Optimization of Supercritical Extraction Process of Laoshan Black Tea by Response Surface Methodology

[Objectives]Laoshan black tea was subjected to supercritical CO_(2) extraction. [Methods]The extraction conditions of Laoshan black tea were studied by an orthogonal experiment and optimized by response surface methodology. [Results] The optimum extraction conditions of black tea extract by supercritical CO_(2) extraction were as follows: extraction pressure 23.53 MPa, extraction time 1.73 h, and extraction temperature 49.75 ℃, with which the extract yield could reach 5.15% theoretically. [Conclusions] Based on the traditional extraction process, a supercritical extraction method optimized by response surface methodology and a unique extraction process were formed, which enriches the extraction processes and methods of natural raw materials.

Extraction of cellulose with subcritical and Supercritical ethanol

Cotton cellulose was extracted with ethanol in sub-and supercritical states dynamically. The degree of conversion was 95.4% and the extract yield was 55.2% when cotton cellulose was non-isothermally extracted with ethanol from 20°C to 400°C. From an engineering standpoint, in the temperature range from 200°C to 320°C, the rate of extract formation could adequately be described by a second-order reaction kinetics equation with the activation energy of 105.3 kJ/mol and the pre-exponential factor of 3.53×107 s?1. With the non-isothermal experimental technique, it was possible to determine the kinetic parameters; conversion degree and extract yield by one experiment.

XPS analysis and combustibility of residues from two coals extraction with sub-and supercritical water

Two kinds of residues,obtained from extraction of one weakly reductive coal,Shenfu-Dongsheng coal(SD),and one reductive coal,Pingshuo coal(PS),with sub-and supercritical water on a semi-continuous apparatus,were characterized by calorific value analysis and XPS analysis,and the combustion behaviors of residues were investigated by thermogravimetric analysis.The results show that the residues have higher calorific value than raw coal samples,and SD residue has higher calorific value than PS residue.C-C,C-O and pyridinic nitrogen,pyrrolic nitrogen are the dominant form of C,O and N on the surface of raw coal samples and their extraction residues.The combustion behaviors of extraction residues show that the SD residue is more reactive and more easily burned than PS residue.

Influence of Modifier in Supercritical CO₂on Qualitative and Quantitative Extraction Results of <i>Eucalyptus</i>Ecential Oil

A supercritical CO2 extraction behavior of Eucalyptus oil was investigated under different conditions of pressure, temperature and time with or without cosolvent. The pressure range was from 8 to 25 MPa, temperature from 35 to 55&deg;C and CO2 flow rate from 10 to 26 g/min. For 1,8-cineole the appropriate extracting pressure was 15 MPa and temperature was 45&deg;C. When CO2 flow rate was 18 g/min, it was benefit to extract the other three substances (limonene, p-cymene and γ-terpinene, respectively) except 1,8-cineole. Prolonging extraction time could not obviously increase the extract concentration, but the extract yield would increase. The results also indicated that ethanol as a modifier could improve extraction velocity and extraction concentration.

Extraction and Characterization of Oil from <i>Moringa oleifera</i>Using Supercritical CO₂and Traditional Solvents

The present work presents a first characterization of the oil from the Moringa (Moringa oleifera) kernel as a potential candidate for biodiesel production. Moringa is an indigenous tree in the Yucatan Peninsula in Mexico, where there is a nascent biodiesel industry. Several extraction methods are compared in terms of the extraction yields, including solvent extraction (n-hexane and ethanol), and supercritical extraction (Sc-CO2). The results are also compared against previ- ously reported data. For supercritical extraction pressures of 200 to 400 bar and temperatures of 40℃ and 60℃ were tested. Gas Chromatography analysis reveals that the main fatty acids in Moringa oil are oleic acid (69%), palmitic acid (10%), and stearic acid (8%).

Isolation and Extraction of Total Flavonoids from Epimedium Koreanum Nakai by Supercritical Fluid Extraction

In the present paper is reported the method for the isolation and extraction of total flavonoids of Epimedium Koreanum Nakai by means of supercritical fluid extraction(SFE). By examining pressure, temperature, amounts of modifier and extraction time, the optimized condition of SFE is confirmed as 30 MPa and 60 ℃, with 70% ethanol as the modifier. The samples were statically extracted for 30 min, followed by dynamic extraction for 120 min at a flow rate of 6 mL/min. The quantitative analysis of total flavonoids was performed by UV-Vis spectrophotometry. Compared with the conventional method, the SFE method is more efficient, more rapid and more friendly environmentally.

Supercritical Fluid Extraction of Total Flavonoids from Leaves of Acanthopanax Senticosus Harms

The herbal plant Acanthopanax Senticosus Harms is natural herb of Changbaishan in Jilin Province of China, which belongs to the Araliaceae family. As the ingredients of folk medicine, it has long been used to treat a variety of human diseases, such as cerebrovascular disease, diabetes, tumor, isochemic heart diseases, hypertension, rheumatic arthritis, etc. E2,33. Flavonoids, a class of constituent compounds, which have a broad distribution in the nature and are found in Acanthopanax Senticosus Harms, have gained particular attention. A number of studies have shown that flavonoid compounds have wide biological activities, such as anti-aging, anticancer, anti-HIV,

Experimental optimization and mathematical modeling of supercritical carbon dioxide extraction of essential oil from Pogostemon cablin

The supercritical carbon dioxide extraction was applied to obtain essential oil from Pogostemon cablin in this work.Effect of extraction parameters including temperature,pressure,extraction time and particle size on extraction yield was investigated,and the response surface methodology with a Box–Behnken Design was used to achieve the optimized extraction conditions.The maximum yield of essential oil was 2.4356%under the conditions of extraction temperature 47°C,pressure 24.5 MPa and extraction time 119 min.Moreover,based on the Brunauer–Emmett–Teller theory of adsorption,a mathematical modeling was performed to correlate the measured data.The model shows a function relationship between extraction yield and time by a simple equation with three significantly adjustable parameters.These model parameters have been optimized through simulated annealing algorithm.The predicted data from the mathematical model show a good agreement with the experimental data of the different extraction parameters.

Metal Ions Extraction with Glucose Derivatives as Chelating Reagents in Supercritical Carbon Dioxide

A series of glucose derivatives have been used as chelating reagents to extract metal ions in supercritical carbon dioxide. With perfluoro-l-octanesulfonic acid tetraethylammonium salt as additive, glucose derivatives were selective for Sr^2＋ and Pb^2＋ extraction in supercritical carbon dioxide.

Supercritical Fluid Extraction of Saponins from Ginseng

Introduction Ginseng（ Panax ginseng C. A. Meyer, Araliaceae） is one of the most valuable Chinese crude drugs and has been used widely for over 2000 years. Studies have demonstrated that ginseng can act on the central nervous system, the cardiovascular system and the endocrine system; it can enhance immune function and metabolism; it possesses a biomodulation action, anticancer effect, anti-stress and anti-ageing activities, and so on.

Supercritical fluid extraction of useful compounds from sage

A qualitative analysis of supercritical fluid extraction (SFE) of the medically useful compound, sage (Salvia officinalis) is presented in this study. Carbon dioxide was used as a supercritical solvent. Effects of operating conditions such as temperature, pressure, and extraction time were investigated. The effect of addition of cosolvents was also studied. The extracted useful compounds were identified and analyzed using GC-MS chromatography. The analysis of the extract obtained by SFE showed certain significant major compounds that are considered medically important. These major compounds are 1R-.alpha.-Pinene, D-Limonene, l-Camphene, and b-Pinene, and Eucalyptol. Although, there was no consistent trend with respect to the effect of the studied parameters on the composition of the extract, the selectivity of these major compounds are dependant on the operating conditions, manily the operating pressure. An increase in the pressure resulted in an increase in herb extraction yield;this is true for certain group of extracts, while the inverse is also true for other group of compounds. The effect of certain cosolvents on the extractability of sage showed a significant improvement of the yield of some particular constituents of sage.

Optimization of conditions for supercritical fluid extraction of flavonoids from hops (Humulus lupulus L.)

Waste hops are good sources of flavonoids. Extraction of flavonoids from waste hops (SC-CO2 extracted hops) using supercritical fluids technology was investigated. Various temperatures, pressures and concentrations of ethanol (modifier) and the ratio (w/w) of solvent to material were tested in this study. The results of single factor and orthogonal experiments showed that at 50 °C, 25 MPa, the ratio of solvent to material (50%), ethanol concentration (80%) resulted in maximum extraction yield fla- vonoids (7.8 mg/g). HPLC-MS analysis of the extracts indicated that flavonoids obtained were xanthohumol, the principal prenylflavonoid in hops.

Response Surface Optimization of Nigella glandulifera Freyn Seed Oil Yield by Supercritical Carbon Dioxide Extraction

Supercritical carbon dioxide （SC-CO2） extraction was employed to extract oil from Nigella glandulifera Freyn seed in this study. Response surface methodology （RSM） was applied to evaluate the effects of the process parameters （pressure, temperature, and CO2 flow rate） on oil yield of N. glandulifera seed. A Box-Behnken design was used to optimize the extraction parameters. The analysis of variance indicated that the linear coefficients of pressure and CO2 flow rate, the quadratic term coefficients of pressure and temperature and the interactions between pressure and temperature, as well as temperature and CO2 flow rate, had significant effects on the oil yield （P〈0.05）. The optimal conditions to obtain the maximum oil yield from N. glandulifera seed were pressure 30.84 MPa, temperature 40.57°C, and CO2 flow rate 22.00 L h-1. Under these optimal conditions, the yield of oil was predicted to be 38.19%. The validation experiment results agreed with the predicted values. The fatty acid composition of N. glandulifera seed oil extracted using SC-CO2 was compared with that of oil obtained by Soxhlet method. The results showed that the fatty acid compositions of oil extracted by the two methods were similar. Identification of oil compounds with gas chromatography-mass spectrometry （GC-MS） showed that the contents of unsaturated fatty acids linoleic acid （48.30%）, oleic acid （22.28%） and saturated fatty acids palmitic acid （16.65%）, stearic acid （4.17%） were the most abundant fatty acids in seed oil from N. glandulifera.

Applicability of Static Supercritical Carbon Dioxide Extraction in Biogeochemical Characterization of Oil Shales

This study aimed at the assessment of applicability of static supercritical carbon dioxide extraction method (SFE) in biogeochemical characterization of oil shales as an alternative to the standard Soxhlet extration. A comparative investigation on yields and compositions of the solvent soluble bitumoids and their constituents extracted from Estonian Kukersite and Dictyonema oil shales by using Soxhlet extraction method (SEM) and static CO2 supercritical fluid extraction in an autoclave at varied subpyrolysis temperatures was carried out. Resulting from TLC- and GC-MS-analyses, aliphatic and aromatic hydrocarbons and neutral oxygen compounds were separated and identified. For the first time, in the composition of the Kukersite bitumoid, homologous series of n-alkanones-3 to n-alkanones-7 were detected. The extracts obtained were similar in both group and individual composition, and geochemical parametres calculated on the basis of aliphatic hydrocarbons including that made static SFE applicable to geochemical investigation of oil shales.

Dynamic analysis of heat extraction rate by supercritical carbon dioxide in fractured rock mass based on a thermal-hydraulic-mechanics coupled model

Heat production from geothermal reservoirs is a typical heat transfer process involving a cold working fluid contacting a hot rock formation.Compared to the thermal-physical characteristics of water,supercritical CO_(2)(scCO_(2))has a higher heat storage capacity over a wide temperature-pressure range and may be favored as a heat transfer fluid.Singularly characteristic of scCO_(2)-based heat extraction is that the hydraulic-thermal properties of the scCO_(2) vary dramatically and dynamically with the spatial pressure gradient during unsteady-state flow along fracture.This highly nonlinear behavior presents a challenge in the accurate estimation of heat extraction efficiency in scCO_(2)-based EGS.In this paper,a thermal-h ydraulic-mechanical(THM)coupled model is developed by considering deformation of the fractured reservoir,non-Darcy flow and the varying thermal-physical properties of scCO_(2).The proposed model is validated by matching the modeling temperature distribution with published data.The results show that during continuous injection of scCO_(2),the fracture first widens and then narrows,ultimately reopening over the long term.The sequential fracture deformation behaviors are in response to the combined impacts of mechanical compression and thermally-induced deformation.By controlling the injection parameters of the scCO_(2),it is found that the heat extraction rate is positively correlated to its pore pressure or mass flow rate.The heat extraction rate can be significantly enhanced,when the inlet temperature of scCO_(2) is below its critical temperature.As a result,the heat increment recovered per unit mass of scCO_(2) decreases as the hot rock is gradually cooled.Meanwhile,the heat increment recovered per unit mass of scCO_(2) decreases by increasing the inlet temperature of scCO_(2) or its mass flow rate,but increases as the outlet pressure rises.Furthermore,multi-linear regression indicates that controlling the inlet temperature of the scCO_(2) can significantly improve the thermodynamic efficiency of heat extraction.

Determination of polycyclic aromatic hydrocarbons with supercritical fluid extraction and chromatography（SFE／SFC）

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Production of De-asphalted Oil and Fine Asphalt Particles by Supercritical Extraction

A continuous three-stage supercritical fluid extraction (SFE) process with a capacity of 1.0kg.h^-1 was setup to extract petroleum residue by pentane to obtain more oil for further upgrading. A discharging system integrated to the bottom of the extractor was used to recover solvent as gas while asphalt was obtained as fine particles. The influence of operating conditions on the yield and quality of extracts, i.e., deasphalted oil (DAO) and resin, was studied in the range of temperature 150-220℃, pressure of 4.0-6.0 MPa and the mass ratio of solvent to oil feed (S/O) 2.5-5.0. The particle size distribution, apparent forms and the packing density, which vary with operating pressure, were measured. The particle structures were observed by SEM as well. With the modification to conventional processes, furnace can be eliminated for solvent recovery from asphalt phase, so as to reduce energy consumption.

Beneficiation of coal using supercritical water and carbon dioxide extraction:sulfur removal

This work explores the use of carbon dioxide,water,and their mixtures as solvent for the precombustion beneficiation of raw coal without using any toxic mineral acids in the temperature range of 200-400℃.The fluid polarity,ionic constant,and supercritical point can be adjusted by H_(2)O/CO_(2)ratio and temperature.Adding carbon dioxide to hydrothermal fluid also increases the ionization by forming carbonic acid.Extractions with supercritical fluids have several benefits including enhanced mass transport,ease of separation and recycle,wide range of extractive capability and tunability,better inherent safety,and in the case of carbon dioxide and water-low cost.A semi-continuous extraction system was designed and built in which pressure,temperature and the relative flow rates of CO_(2)and H_(2)O can be controlled.Coal powder is kept in a packed bed and the extraction is carried out at 143 bar pressure.Using sulfur as a model heteroatom,extractive efficiency is examined as a function of the temperature,fluid composition,fluid flow,and extraction time.The results indicate that carbon dioxide,water,and supercritical water-carbon dioxide(ScWC)all can effectively extract about 50%of total sulfur from bituminous coal in 1 h.Extraction above 350℃decreased effectiveness,and extraction above the supercritical point of pure water caused hydrothermal carbonization.ScWC extraction may provide necessary control to prevent organic dissolution while removing sulfur.

Kinetics of Extraction of <i>β</i>-Carotene from Tray Dried Carrots by Using Supercritical Fluid Extraction Technique

β-carotene acts as an antioxidant and is receiving growing interest due to its ability as protecting agent against heart diseases, cancer and strengthening effect on red blood cells. The main aim of this work was to study the kinetics of the supercritical fluid extraction of β-carotene from tray dried carrots at 40℃, 50℃ and 55℃ and 30, 35 and 40 MPa at SC-CO2 flow rate of 2.0 L/min for extraction time of up to 6 h. It was observed that the concentration of β-carotene in the extract increased with pressure, temperature and extraction time. The results indicated that yield was found to be maximum at 45℃ and 35 MPa at 2 L/min SC-CO2 flow rate. Concentration of β-carotene in the extract increased with SC-CO2 flow rate. Weibull distribution model described adequately the kinetics of extraction of β-carotene from carrots.

Fast analysis of derivatives of polycyclic aromatic hydrocarbons in soil by ultra-high performance supercritical fluid chromatography after supercritical fluid extraction enrichment

An efficient and environment-friendly method for simultaneous determination of 13 typical derivatives of polycyclic aromatic hydrocarbon(PAH)in petroleum-polluted soil with nitro-,oxy-and alkylfunctional group was developed using supercritical fluid extraction(SFE)followed by ultra-high performance supercritical fluid chromatography(UHPSFC).Parameters of UHPSFC,including type of stationary phase and mobile phase modifiers,gradient elution process,backpressure,column temperature,and the flow rate of mobile phase,were systematically optimized,achieving a fast separation within4.2 min.Limits of detection(LOD)were 0.005-0.1μg mL^(-1)or 0.1-2.0 ng g^(-1),respectively,with a good repeatability(RSD<5.0%).Before UHPSFC-PDA analysis,the PAH-derivatives in soil samples were effectively enriched in 15.0 min using SFE with an online carbon nanotubes(CNTs)collection trap.The soil samples were analyzed by the proposed method and the results were verified by GC-MS.Thus,SFE equipped with an online CNTs trap followed by UHPSFC-PDA analysis,which only consumed about2.0 mL organic solvent for a whole run,has been demonstrated to be an efficient way for screening and quantitative analysis of trace-level PAH-derivatives in soil samples.