Optimization of Supercritical Carbon dioxide Extraction of Ginger Essential Oil by Response Surface Method

[Objective] Ginger essential oil （GEO） is widely used in food production and medical field in recent years due to its prominent biological functions, and this study was conducted to obtain high-quality and high-purity ginger essential oil from the fresh ginger. [Method] GEO was extracted from ginger roots by supercritical fluid extraction （SFE） method. The effects of flow rate of CO2, mesh size of ginger powder and volume of entrainer were investigated by single-factor experiments and response surface method. The content and extraction rate of 6-gingerol represented the extraction index of GEO. [Result] The conditions were optimized as follows： flow rate of CO2 at 25 L/h, mesh size of ginger power of 80 mesh, and volume of anhydrous ethanol as entrainer of 92.46 ml. The optimal extraction rate of 6-gingerol was 3.21%, which was predicted by RSM. [Conclusion] The optimal process of supercritical carbon dioxide extraction of ginger essential oil was identified by singlefactor experiments and response surface method. The present study provides a satisfactory method for purifying GEO from ginger for industrial purpose.

Extraction of Perilla Seed Oil Using Supercritical Carbon Dioxide and GC-MS Analysis

[Objective] This study was aimed to determine the optimal parameters for the extraction of perilla seed oil to obtain high-quality perilla seed oil and analyze its compositions. [Method] In this study, perilla seed oil was extracted using supercritical CO2 （SC-CO2）. The effects of extraction time, temperature and pressure were investigated by single-factor experiments and orthogonal array testing （ORT）. The chemical compositions of extracted perilla seed oil were investigated by GC-MS. [Result] The optimal conditions for the extraction of perilla seed oil using SC-CO2 were extraction time of 4 h, extraction temperature at 40 ℃, and extraction pressure at 23 MPa. Under these conditions, the extraction yield of perilla seed oil was maximized to 12.43%. GC-MS analysis revealed that perilla seed oil was a complex mixture containing 76.183% α-linolenic acid. [Conclusion] Supercritical CO2 extraction was proven to be an effective technology to extract oil from perilla seed, and GCMS was also a satisfactory method for analyzing the compositions of perilla seed oil.

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.

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 Carbon Dioxide Extraction of Andrographolide from Andrographis paniculata： Effect of the Solvent Flow Rate, Pressure, and Temperature

Andrographis paniculata Nees has been extensively used for traditional medicine and help against fever dysentery, diarrhoea, inflammation, and sore throat. In this study, andrographolide, the main component of this plant was extracted from the leaves of A. paniculata using supercritical carbon dioxide. The operating pressures were varied from 7.50 to 20MPa, the temperatures were varied from 30℃ to 60℃, and the flow rates were varied from 0.5 to 4ml.min^-1. The best extraction condition occurred at 10MPa, 40℃, and a flow rate of 2ml.min^-1 for a 3g sample of A. paniculata ground-dried leaves. The measured extraction rate was found to be about 0.0174g of andrographolide per gram of andrographolide present in the leaves per hour of operation. The future studies must focus on the interaction between the various operating parameters such as temperature, pressure, and flow rate of supercritical carbon dioxide.

Kinetics of Reactive Extraction of Nd from Nd2O3 with TBP-HNO3 Complex in Supercritical Carbon Dioxide

The process based on supercritical fluid extraction for reprocessing of the spent nuclear fuel has some remarkable advantages over the plutonium-uranium extraction(PUREX) process.Especially,it can minimize the generation of secondary waste.Dynamic reactive extraction of neodymium oxide(Nd2O3) in supercritical carbon dioxide(SC-CO2) containing tri-n-butyl phosphate-nitric acid(TBP-HNO3) complex was investigated.Temperature showed a positive effect on the extraction efficiency,while pressure showed a negative effect when the unsaturated TBP-HNO3 complex was employed for the dynamic reactive extraction of Nd2O3 in SC-CO2.Both temperature and pressure effects indicated that the kinetic process of the reactive extraction was controlled by the chemical reaction.A kinetic model was proposed to describe the extraction process.

Supercritical Fluid Carbon Dioxide in the Extraction of Lanolin and Its Alcohol

The use of supercritical fluid carbon dioxide (SFCO2) in extraction of lanolin and its alcohol is superior to the conventional solvent extraction method. Its distinctive advantages include high extractive ratio, nontoxic and nonflammable solvents, and minimal by -product pollution. The resulting refined lanolin and its alcohol have light color and little odor, and can be used as raw materials for high grade cosmetic products.

Separation of Molybdenum Isotopes at Supercritical Fluid Extraction with Carbon Dioxide in a Vertical Gradient Field of Temperatures

Separation of molybdenum isotope complexes by supercritical fluid extraction (SFE) with carbon dioxide was studied experimentally. The extraction of molybdenum isotope complexes was carried out in the updated extraction chamber (reactor) of the SFE-U installation, which provided an initial pressure of P ≤ 20 MPa at constant temperatures of the upper T1 = 35°C and bottom T2 = 45°C flanges. The device, through which the eluent was discharged, involved a set of four thin tubes of different lengths located inside the reactor. The axes of the tubes and the reactor are parallel and the tubes are equally spaced circumferentially inside the reactor. The extract was removed from each tube through channels isolated from each other and located in the bottom flange with cylindrical expansion, in which several layers of filter paper were placed. After passing through the filters the extract entered a restrictor designed to remove the eluent from the reactor. The initial pressure of carbon dioxide and the holding time of the extract were specified in the experiments. The level of the eluent sampling was set by the lengths of the tubes depending on the reactor height. A method of producing molybdenum complexes was described. It was experimentally shown that at an initial pressure of 20 MPa and a given holding time a difference from the natural content of Mo isotopes for given heights of extract sampling depending on the reactor height was observed in extracts removed through filters. The ranges of deviation of the content of molybdenum isotopes in extracts from natural one were determined.

Supercritical Carbon Dioxide Extraction of Organic Matter from Petroleum Source Rocksand Its Implications

Organic matter was experimentally extracted by supercritical fiuids （CO2 +1% isopropanol） from petroleum source rocks of different thermo-maturities at different buried depths in the same stratigraphic unit in the Dongying Basin. The results show that supercritical fluid extraction （SFE） is more effective than Soxhlet extraction （SE）, with higher amounts and greater varieties of hydrocarbons and soluble organic matter becoming extractive. The supercritical CO2 extraction is therefore considered more valuable in evaluation of petroleum source rocks and oil resources, particularly those of immature types.

A study of the mechanism of enhancing oil recovery using supercritical carbon dioxide microemulsions

Supercritical carbon dioxide （scCO2） microemulsion was formed by supercritical CO2, H20, sodium bis（2-ethylhexyl） sulfosuccinate （AOT, surfactant） and C2HsOH （co-surfactant） under pressures higher than 8 MPa at 45 ℃. The fundamental characteristics of the scCO2 microemulsion and the minimum miscibility pressure （MMP） with Daqing oil were investigated with a high-pressure falling sphere viscometer, a high-pressure interfacial tension meter, a PVT cell and a slim tube test. The mechanism of the scCO2 microemulsion for enhancing oil recovery is discussed. The results showed that the viscosity and density of the scCO2 microemulsion were higher than those of the scCO2 fluid at the same pressure and temperature. The results of interfacial tension and slim tube tests indicated that the MMP of the scCO2 microemulsion and crude oil was lower than that of the scCO2 and crude oil at 45 ℃. It is the combined action of viscosity, density and MMP which made the oil recovery efficiency of the scCO2 microemulsion higher than that of the scCO2 fluid.

Solubility of red palm oil in supercritical carbon dioxide： Measurement and modelling

The solubility of red palm oil （RPO） in supercritical carbon dioxide （scCO2） was determined using a dynamic method at 8.5-25 MPa and, 313.15-333.15 K and at a fixed scCO2 flow rate of 2.9 g. mn -1 using a full factorial design. The solubility was determined under low pressures and temperatures as a preliminary study for RPO par- ticle formation using scCO2. The solubility of RPO was 0.5-11.3 mg. （g CO2） -1 and was significantly affected by the pressure and temperature. RPO solubility increased with pressure and decreased with temperature. The Adachi-Lu model showed the best-fit for RPO solubility data with an average relative deviation of 14% with a high coefficient of determination, R2 of 0.9667, whereas the Peng-Robinson equation of state thermodynamic model recorded deviations of 17%-30%.

Supercritical Equilibrium Data of the Systems Carbon Dioxide—Linalool and Carbon Dioxide—Orange Essential Oil

In this paper experimental equilibrium data on the system supercritical CO2-orange essential oil and the system supercritical CO2-linalool are reported at 323.15 K and 343.15 K, for pressures in the ranges of 7.6-13.5 MPa. The behavior of the system supercritical CO2-orange essential oil was represented by means of thermodynamic model, based on Peng-Robinson equation of state. To this aim the orange essential oil was represented by a mixture of limonene, linalool and β-caryophyllene, selected to represent the classes of monoterpenes, oxygenated terpenes and sesquiterpenes respectively. The model uses only regression parameters calculated from binary sub-systems, CO2-limonene and CO2-β-caryophyllene (taken from literature) and CO2-linalool (calculated from the fitting of original data reported in the present work) thus being predictive with respect to the multicomponent mixture.

A simulation of citrus oil adsorption separation in the supercritical carbon dioxide

Aspen Adsim was used to simulate the fractionation of citrus oil with extraction and adsorption combined method in supercritical carbon dioxide.The dynamic behavior in a isothemal and adiabatic bed could be described succesfully,and the simulation results agreed with the experimental data.The effect of adsorption time,the flow rate of feed on the concentration of components in product and the recovery were studied.The amount of loading composition on the adsorbents changed with adsorption time and axial distance of bed was also investigated.

Separation of Biomass Pyrolysis Oil by Supercritical CO2 Extraction

Supercritical CO2 extraction was employed to separate simulated and real bio-oils. Effects of extraction pressure, temperature and adsorbents on distribution coefficient (or enrichment coefficient) of five representative compounds were investigated using a simulated bio-oil, which was composed of acetic acid (AC), propanoic acid (PA), furfural (FR), acetylacetone (AA) and 2-methoxyphenol (MP). The distribution coefficients of AA, FR and MP between super-critical CO2 phase and liquid phase were bigger than 1.5, while those of AC and PA characteristic of relatively strong polarity were less than 1. Temperature and pressure also had impacts on the distribution coefficients of AA, FR and MP, especially remarkable for AA. The extraction of simulated bio-oil spiked on three adsorbents shows that adsorbents influence extraction efficiency and selectivity by changing intermolecular forces. High extraction pressure and relative low temperature are beneficial to reduce the water content in the extract. In addition, the feasibility of supercritical CO2 extraction of real bio-oil was examined. After extraction in the extraction fraction total ketones increased from 14.1% to 21.15~25.40%, phenols from 10.74% to 31.32~41.25%, and aldehydes from 1.92% to 3.95~8.46%, while the acids significantly dropped from 28.15% to 6.92~12.32%, and water from 35.90% to 6.64~4.90%. In view of extraction efficiency, the optimal extraction temperature was determined to be 55℃. Extraction efficiency of the real bio-oil increased with rising pressure. The maximal extraction efficiency of real bio-oil on water-free basis could reach to 88.6%. After scCO2 extraction, the calorific value and stability of the extract fraction evidently increased and the acidity slight decreased with nearly 100% volatility below 140℃, suggesting potentially applicable as substitute for engine fuel.

Supercritical carbon dioxide extraction of CLA-ethyl ester

Supercritical carbon dioxide(SC-CO_(2))extraction of Conjugated linoleic acid(CLA)ethyl ester was investigated at pressures in the range of 9 to 10.5 MPa and temperature gradients ranging from 0℃ to 21℃.The content of CLA-ethyl ester in the fraction was analyzed with gas chromatography(GC).The experimental results indicated that the rate of extraction would rise with the increase of pressure when temperature gradient was given.Moreover,the extraction pressure had insignificant influence on the selectivity of CLA-ethyl ester in SCCO_(2).When pressure was fixed,setting certain temperature gradient can improve the selectivity of CLA-ethyl ester in SC-CO_(2),and CLA-ethyl ester can be concentrated more effectively than without a temperature gradient.The acid value and peroxide value of the fractions were reduced obviously,compared to the raw material.The optimal condition is pressure at 10 MPa and temperature gradient at 11℃.

Essential Oil from Inula britannica Extraction with SF-CO_2 and Its Antifungal Activity

The aim of this study was to determine the extraction technique of supercritical fluid carbon dioxide（SF-CO 2） for the essential oil from Inula britannica flowers and its antifungal activities against plant pathogenic fungi for its potential application as botanical fungicide.The effects of factors,including extraction temperature,extraction pressure,SF-CO 2 flow rate,flower powder size,and time on the essential oil yield were studied using the single factor experiment.An orthogonal experiment was conducted to determine the best operating conditions for the maximum extraction oil yield.Adopting the optimum conditions,the maximum yield reached 10.01% at 40°C temperature,30 MPa pressure,60 mesh flower powder size,20 L h-1SF-CO 2 flow rate,and 90 min extraction time.The antifungal activities of I.britannica essential oil using the SF-CO 2 against the most important plant pathogenic fungi were also examined through in vitro and in vivo tests.Sixteen plant pathogenic fungi were inhibited to varying degrees at 1 mg mL-1concentration of the essential oil.The mycelial growth of Gaeumannomyces graminis var.tritici was completely inhibited.The radial growths of Phytophthora capsici and Fusarium monilifome were also inhibited by 83.76 and 64.69%,respectively.In addition,the essential oil can inhibit the spore germination of Fusarium oxysporum f.sp.vasinfectum,Phytophthora capsici,Colletotrichum orbiculare,and Pyricularia grisea,and the corresponding inhibition rates were 98.26,96.54,87.89,and 87.35% respectively.The present study has demonstrated that the essential oil of I.britannica flowers extracted through the SF-CO 2 technique is one potential and promising antifungal agent that can be used as botanical fungicide to protect crops.

An extraction-assay system： Evaluation on flavonols in plant resistance to Pb and Cd by supercritical extraction-gas chromatography

In this research, supercritical carbon dioxide extraction （SFE） showed better extraction etlect when compared with Solid- liquid extraction （SLE）, Soxhlet extraction （SEt and Ultrasonic extraction （UE）, not only in the rate but also the time. The comparison among these three extraction modifiers, including acetone, ethanol and methanol demonstrated that ethanol was preferred to SFE due to its high extraction effect and low toxicology. In addition, parameter of SFE, influence of temperature and pressure were investigated, and the best extraction effect was achieved at the optima conditions, temperature of 40℃ and the pressure of 35 MPa. Thus, SFE is a highly effective method for flavonols extraction, requiring minimum energy and producing non-toxic byproduct. SFE-GC system is applied for the evaluation on flavonols that plays a key role in plant resistance to heavy metal, with its content and synthetase gene expression significantly increasing in plant when threatened by heavy metal. Besides, results indicated that flavonols can improve plant resistance to oxidative stress by quenching the redundant ROS in matrix.

The Solubility of Styrene from Polystyrene in Supercritical CO_2

The solubility of styrene from polystyrene in supercritical carbon dioxide is measuredat 323 K,333 K,and 343 K in the pressure range from 12 to 28 MPa.Based on the associationconcept and the theory of dense gas sorption in polymers,a displacement and association mechanismon supercritical fluid extraction of the monomer from the polymer is proposed.And,a novel math-ematical model for correlating the solubility data obtained from the experiments is also proposed inthe paper.

超临界二氧化碳与页岩相互作用机制

超临界二氧化碳与页岩相互作用机制及规律对页岩油气开发非常重要。目前缺少对超临界二氧化碳注入页岩储层后页岩润湿性、孔隙度和渗透率变化规律的研究。为了明确在不同条件下经过超临界二氧化碳浸泡处理后页岩矿物成分和微观结构的变化规律,以四川盆地龙马溪地区页岩为研究对象,对其总有机碳含量、矿物成分、表面形貌及低压N2和CO_(2) 吸附进行了测试。通过对不同浸泡时间、压力和含水条件下页岩处理前、后的物理性质和微观结构进行定量表征,研究了超临界二氧化碳对页岩孔隙度、渗透率以及润湿性的影响。研究结果表明:①随着浸泡时间和浸泡压力的增加,页岩中的黏土矿物和碳酸盐矿物(方解石和白云石)含量降低,石英含量增加,有机质含量降低明显。②扫描电镜图像显示页岩中微观孔隙结构变化受萃取作用、溶蚀作用和吸附膨胀作用共同影响。页岩中微观孔隙结构的变化导致了页岩孔隙度和渗透率的改变。页岩渗透率变化受到黏土矿物、碳酸盐矿物和有机质含量的影响。③超临界二氧化碳浸泡处理后页岩的润湿性发生改变,随着浸泡时间和压力的增加,页岩-水接触角增大,页岩的润湿性由强水湿转变为弱水湿和中等润湿。