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.

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.

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.

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.

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.

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.

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.

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.

超临界二氧化碳萃取元宝枫籽油工艺优化

为了得到品质优良的元宝枫籽油产品,采用超临界二氧化碳萃取元宝枫籽油,以油脂萃取率为指标,通过单因素试验和响应面试验优化工艺条件,并对所得元宝枫籽油的脂肪酸组成、理化指标、甾醇和生育酚含量进行分析。结果表明:超临界二氧化碳萃取元宝枫籽油的最优工艺条件为原料粒度380~830μm(20~40目)、二氧化碳流量28 L/h、萃取温度37℃、萃取压力44 MPa、萃取时间100 min,在该条件下油脂萃取率达(98.7±0.2)%;元宝枫籽油中神经酸含量高达9.34%,总不饱和脂肪酸含量为86.7%,各项理化指标均符合相关标准,总甾醇和总生育酚含量分别为988.1μg/g和991.4μg/g,综合品质优于正己烷萃取和低温压榨制取的油脂。综上,超临界二氧化碳萃取元宝枫籽油的萃取率高,产品品质优良,是一种绿色、高效的提油技术。

基于响应曲面法的超临界CO_(2)萃取油基钻屑油相工艺优化

目的对超临界CO_(2)萃取油基钻屑中油相工艺参数进行优化。方法采用响应曲面法对影响超临界CO_(2)萃取工艺的重要参数进行具体实验并根据实验结果进行数值模拟,通过模拟得出萃取时间、压力、温度和超临界CO_(2)流量等参数的优化数据。结果响应曲面分析了各变量之间对萃取效果的影响,基于萃取数据建立了二次多项式模型,能够较好地拟合实验结果,得出最佳萃取条件为萃取压力25 MPa、温度323.15 K、时间90 min和流量25.0 L/h。结论通过具体实验数据结合响应曲面法得出了最佳萃取条件,在该条件下油类最大去除率为95.22%。利用气相色谱仪-质谱联用仪(GC-MS)分析萃取物前后性状未发生明显变化,该方法能够更好地实现固液分离和资源回收。

二氧化碳压裂技术研究进展

水力压裂开发非常规油气存在用水量大、引发储层伤害和污染地下水等问题。二氧化碳压裂技术因拥有造缝范围广、裂缝复杂、增产效果好、对地下水污染小、返排速率快等优势,且响应国家“双碳政策”要求,正逐渐成为非常规油气资源开发的热点。本文调研了国内外二氧化碳压裂技术发展历史及二氧化碳干法压裂、二氧化碳泡沫压裂、超临界二氧化碳压裂三类基本二氧化碳压裂技术,总结了二氧化碳压裂技术的基本工艺流程、增产原理、技术特点并介绍了近年来改进的二氧化碳压裂新方法和增产效果,为今后二氧化碳压裂技术的深入研究和现场应用提供一定的借鉴意义,有利于我国“双碳”目标的实现。

超临界二氧化碳混相驱油机理实验研究

根据大庆榆树林油田原油组分变化、CO2与原油界面张力关系及CO2超临界性质,对CO2混相驱地层情况进行了模拟研究,建立了CO2混相驱驱替模型和方程。研究结果表明,超临界状态的CO2可以降低所波及油水的界面张力;混相时混相带原油含碳组分中C20以下的含量达到了最高值;水气交替注入时,水对混相有不利的影响。

利用SFE-MD技术分离提纯玫瑰精油及其成分分析

用超临界CO2流体萃取技术（SFE）萃取平阴玫瑰浸膏,用分子蒸馏技术（MD）进行精制,所得玫瑰精油呈淡黄色,质量标准达到FCC（2004）,得率由传统水蒸气蒸馏法的0.03%提高到0.1%.超临界CO2流体萃取最佳工艺条件为：萃取压力25 MPa,温度50 ℃,CO2流量25 kg/h,萃取时间2.5 h;分子蒸馏温度为80～120 ℃;所得精油GC-MS分析,检测出63种成分,主体呈香成分为酯类物质,质量分数超过50%,相对分子质量主要集中在200～250.

超临界二氧化碳萃取葡萄籽油的研究

葡萄籽油中富含亚油酸和其它不饱和脂肪酸,具有较高的食用和药用价值。传统的葡萄籽油提取方法存在着收率低和溶剂残留的问题。今基于对酿酒过程中废弃葡萄籽的开发利用,探讨了采用绿色洁净分离技术——超临界流体萃取技术从废弃葡萄籽中萃取葡萄籽油的可行性,重点考察了萃取温度、萃取压力、CO2用量及不同原料对葡萄籽油产率的影响。研究表明萃取压力对产率的影响较温度显著,实验确定适宜工艺条件为萃取温度55C,萃取压力30MPa。此条件下以张裕酒厂提供的籽为原料所得产率为9.71%,同时气相色谱分析表明,葡萄籽油产品中含有72.05%的亚油酸。另外,分别以三种不同来源的葡萄籽为原料进行实验,研究显示,葡萄籽油产率随原料不同而存在一定差异,产率较高者可达13.51%。

超临界CO_2萃取-分子蒸馏对白术挥发油的提取分离和GC-MS分析

用超临界CO2 萃取技术提取白术挥发油 ,然后用分子蒸馏对所得的萃取物进行精分离 ,得到蒸出物 ;超临界萃取物收率为2.42 % (w) ,分子蒸馏蒸出物收率26.3% (w) ;对超临界萃取物和分子蒸馏蒸出物分别进行GC -MS分析 ,结果超临界萃取物检测出33个化合物 ,分子蒸馏蒸出物检测出27个化合物 ,主要成分均为2,7_二甲氧基_3,6_二甲基萘、γ_芹子烯、大根香叶烯等 。

玉米胚芽油的超临界CO_2萃取

研究了超临界CO2 流体萃取玉米胚芽油的条件 ,着重研究了萃取压力、温度、萃取时间和CO2 流量对油脂萃取率的影响 ,优化了萃取工艺条件 ;萃取压力 35Mpa ,温度 50℃ ,时间 3h ,CO2 流量 34kg/h ,并利用GC/MS分析了最佳条件下萃取的玉米胚芽油成分组成。并比较了超临界CO2

微波和超临界CO_2萃取杜仲籽油工艺研究

通过微波萃取和超临界CO2萃取杜仲籽油的正交试验,考察影响萃取效果的主要因素,寻求最佳萃取工艺条件。微波萃取最佳工艺条件为:以环己烷为萃取剂,原料粉碎度40目,溶剂与物料质量比值为5.0,微波功率700W,每次微波辐射时间50s,微波累计辐射8次,在此条件下油脂得率为27.07%。超临界CO2萃取的最佳工艺条件为:萃取压力35MPa、萃取温度45℃、萃取时间70min、分离温度30℃、CO2流量25～30kg/h,原料粉碎度40目,在此条件下油脂得率27.76%。并比较不同提取方法对油脂得率和油脂品质的影响。结果表明,微波萃取所需时间最短,油脂得率较高;超临界CO2萃取所得杜仲籽油的品质最优,是提取优质杜仲籽油的首选方法。

超临界CO_2萃取芹菜籽油研究

用超临界ＣＯ２萃取技术对广东白芹菜籽进行了萃取研究。结果表明，萃取压力低于１５ＭＰａ时，较重的油树脂等成分难以被萃取出来；萃取温度为３０８Ｋ时对萃取最有利；解析温度对萃取效率影响较小；ＣＯ２流量对萃取效率的影响比床层高度引起的扩散阻力的影响大得多。超临界ＣＯ２萃取所得芹菜籽油品质优越，且其中的药用有效成分（３－正丁基－４，５－二氢苯并呋喃酮）含量比水汽法所得芹菜籽油的高五倍多。