. Both of them display large deviations at critical point. For instance, PR-EoS exhibits discrepancies as high as 47% for the specific volume, 28% for the enthalpy departure and 43% for the entropy departure at critical point. It is shown that incorporating P-v-T data of the supercritical region into the retuning of a cubic EoS can improve its performance above the critical point dramatically. Adopting a retuned acentric factor of 0.5491 instead of its genuine value of 0.344 for water in PR-EoS and a new F of 0.8854 instead of its original value of 0.6898 for water in PT-EoS reduces the discrepancies to about one third or less.

Keywords: equation of state, EoS, supercritical water, SCW

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Authors: Haibo Zhao, Thomas Andre, Katherine Avery, Alper Kiziltas, Deborah Mielewski

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Silica aerogels were fabricated through a modified rapid supercritical extraction (RSCE) process. The silica aerogels were made using a tetramethyl orthosilicate precursor and then placed in a hot press and brought to the supercritical point of the solvent, ethanol. In order to control the pressure release without a pressure controller, a needle valve was used. The resulting aerogels were then characterized for their physical and chemical properties and compared to silica aerogels created using similar methods. The aerogels fabricated using this modified RSCE method were found to have similar properties to those in other papers using the unmodified RSCE method. Silica aerogel infused glass blanket composite, graphene reinforced silica aerogel composite were also successfully fabricated by this new method. The modified RSCE process and system is a prototype for better gas outflow control with a lower cost of equipment setup. Potentially, this process could be evolved to a continuous low-cost high-volume production process to meet automotive requirements.

Keywords: aerogel, automotive, rapid supercritical extraction process, low cost production

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Authors: Yang Wanhuan, Zou Jichun, LI Shen, Zhong Weihua, Yang Wen

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High entropy alloys (HEAs) have aroused significant concern in high-temperature supercritical carbon dioxide (S-CO2) environments due to their unique microstructures and outstanding properties. However, the anti-corrosion ability and mechanism of these HEAs in the S-CO₂ remain unclear. Herein, we developed a new AlCrFeNiMn (AM)-HEA with double phases by vacuum arc melting furnace. The corrosion behavior of AM-HEA in the S-CO₂ at 500 ℃ under 25 MPa for 400 hours was deciphered by multiple characterization techniques. The results show that the discrepancy of corrosion between the matrix and boundary was accounted for by their microstructure and components. The role and mechanism of Mn contents for their oxide scales in boundary zones were emphasized. More importantly, the nano-precipitated second phase and numerous boundaries for the outstanding anti-corrosion ability of the matrix were proposed.

Keywords: high entropy alloy, microstructure, corrosion, supercritical carbon oxide, AlCrFeNiMn

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Authors: Saziye Ilgaz, Atilla Polat

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There is a need for development of new processing techniques to ensure safety and quality of final product while minimizing the adverse impact of extraction solvents on environment and residue levels of these solvents in final product, decaffeinated black tea. In this study pilot scale supercritical carbon dioxide (SCCO₂) extraction was used to produce decaffeinated black tea in place of solvent extraction. Pressure (250, 375, 500 bar), extraction time (60, 180, 300 min), temperature (55, 62.5, 70 °C), CO₂ flow rate (1, 2 ,3 LPM) and co-solvent quantity (0, 2.5, 5 %mol) were selected as extraction parameters. The five factors BoxBehnken experimental design with three center points was performed to generate 46 different processing conditions for caffeine removal from black tea samples. As a result of these 46 experiments caffeine content of black tea samples were reduced from 2.16 % to 0 – 1.81 %. The experiments showed that extraction time, pressure, CO₂ flow rate and co-solvent quantity had great impact on decaffeination yield. Response surface methodology (RSM) was used to optimize the parameters of the supercritical carbon dioxide extraction. Optimum extraction parameters obtained of decaffeinated black tea were as follows: extraction temperature of 62,5 °C, extraction pressure of 375 bar, CO₂ flow rate of 3 LPM, extraction time of 176.5 min and co-solvent quantity of 5 %mol.

Keywords: supercritical carbon dioxide, decaffeination, black tea, extraction

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Authors: Shyh-Ming Chern, Hung-Chi Tu

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One way to utilize biomass is to thermochemically convert it into gases and chemicals. For conversion of biomass, glucose is a particularly popular model compound for cellulose, or more generally for biomass. The present study takes a different approach by employing lactic acid as the model compound for cellulose. Since lactic acid and glucose have identical elemental composition, they are expected to produce similar results as they go through the conversion process. In the current study, lactic acid was thermochemically converted to assess its reactivity and reaction mechanism in subcritical and supercritical water, by using a 16-ml autoclave reactor. The major operating parameters investigated include: The reaction temperature, from 673 to 873 K, the reaction pressure, 10 and 25 MPa, the dosage of oxidizing agent, 0 and 0.5 chemical oxygen demand, and the concentration of lactic acid in the feed, 0.5 and 1.0 M. Gaseous products from the conversion were generally found to be comparable to those derived from the conversion of glucose.

Keywords: lactic acid, subcritical water, supercritical water, thermochemical conversion

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Authors: Hasan Izhar Khan, Naiqiang Zhang, Hong Xu, Zhongliang Zhu, Dongfang Jiang

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Inconel 617, a nickel-based alloy designed for high-temperature applications, got an excellent amalgamation of strength and oxidation resistance at high temperatures. For a better understanding of its suitability to be used in superheater and reheater tubes in ultra-supercritical power plants, stress corrosion cracking (SCC) susceptibility must be evaluated. In the present study, the effect of medium environment on SCC behavior of Inconel 617, in the form of a round bar tensile specimen, was tested via slow strain rate tensile tests in steam and supercritical water (SCW) at 650 °C. The results showed that SCC susceptibility has a linear relationship with exposed pressure and increases monotonically with an increase in pressure. A severe SCC susceptibility was observed in SCW followed by that in a steam environment. Fracture and gage surface showed apparent characteristics of brittle fracture. Intergranular cracks initiated from the edge region and propagated into the matrix through cross section until ductile rupture. When dissolved oxygen contents were decreased in SCW environment, it showed no noticeable effect on mechanical properties but SCC susceptibility slightly decreased. The research revealed the influence of environment on SCC susceptibility of Inconel 617 in steam and SCW.

Keywords: Inconel 617, steam, supercritical water, stress corrosion cracking

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Authors: Najwa Othman, Norhidayah Suleiman, Gun Hean Chong

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Palm fatty acid distillate (PFAD) is a by-product of palm oil refineries which contains valuable compounds such as phytosterols, squalene, polycosanol, co-enzyme Q10 and vitamin E (tocopherols and tocotrienols). Approximately 0.7-1.0% of vitamin E accumulates in PFAD, and it functions as antioxidants and anti-inflammatory. The objective of this research is to evaluate the effect of manipulated variables in supercritical carbon dioxide towards the recovery of tocotrienols in PFAD. The vitamin E concentrate isolated varies depending on the pre-treatment of sample and extraction techniques. In this research, tocotrienols in PFAD was concentrated by removing the extraneous matters, especially free fatty acid (FFA) and acylglycerols. Pre-treatment method such as enzymatic hydrolysis by using lipase from Candida rugosa as an enzyme was used to remove FFA and improve recovery of vitamin E. After that, treated PFAD was extracted by using supercritical fluid extraction in co-current glass beads packed column (22 cm x 75 cm i.d) at different temperatures (40-60°C) and pressures (100-300 bar) for 5 hours. After the extraction, the sample was analyzed by using high-pressure liquid chromatography (HPLC) system to quantify the tocotrienols. The results indicated that a combined pressure (200 bar) and temperature (60°C) was predicted to provide highest tocotrienols yield and the extraction yield obtained was 106.45%.

Keywords: enzymatic hydrolysis, palm fatty acid distillate, supercritical fluid extraction, tocotrienols

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Authors: Muhamad Syafiq Hakimi Kamaruddin, Norhidayah Suleiman

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Ginger extracts (Zingiber officinale Rosc.) have been attributed therapeutic properties primarily as antioxidant, anticancer, and anti-inflammatory properties. Conventional extractions including Soxhlet and maceration are commonly used to extract the bioactive compounds from plant material. Nevertheless, high energy consumption and being non-environmentally friendly are the predominant limitations of the conventional extractions method. Herein, green technology, namely supercritical carbon dioxide (scCO2) extraction, is used to study process variables' effects on extract yields. Herein, green technology, namely supercritical carbon dioxide (scCO2) extraction, is used to study process variables' effects on extract yields. A pressure (10-30 MPa), temperature (40-60 °C), and median particle size (300-600 µm) were conducted at a CO2 flow rate of 0.9 ± 0.2 g/min for 120 mins. The highest overall yield was 4.58% obtained by the scCO2 extraction conditions of 300 bar and 60 °C with 300µm of ginger powder for 120 mins. In comparison, the yield of the extract was increased considerably within a short extraction time. The results show that scCO2 has a remarkable ability over ginger extract and is a promising technology for extracting bioactive compounds from plant material.

Keywords: conventional, ginger, non-environmentally, supercritical carbon dioxide, technology

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Authors: Norhidayah Suleiman, Afza Zulfaka

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Zingiber officinale var. Bentong has been identified as the source of high added value compound specifically gingerol-related compounds. The extraction of the high-value compound using conventional method resulted in low yield and time consumption. Hence, the motivation for this work is to investigate the effect of the extraction technique on the essential oil from Zingiber officinale var. Bentong rhizome for commercialization purpose in many industries namely, functional food, pharmaceutical, and cosmeceutical. The investigation begins with a pre-treatment using ultrasound assisted in order to enhance the recovery of essential oil. It was conducted at a fixed frequency (20 kHz) of ultrasound with various time (10, 20, 40 min). The extraction using supercritical carbon dioxide (scCO2) were carried out afterward at a specific condition of temperature (50 °C) and pressure (30 MPa). scCO2 extraction seems to be a promising sustainable green method for the extraction of essential oil due to the benefits that CO2 possesses. The expected results demonstrated the ultrasound-assisted-scCO2 produces a higher yield of essential oil compared to solely scCO2 extraction. This research will provide important features for its application in food supplements or phytochemical preparations.

Keywords: essential oil, scCO2, ultrasound assisted, Zingiber officinale Var. Bentong

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Authors: N. A. Zainuddin, I. Norhuda, I. S. Adeib, A. N. Mustapa, S. H. Sarijo

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Recently, RESS (Rapid Expansion Supercritical Solution) method has been used by researchers to produce fine particles for pharmaceutical drug substances. Since RESS technology acknowledges a lot of benefits compare to conventional method of ginger extraction, it is suggested to use this method to explore particle formation of bioactive compound from powder ginger. The objective of this research is to produce direct solid oil particles formation from ginger rhizome which contains valuable compounds by using RESS-CO₂ process. RESS experiments were carried using extraction pressure of 3000, 4000, 5000, 6000 and 7000psi and at different extraction temperature of 40, 45, 50, 55, 60, 65 and 70°C for 40 minutes extraction time and contant flowrate (24ml/min). From the studies conducted, it was found that at extraction pressure 5000psi and temperature 40°C, the smallest particle size obtained was 2.22μm on 99 % reduction from the original size of 370μm.

Keywords: particle size, RESS, solid oil particle, supercritical carbon dioxide,

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Authors: Angela Justina Kumalaputri

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Indonesia, as a maritime country, has abundant marine living resources yet has not been optimally utilized. So far, we only focusing on fisheries. In the other hand, Indonesia, as the country with the fourth longest coastline, is a very good cultivation place for microalgae. Microalgae can be diversified to many important products, such as food, fuel, pharmaceutical products, functional food, and cosmetics.This research is focusing on the literature study about types of microalgae as sources for functional foods (such as antioxidants), including the contents and the separation methods. The research methods which we use are: (1) Literature study about various microalgaes (2) Literature study about extractions using supercritical fluid of CO₂, which are free from toxic organic solvents, environmentally friendly, and safe for food products. Supercritical fluid extraction using CO₂ (low critical points: temperature at 31.1 oC and pressure at 72.9 bars) could be done at a low temperature which are suitable for temperature labile compounds, low energy, and faster extraction time compared with conventional method of extraction.

Keywords: antioxidants, supercritical fluid extraction, solvent-free extraction, microalgae

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Authors: Antonio Montes, Antonio Cozar, Clara Pereyra, Diego Valor, Enrique Martinez de la Ossa

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Tissues and organs can be damaged because of traumatism, congenital illnesses, or cancer and the traditional therapeutic alternatives, such as surgery, cannot usually completely repair the damaged tissues. Tissue engineering allows regeneration of the patient's tissues, reducing the problems caused by the traditional methods. Scaffolds, polymeric structures with interconnected porosity, can be promoted the proliferation and adhesion of the patient’s cells in the damaged area. Furthermore, by means of impregnation of the scaffold with beneficial active substances, tissue regeneration can be induced through a drug delivery process. The objective of the work is the fabrication of a PVA scaffold coated with Gallic Acid and polypyrrole through a one-step foaming and impregnation process using the SSI technique (Supercritical Solvent Impregnation). In this technique, supercritical CO₂ penetrates into the polymer chains producing the plasticization of the polymer. In the depressurization step a CO₂ cellular nucleation and growing to take place to an interconnected porous structure of the polymer. The foaming process using supercritical CO₂ as solvent and expansion agent presents advantages compared to the traditional scaffolds’ fabrication methods, such as the polymer’s high solubility in the solvent or the possibility of carrying out the process at a low temperature, avoiding the inactivation of the active substance. In this sense, the supercritical CO₂ avoids the use of organic solvents and reduces the solvent residues in the final product. Moreover, this process does not require long processing time that could cause the stratification of substance inside the scaffold reducing the therapeutic efficiency of the formulation. An experimental design has been carried out to optimize the SSI technique operating conditions, as well as a study of the morphological characteristics of the scaffold for its use in tissue engineerings, such as porosity, conductivity or the release profiles of the active substance. It has been proved that the obtained scaffolds are partially porous, conductors of electricity and are able to release Gallic Acid in the long term.

Keywords: scaffold, foaming, supercritical, PVA, polypyrrole, gallic acid

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Authors: Andrey Davydov, Konstantin Sveshnikov, Yulia Voronina

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There is now a lot of interest to the non-perturbative QED-effects, caused by diving of discrete levels into the negative continuum in the supercritical static or adiabatically slowly varying Coulomb fields, that are created by the localized extended sources with Z > Z_cr. Such effects have attracted a considerable amount of theoretical and experimental activity, since in 3+1 QED for Z > Z_cr,1 ≈ 170 a non-perturbative reconstruction of the vacuum state is predicted, which should be accompanied by a number of nontrivial effects, including the vacuum positron emission. Similar in essence effects should be expected also in both 2+1 D (planar graphene-based hetero-structures) and 1+1 D (one-dimensional ‘hydrogen ion’). This report is devoted to the study of such essentially non-perturbative vacuum effects for the supercritical Dirac-Coulomb systems in 1+1D and 2+1D, with the main attention drawn to the vacuum polarization energy. Although the most of works considers the vacuum charge density as the main polarization observable, vacuum energy turns out to be not less informative and in many respects complementary to the vacuum density. Moreover, the main non-perturbative effects, which appear in vacuum polarization for supercritical fields due to the levels diving into the lower continuum, show up in the behavior of vacuum energy even more clear, demonstrating explicitly their possible role in the supercritical region. Both in 1+1D and 2+1D, we explore firstly the renormalized vacuum density in the supercritical region using the Wichmann-Kroll method. Thereafter, taking into account the results for the vacuum density, we formulate the renormalization procedure for the vacuum energy. To evaluate the latter explicitly, an original technique, based on a special combination of analytical methods, computer algebra tools and numerical calculations, is applied. It is shown that, for a wide range of the external source parameters (the charge Z and size R), in the supercritical region the renormalized vacuum energy could significantly deviate from the perturbative quadratic growth up to pronouncedly decreasing behavior with jumps by (-2 x mc^2), which occur each time, when the next discrete level dives into the negative continuum. In the considered range of variation of Z and R, the vacuum energy behaves like ~ -Z^2/R in 1+1D and ~ -Z^3/R in 2+1D, exceeding deeply negative values. Such behavior confirms the assumption of the neutral vacuum transmutation into the charged one, and thereby of the spontaneous positron emission, accompanying the emergence of the next vacuum shell due to the total charge conservation. To the end, we also note that the methods, developed for the vacuum energy evaluation in 2+1 D, with minimal complements could be carried over to the three-dimensional case, where the vacuum energy is expected to be ~ -Z^4/R and so could be competitive with the classical electrostatic energy of the Coulomb source.

Keywords: non-perturbative QED-effects, one- and two-dimensional Dirac-Coulomb systems, supercritical fields, vacuum polarization

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Authors: Oscar Corredor, Alexander Guzman, Adan Leon

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Density is a bulk physical property that indicates the quality of a petroleum fraction. It is also a useful property to estimate various physicochemical properties of fraction and petroleum fluids; however, the determination of density of extra heavy residual (EHR) fractions by standard methodologies, (ASTM D70) shows limitations for samples with higher densities than 1.0879 g/cm3. For this reason, a dilution methodology was developed in order to determinate density for those particular fractions, 87 (EHR) fractions were obtained as products of the fractionation of Colombian typical Vacuum Distillation Residual Fractions using molecular distillation (MD) and extraction with Solvent N-hexane in Supercritical Conditions (SFEF) pilot plants. The proposed methodology showed reliable results that can be demonstrated with the standard deviation of repeatability and reproducibility values of 0.0031 and 0.0061 g/ml respectively. In the same way, it was possible to determine densities in fractions EHR up to 1.1647g/cm3 and °API values obtained were ten times less than the water reference value.

Keywords: API, density, vacuum residual, molecular distillation, supercritical fluid extraction

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Authors: Buket Boz, Alvaro Diez

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Waste heat recovery by means of Organic Rankine Cycle is a promising technology for the recovery of engine exhaust heat. However, it is complex to find out the optimum cycle conditions with appropriate working fluids to match exhaust gas waste heat due to its high temperature. Hence, this paper focuses on comparing sub-critical and supercritical ORC conditions with eight working fluids on a combined diesel engine-ORC system. The model employs two ORC designs, Regenerative-ORC and Pre-Heating-Regenerative-ORC respectively. The thermodynamic calculations rely on the first and second law of thermodynamics, thermal efficiency and exergy destruction factors are the fundamental parameters evaluated. Additionally, in this study, environmental and safety, GWP (Global Warming Potential) and ODP (Ozone Depletion Potential), characteristic of the refrigerants are taken into consideration as evaluation criteria to define the optimal ORC configuration and conditions. Consequently, the studys outcomes reveal that supercritical ORCs with alkane and siloxane are more suitable for high temperature exhaust waste heat recovery in contrast to sub-critical conditions.

Keywords: internal combustion engine, organic Rankine cycle, waste heat recovery, working fluids

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Authors: Strahinja Kovačević, Jelena Vladić, Senka Vidović, Zoran Zeković, Lidija Jevrić, Sanja Podunavac Kuzmanović

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Supercritical extracts of highly valuated medicinal plant Satureja montana were prepared by application of supercritical carbon dioxide extraction in the carbon dioxide pressure range from 125 to 350 bar and temperature range from 40 to 60°C. Using GC/MS method of analysis chemical profiles (aromatic constituents) of S. montana extracts were obtained. Self-training artificial neural networks were applied to predict the retention time of the analyzed terpenes in GC/MS system. The best ANN model obtained was multilayer perceptron (MLP 11-11-1). Hidden activation was tanh and output activation was identity with Broyden–Fletcher–Goldfarb–Shanno training algorithm. Correlation measures of the obtained network were the following: R(training) = 0.9975, R(test) = 0.9971 and R(validation) = 0.9999. The comparison of the experimental and predicted retention times of the analyzed compounds showed very high correlation (R = 0.9913) and significant predictive power of the established neural network.

Keywords: ANN regression, GC/MS, Satureja montana, terpenes

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Authors: M. Bouinoun, M. Bouhadef

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The present study is concerned with the problem of determining the shape of the free surface flow in a hydraulic channel which has an uneven bottom. For the mathematical formulation of the problem, the fluid of the two-dimensional irrotational steady flow in water is assumed inviscid and incompressible. The solutions of the nonlinear problem are obtained by using the usual conformal mapping theory and Hilbert’s technique. An experimental study, for comparing the obtained results, has been conducted in a hydraulic channel (subcritical regime and supercritical regime).

Keywords: free-surface flow, experiments, numerical method, uneven bottom, supercritical regime, subcritical regime

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Authors: Vadim V. Zefirov, Victor E. Sizov, Marina A. Pigaleva, Igor V. Elmanovich, Mikhail S. Kondratenko, Marat O. Gallyamov

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This work presents a novel method for treating porous hydrophobic polyolefin membranes using supercritical carbon dioxide that allows usage of the modified membrane in redox flow batteries with an aqueous electrolyte. Polyolefin membranes are well known and widely used, however, they cannot be used as separators in redox flow batteries with an aqueous electrolyte since they have insufficient wettability, and therefore do not provide sufficient proton conductivity. The main aim of the presented work was the development of hydrophilic composites based on cheap membranes and precursors. Supercritical fluid was used as a medium for the deposition of the hydrophilic phase on the hydrophobic surface of the membrane. Due to the absence of negative capillary effects in a supercritical medium, a homogeneous composite is obtained as a result of synthesis. The in-situ synthesized silicon oxide nanoparticles and the chitosan polymer layer act as the hydrophilic phase and not only increase the affinity of the membrane towards the electrolyte, but also reduce the pore size of the polymer matrix, which positively affects the ion selectivity of the membrane. The composite material obtained as a result of synthesis has enhanced hydrophilic properties and is capable of providing proton conductivity in redox flow batteries. The morphology of the obtained composites was characterized by electron microscopy. To analyze the phase composition, infrared spectroscopy was used. The hydrophilic properties were studied by water contact angle measurements. In addition, the proton conductivity and ion selectivity of the obtained samples were studied, and tests in real redox flow batteries were performed. As a result, modified membrane was characterised in detail and moreover it was shown that modified cheap polyolefin membranes have pronounced proton conductivity and high ion selectivity, so their performance in a real redox flow battery approaches expensive commercial analogues, reaching 70% of energy efficiency.

Keywords: carbon dioxide, chitosan, polymer membrane, redox flow batteries, silica nanoparticles, supercritical fluid

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Authors: Y. A. Shapovalov, F. M. Gumerov, M. K. Nauryzbaev, S. V. Mazanov, R. A. Usmanov, A. V. Klinov, L. K. Safiullina, S. A. Soshin

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A flow-through installation was created and manufactured for the transesterification of triglycerides of fatty acids and production of biodiesel fuel under supercritical fluid conditions. Transesterification of rapeseed oil with ethanol was carried out according to two parameters: temperature and the ratio of alcohol/oil mixture at the constant pressure of 19 MPa. The kinetics of the yield of fatty acids ethyl esters (FAEE) was determined in the temperature range of 320-380 °C at the alcohol/oil molar ratio of 6:1-20:1. The content of the formed FAEE was determined by the method of correlation of the resulting biodiesel fuel by its kinematic viscosity. The maximum FAEE yield (about 90%) was obtained within 30 min at the ethanol/oil molar ratio of 12:1 and a temperature of 380 °C. When studying of transesterification of triglycerides, a kinetic model of an isothermal flow reactor was used. The reaction order implemented in the flow reactor has been determined. The first order of the reaction was confirmed by data on the conversion of FAEE during the reaction at different temperatures and the molar ratios of the initial reagents (ethanol/oil). Using the Arrhenius equation, the values of the effective constants of the transesterification reaction rate were calculated at different reaction temperatures. In addition, based on the experimental data, the activation energy and the pre-exponential factor of the transesterification reaction were determined.

Keywords: biodiesel, fatty acid esters, supercritical fluid technology, transesterification

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Authors: Radek Novotny, Michal Novak, Daniela Marusakova, Monika Sipova, Hugo Fuentes, Peter Borst

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This research has been conducted within the European HORIZON 2020 project ECC-SMART. The main objective is to assess whether it is feasible to design and develop a small modular reactor (SMR) that would be cooled by supercritical water (SCW). One of the main objectives for material research concerns the corrosion of the candidate cladding materials. The experimental part has been conducted in support of the qualification procedure of the future SCW-SMR constructional materials. The last objective was to identify the gaps in current norms and guidelines. Apart from corrosion, resistance testing of candidate materials stresses corrosion cracking susceptibility tests have been performed in supercritical water. This paper describes part of these tests, in particular, those slow strain rate tensile loading applied for tangential ring shape specimens of two candidate materials, Alloy 800H and 310S stainless steel. These ring tensile tests are one the methods used for tensile testing of nuclear cladding. Here full circular heads with dimensions roughly equal to the inner diameter of the sample and the gage sections are placed in the parallel direction to the applied load. Slow strain rate tensile tests have been conducted in 380 or 500oC supercritical water applying two different elongation rates, 1x10-6 and 1x10-7 s-1. The effect of temperature and dissolved oxygen content on the SCC susceptibility of Alloy 800H and 310S stainless steel was investigated when two different temperatures and concentrations of dissolved oxygen were applied in supercritical water. The post-fracture analysis includes fractographic analysis of the fracture surfaces using SEM as well as cross-sectional analysis on the occurrence of secondary cracks. Assessment of the effect of environment and dissolved oxygen content was by comparing to the results of the reference tests performed in air and N2 gas overpressure. The effect of high temperature on creep and its role in the initiation of SCC was assessed as well. It has been concluded that the applied test method could be very useful for the investigation of stress corrosion cracking susceptibility of candidate cladding materials in supercritical water.

Keywords: stress corrosion cracking, ring tensile tests, super-critical water, alloy 800H, 310S stainless steel

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Authors: Wen-Chyan Tsai, Syed S. H. Rizvi

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Organic solvent residues are always associated with liposomes produced by the traditional techniques like the thin film hydration and reverse phase evaporation methods, which limit the applications of these vesicles in the pharmaceutical, food and cosmetic industries. Our objective was to develop a novel and benign process of liposomal microencapsulation by using supercritical carbon dioxide (SC-CO2) as the sole phospholipid-dissolving medium and a green substitute for organic solvents. This process consists of supercritical fluid extraction followed by rapid expansion via a nozzle and automatic cargo suction. Lecithin and cholesterol mixed in 10:1 mass ratio were dissolved in SC-CO2 at 20 ± 0.5 MPa and 60 oC. After at least two hours of equilibrium, the lecithin/cholesterol-laden SC-CO2 was passed through a 1000-micron nozzle and immediately mixed with the cargo solution to form liposomes. Liposomal micro-encapsulation was conducted at three pressures (8.27, 12.41, 16.55 MPa), three temperatures (75, 83 and 90 oC) and two flow rates (0.25 ml/sec and 0.5 ml/sec). Liposome size, zeta potential and encapsulation efficiency were characterized as functions of the operating parameters. The average liposomal size varied from 400-500 nm to 1000-1200 nm when the pressure was increased from 8.27 to 16.55 MPa. At 12.41 MPa, 90 oC and 0.25 ml per second of 0.2 M glucose cargo loading rate, the highest encapsulation efficiency of 31.65 % was achieved. Under a confocal laser scanning microscope, large unilamellar vesicles and multivesicular vesicles were observed to make up a majority of the liposomal emulsion. This new approach is a rapid and continuous process for bulk production of liposomes using a green solvent. Based on the results to date, it is feasible to apply this technique to encapsulate hydrophilic compounds inside the aqueous core as well as lipophilic compounds in the phospholipid bilayers of the liposomes for controlled release, solubility improvement and targeted therapy of bioactive compounds.

Keywords: liposome, micro encapsulation, supercritical carbon dioxide, non-toxic process

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Authors: Asım Egitmen, Aysen Demir, Burcu Darendeli, Fatma Ulusal, Bilgehan Güzel

Abstract:

Synthesizing supercritical carbon dioxide (scCO₂) soluble precursors would be helpful for many processes of material syntheses based on scCO₂. Ligand (amphi-(1Z, 2Z)-N-(2-fluoro-3-(trifluoromethyl) phenyl)-N'-hydroxy-2-(hydroxyimino) were synthesized from chloro glyoxime and flourus aniline and Pd(II) complex (precursor) prepared. For scCO₂ deposition method, organometallic precursor was dissolved in scCO₂ and impregnated onto the SBA-15 at 90 °C and 3000 psi. Then the organometallic precursor was reduced with H₂ in the CO₂ mixture (150 psi H₂ + 2850 psi CO₂). Pd deposited support material was characterized by ICP-OES, XRD, FE-SEM, TEM and EDX analyses. The Pd loading of the prepared catalyst, measured by ICP-OES showed a value of about 1.64% mol/g Pd of catalyst. Average particle size was found 5.3 nm. The catalytic activity of prepared catalyst was investigated over Suzuki-Miyaura C-C coupling reaction in different solvent with K₂CO₃ at 50 ^oC. The conversion ratio was determined by gas chromatography.

Keywords: nanoparticle, nanotube, oximes, precursor, supercritical CO2

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Authors: Dhara Adhnandya Kumara, Novrizal Novrizal

Abstract:

Hot Dry Rock (HDR) is one of geothermal energy which is abundant in many provinces in Indonesia. Heat exploitation from HDR would need a method which injects fluid to subsurface to crack the rock and sweep the heat. Water is commonly used as the working fluid but known to be less effective in some ways. The new research found out that Supercritical CO2 (SCCO2) can be used to replace water as the working fluid. By studying heat transfer efficiency, pumping power, and characteristics of the returning fluid, we might decide how effective SCCO2 to replace water as working fluid. The method used to study those parameters quantitatively could be obtained from pre-existing researches which observe the returning fluids from the same reservoir with same pumping power. The result shows that SCCO2 works better than water. For cold and hot SCCO2 has lower density difference than water, this results in higher buoyancy in the system that allows the fluid to circulate with lower pumping power. Besides, lower viscosity of SCCO2 impacts in higher flow rate in circulation. The interaction between SCCO2 and minerals in reservoir could induce dehydration of the minerals and enhancement of rock porosity and permeability. While the dissolution and transportation of minerals by SCCO2 are unlikely to occur because of the nature of SCCO2 as poor solvent, and this will reduce the mineral scaling in the system. Under those conditions, using SCCO2 as working fluid for HDR extraction would give great advantages to advance geothermal energy in Indonesia.

Keywords: geothermal, supercritical CO2, injection fluid, hot dry rock

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Authors: Sudhir Kumar Sharma, Abiy D. Woldetsadik, Mazin Magzoub, Ramesh Jagannathan

Abstract:

It is well known that bioactive ceramics exhibit specific biological affinities, especially in the area of tissue re-generation. In this context, we report the development of an eminently scalable, novel, supercritical CO₂ based process for the fabrication of hierarchically porous 'soft' CaCO₃ scaffolds. Porosity at the macro, micro, and nanoscales was obtained through process optimization of the so-called 'coffee-ring effect'. Exposure of these CaCO₃ scaffolds to monocytic THP-1 cells yielded negligible levels of tumor necrosis factor-alpha (TNF-α) thereby confirming the lack of immunogenicity of the scaffolds. ECM protein treatment of the scaffolds showed enhanced adsorption comparable to standard control such as glass. In vitro studies using osteoblast precursor cell line, MC3T3, also demonstrated the cytocompatibility of hierarchical porous CaCO₃ scaffolds.

Keywords: supercritical CO2, CaCO3 scaffolds, coffee-ring effect, ECM proteins

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Authors: A. Bahadoran, M. Zomorodian

Abstract:

The synthesizer of cobalt oxide nanoballs (length 3−4 μm, width 250−400 nm) was achieved by a simple high-temperature supercritical solution method. Multiwalled carbon aerogels are a step towards high-density nanometer-scale nanostructures. Cobalt oxide nanoballs were prepared by supercritical solution method. Synthesis in an aqueous solution containing cobalt hydroxide at ∼80 °C without any further heat treatment at high temperature. The formation of cobalt oxide nanoballs on carbon aerogel was confirmed by X-ray diffraction and Raman spectroscopy. The FE-SEM images showed the presence of cobalt oxide nanoballs. The reaction mechanism of the ultrasound-assisted synthesis of cobalt oxide nanostructures was proposed on the basis of the XRD, X-ray absorption spectroscopy analysis and FE-SEM observation of the reaction products taken during the course of the synthesis.

Keywords: cobalt oxide nano balls, carbon aerogel, synthesize, nanostructure

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Authors: Senem Suna

Abstract:

Extraction of bioactive compounds from several food/food products comes as an important topic and new trend related with health promoting effects. As a result of the increasing interest in natural foods, different methods are used for the acquisition of these components especially polyphenols. However, special attention has to be paid to the selection of proper techniques or several processing technologies (supercritical fluid extraction, microwave-assisted extraction, ultrasound-assisted extraction, powdered extracts production) for each kind of food to get maximum benefit as well as the obtainment of phenolic compounds. In order to meet consumer’s demand for healthy food and the management of quality and safety requirements, advanced research and development are needed. In this review, advantages, and disadvantages of different extraction methods, their opportunities to be used in food industry and the effects of polyphenols are mentioned in details. Consequently, with the evaluation of the results of several studies, the selection of the most suitable food specific method was aimed.

Keywords: bioactives, extraction, powdered extracts, supercritical fluid extraction

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