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.

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.

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.

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.

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.

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.

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 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.

The Analysis of the Equilibrium Cluster Structure in Supercritical Carbon Dioxide

The monomer fraction density based analysis of precise thermophysical data for pure fluids is developed to study the molecular structures in supercritical fluids in general and in CO2 in particular. The series expansion by powers of the monomer fraction density of the potential energy density is used to discover the cluster structure in supercritical fluids and the clusters’ bond energies in CO2. The method of clusters separation between classes of loose and dense clusters in the CO2 supercritical fluid is developed. The method of the energetically averaged number of dense clusters is developed to study the mechanism of the soft structural transition between the gas-like and liquid-like fluids in the supercritical CO2.

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.

Theoretical Studies on Critical Properties of Binary System with Supercritical Carbon Dioxide

A new expression of mixing rule is suggested according to the Mayson′s mixing rule in this paper, which adopts the Redlich Kwong cubic equation of state and the modified Chueh Prausnitz method to calculate the experiment critical points of six binary mixtures CO 2+toluene, CO 2+cyclohexane, CO 2+ n butanal, CO 2+ i butanal , CO 2+methanol, CO 2+ethanol. The coefficients of interaction parameter in the expression of mixing rule were optimized from experimental data. The calculated results of critical temperature and critical pressure meet the experiment data well. The maximum relative errors of temperature and pressure between the calculation results and experiment data are 1 493% and 5 2236% respectively, indicating that the proposed expression of mixing rule is reasonable. This may provide a fundamental method for studying and predicting the properties of supercritical fluids.

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.

Critical temperatures and pressures of reacting mixture in synthesis of dimethyl carbonate with methanol and carbon dioxide

Critical temperatures and pressures of nominal reacting mixture in synthesis of dimethyl carbonate （DMC） from methanol and carbon dioxide （quaternary mixture of carbon dioxide ＋ methanol ＋ water ＋ DMC） were measured using a high-pressure view cell. The results suggested that the critical properties of the reacting mixture depended on the reaction extent as well as its initial composition （initial ratio of carbon dioxide to methanol）. Such information is essential for determining the reaction conditions when one intends to carry out the synthesis of DMC with CO2 and methanol under supercritical conditions.

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.

Research of Supercritical CO2 Fluid Refined Natural Borneol

In this study, with borneol fragments in the crystallized mother liquor of natural borneol used as the raw materials, supercritical carbon dioxide method is adopted for refining to get high purity borneol. The result of the experiment shows that the yield and purity are excellent with an extraction pressure of 11 MPa, an extracting temperature of 40°C, a carbon dioxide flow rate of 25 L·h-1 and an extraction time of 20 minutes. After detected by gas chromatography, the purity of the crystallization products could reach 96%.

Extending Functionality of Microalgae and Transesterification under Supercritical Fluid Conditions

The experimental data on supercritical CO2 extraction of microalgae are presented. It is confirmed that microalgae contains omega-3 fatty acid components. Phase equilibria data are presented for the triolein-methanol (T = 413 K, P = 5.8 - 11.9 MPa) and ethyl eicosapentaenoate-carbon dioxide (T = 313 - 333 K, P = 10 - 21 MPa) binary systems. The scheme of the batch-type experimental setup for supercritical transesterification of oils is presented. Temperature and molar ratio dependences of non-refined palm oil yield to fatty acid methyl esters (FAME) are presented for T = 563 - 693 K, methanol to palm oil molar ratio 39:1. Experiments on ultrasonic emulsification of rapeseed oil-ethanol mixture (molar ratios 150:1 - 7:1) were conducted. Research data on ultrasonic emulsion stability are presented for the time range of 0 - 40 minutes after ultrasonication completion. Correlation is defined between FAME yield of emulsified reaction mixtures and the emulsion grain size. FAME yields are compared for emulsified and non-emulsified reaction mixtures.

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。

超临界二氧化碳介质中晶圆清洗与选择性刻蚀研究进展

随着集成电路特征尺寸的逐渐减小,器件结构会要求更高的纵横比,常规湿法清洗由于表面张力很难进入晶圆深沟槽结构内部,不能满足更细线条工艺要求和高深宽比结构,直接影响沟槽内的污染物去除效果;常规湿法刻蚀各向异性差、结构坍塌严重、深沟槽刻蚀效果不明显;而等离子体干法刻蚀则存在刻蚀速率慢、光刻胶脱落和黏附、结构损伤、废气处理等一系列问题。超临界清洗和刻蚀技术是最具有前景的环境友好、无损伤技术,能够耦合刻蚀、清洗与干燥工艺为一体,且可以循环使用,安全环保,是晶圆制造过程中常规清洗和刻蚀的首选替代技术。综述了超临界二氧化碳中晶圆清洗与选择性刻蚀的研究进展,重点介绍了超临界二氧化碳共溶剂、微乳液体系在光刻胶剥离以及含硅基底选择性蚀刻中的应用,展望了超临界二氧化碳晶圆清洗和刻蚀存在的问题和发展趋势。