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.

Study on Extraction of Effective Aroma Components from Formula Tobacco by the Supercritical CO2 Extraction Method and Its Aroma Composition

[Objectives]This study was conducted to improve the sensory quality and industrial availability of tobacco extracts.[Methods]The L9(34)design was adopted to carried out an extraction experiment,in which formula tobacco was extracted using supercritical CO2,and the extract was concentrated by vacuum distillation.Through sensory evaluation and chemical analysis,the function determination and chemical composition analysis of the tobacco extracts were carried out,and the optimal supercritical fluid extraction process was finally determined.[Results]The obtained optimal supercritical fluid extraction conditions were as follows:extraction temperature 55℃,extraction pressure 25 MPa,CO2 flow rate of 20 L/h,and entrainer of 95%ethanol.The tobacco extract obtained under the optimal conditions endowed the cigarettes with full and delicate aroma,less irritation and clean aftertaste and made the flavor of the cigarettes overall coordinated and softer,so the sensory quality was significantly improved.[Conclusions]The tobacco extract obtained by the supercritical CO2 extraction method from formula tobacco can effectively improve the quality of cigarettes.

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 betulin from bark of Betula platyphylla by supercritical carbon dioxide extraction

Betulin, which is a medicinal pentacyclic triterpene, is abundant in the bark of white birch (Betula platyphlly). The bark of birch was collected at Tayuan Forest Farm of Jiagedaqi, Heilongjiang Province in September 2000. Supercritical fluid extraction (SFE) that is a new separation technology has been used for the processing pharmaceutical and natural products. In this paper, the extraction of betulin from the bark of birch by supercritical CO2 extraction was studied. The authors investigated and analyzed a few parameters such as modifier dosage, extraction pressure and extraction temperature. The optimal extrac-tion conditions showed that the modifier dosage used for per gram bark powder was 1.5 mL, the extraction pressure was at 20 Mpa, and the extraction temperature was at 55 C. The velocity of flow of liquid CO2 was at 10 kg/h. The pressure and tem-perature in separation vessel were at 5.5 Mpa and 50 C, respectively.

A Comparative Study on Chemical Composition of Supercritical CO_2 Extraction Products in Peels of Trichosanthes kirilowii Maxim. from Changqing District

[Objective] This study aimed to investigate the differences in chemical composition of supercritical CO2 extraction products in peels of Trichosanthes kirilowii Maxim. from Changqing district. [Method] Supercritical fluidextraction （SFE） and GCMS method were applied to determine and analyze the chemical components of the extracts in peels of three strains of Trichosanthes kirilowii Maxim. [Result] The chemical components of supercritical CO2 extraction products in peels of three strains of Trichosanthes kirilowii Maxim. varied., and the number of chemical components with normalized percentage content higher than 1% was 5, 7 and 8, respectively. There are 14 kinds of common components, and the relative content of hexadecanoic acid was the highest. [Conclusion] Supercritical CO2 extracts in peels of different strains of Trichosanthes kirilowii Maxim. contain different chemical components, providing scientific basis for breeding excellent varieties and the development and utilization of Trichosanthes kirilowii Maxim.

Effect of Allelochemicals of Chinese-fir root extracted by supercritical CO_2 extraction on Chinese fir

Allelochemicals of Chinese-fir root was extracted by technology ofsupercritical CO_2 extraction under orthogonal experiment design, and it was used to analyzeallelopathic activity of Chinese-fir through bioassay of seed germination. The results showed thatas to the available rate of allelochemicals, the pressure and temperature of extraction were themost important factors. The allelochemicals of Chinese-fir root extracted by pure CO_2 and ethanolmixed with CO_2 have different allelopathic activities to seed germination, and the allelochemicalsextracted by ethanol mixed with CO_2 had stronger inhibitory effects on seed germination than thatextracted by pure CO_2.

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.

Comparison of Constituents and Insecticidal Activities of Essential Oil from Artemisia lavandulaefolia by Steam Distillation and Supercritical-CO_2 Fluid Extraction

Essential oil was extracted from Artemisia lavandulaefolia DC.by steam distillation（SD） and supercritical-CO2 fluid extraction（SFE）,respectively.The constituents of the essentil oils extracted with those two methods were analyzed by gas chromatography-mass spectrometry（GC-MS） and insecticidal activities of the essential oils were evaluated,then the results were compared to assess their biological activity.Thirty-one compounds were identified in the essential oil extracted by SD,and its main components were eucalyptol,α,α,4-trimethyl-3-cyclohexene-1-methanol and so on.Twenty-two compounds were identified for the essential oil extracted by SFE,and its main components were cyclodecene,n-hexadecanoic acid and so on.Six chemical compositions were all contained in the essential oils extracted by the two methods,i.e.,eucalyptol,α,α,4-trimethyl-3-cyclohexene-1-methanol,caryophyllene,[3aS-（3aα,3bβ,4β,7α,7aS）]-octahydro-7-methyl-3-methylene-4-（1-methylethyl）-1H-cyclopenta[1,3]cyclopropa-[1,2]benzene,nerolidol and（-）-Spathulenol.The fumigation toxicity of the essential oil obtained by means of SD to the adults of Sitophilus zeamais is significantly higher than that of the essential oil by means of SFE.The contact toxicity of the essential oil obtained by means of SFE to the adults of S.zeamais is higher than that of the essential oil obtained by means of SD,but the difference is not significant.

Experimental and Simulating Study of Supercritical CO_2 Extraction of Ginger Essential Oil

An experimental setup for separating ginger essential oil by supercritical fluid extraction is established. The effects of the extraction pressure, temperature, CO2 flow rate and particle size of raw material on the extraction rate are investigated, and the optimum process conditions of supercritical CO2 extraction are determined. A mathematical simulation model is established based on the mass conservation in differential units of extraction bed. The total mass transfer driving force and the equilibrium absorption constant are evaluated by the linear driving force theory. The results from numerical simulation agree well with the experimental data.

Combination of Supercritical Fluid Extraction with Ultrasonic Extraction for Obtaining Sex Hormones and IGF-1 from Antler Velvet

Supercritical CO2 (SC-CO2) extraction technology and ultrasonic technology were used to extract two active sex hormones, estradiol and progesterone, and insulin-like growth factor-1 (IGF-1) from antler velvet. The effects of SC-CO2 extraction condition on the extraction yield and content of sex hormones, the ultrasonic extrac-tion condition on the content of IGF-1 and the SC-CO2 extraction condition on the activity remaining of IGF-1 were studied. The optimal conditions were obtained. The experimental results showed that, in presence of 75% ethanol as the co-solvent, the mean yield and content of estradiol and progesterone were 87.67 pg·g-1 and 1224.10 pg·g-1, 12.38 ng·g-1 and 354.06 ng·g-1, respectively, with extraction pressure of 30 MPa, temperature of 35°C, extraction time of 30 min and CO2 consumption of 15 L·g-1 at the flow rate of 2.0 L·min-1. The highest content of IGF-1 was 7425.75 ng·g-1 antler velvet residue, when the pH10 ammonia-ammonium chloride buffer solution was used as the solvent, the ratio of solvent to sample was 20/1 (volume/mass), the extraction temperature was 0-35°C, and the ex-traction time was 4×15 min. Under these conditions, 93.68% activity remaining of IGF-1 in the residue was ob-tained, while little IGF-1 activity exists in traditional residue. The experimental results indicate that the technology of SC-CO2 with co-solvent is of advantage for getting high content sexual hormones and keeping high activity of IGF-1 in the residue, which can not be achieved by traditional extraction methods.

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.

Effect of Allelochemicals of Chinese-fir root extracted by supercritical CO2 extraction on Chinese fir

Allelochemicals of Chinese-fir root was extracted by technology of supercritical CO2 extraction under orthogonal experiment design, and it was used to analyze allelopathic activity of Chinese-fir through bioassay of seed germination. The results showed that as to the available rate of allelochemicals, the pressure and temperature of extraction were the most important factors. The allelochemicals of Chinese-fir root extracted by pure CO2 and ethanol mixed with CO2 have different allelopathic activities to seed germination, and the allelochemicals extracted by ethanol mixed with CO2 had stronger inhibitory effects on seed germination than that extracted by pure CO2.

Application of Supercritical CO2 Gas Turbine for the Fossil Fired Thermal Plant

A supercritical CO2 gas turbine cycle can produce power at high efficiency and the gas turbine is compact compared with the steam turbine. Therefore, it is very advantageous power cycle for the medium temperature range less than 650 ℃. The purpose of this paper is to show how it can be effectively applied not only to the nuclear power but also to the fossil fired power plant. A design of 300 MWe plant has been carried out, where thermal energy of flue gas leaving a CO2 heater is utilized effectively by means of economizer and a high cycle thermal efficiency of 43.4 % has been achieved. Since the temperature and the pressure difference of the CO2 heater are very high, the structural design becomes very difficult. It is revealed that this problem can be effectively solved by introducing a double expansion turbine cycle. The component designs of the CO2 heater, the economizer, supercritical CO2 turbines, compressors and the recuperators are given and it is shown that these components have good performances and compact sizes.

Extraction of Heavy Metals from Solid Material by Supercritical CO_2

Extraction of heavy metal ions from solid matrix by means of an incorporation of chelating agents with supercritical carbon dioxide（scCO2） was investigated experimentally. Four commercially available chelating agents, diethylammonium diethyldithiocarbamate（Et2NH2DDC）, trifluoroacetylacetone（TFA）, hexafluoroacetylacetone（HFA） and thenoyltrifluoroacetone（TTA） were tested. The extraction experiments were conducted at 50 °C and 1.39×107― 2.80×107 Pa. According to the experimental results, for the extraction of Cu2＋, all the chelating agents investigated here are effective. For other metal ions, such as Pb2＋, Ni2＋ and Cd2＋, Et2NH2DDC exhibited a better extraction result, while other chelating agents were less effective. This investigation is expected to provide a tentative evaluation on the scCO2-based metal extraction from solid media.

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%).

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.

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.

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.

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.