Journal of Supercritical Fluids最新文献

英文中文

Sequential high-pressure extraction using green solvents to recover bioactive compounds from sesame cake 使用绿色溶剂进行顺序高压萃取，从芝麻饼中回收生物活性化合物

IF 3.4 3区工程技术 Q2 CHEMISTRY, PHYSICAL

Journal of Supercritical Fluids

Pub Date : 2024-09-30 DOI: 10.1016/j.supflu.2024.106421

Marta Alessandra de Avila Souza , Adenilson Renato Rudke , Amanda Tavares Germano , Luciano Vitali , Sandra Regina Salvador Ferreira

Sesame cake was submitted to pressurized liquid extraction (PLE) for process optimization. Then, supercritical fluid extraction (SFE), followed by optimized PLE were applied to recover the oily fraction and the polar extract, respectively. PLE samples, at optimized condition and from SFE deffated cake, showed high levels of TPC (33.15 and 31.86 mg GAE/g), DPPH (97.64 and 94.38 µmol TE/g), FRAP (46.12 and 46.69 mg TEg), flavonoids (2.26 and 2.31mgQE/g extract), yield (13.76 and 16.25 %) and protein (56.52 and 54.08 mg BSA/g), respectively. The oily fraction presented high levels of carotenoids and essential fatty acids, while PLE extracts presented higher concentration of ferulic acid, 4-aminobenzoic acid, and quercetin compared to Soxhlet extract. Total Reduced Sugar (TRS) content suggests sesame cake as good biomass for bioethanol production. The sequential process (SFE + PLE) was efficient to recover two bioactive fractions from sesame cake, contributing to improve the value of this co-product.

芝麻饼经过加压液体萃取（PLE）进行工艺优化。然后，采用超临界流体萃取（SFE）和优化的 PLE 分别回收油性馏分和极性提取物。优化条件下的 PLE 样品和从 SFE 脱脂饼中提取的 PLE 样品分别显示出较高的 TPC（33.15 和 31.86 mg GAE/g）、DPPH（97.64 和 94.38 µmol TE/g）、FRAP（46.12 和 46.69 mg TE/g）、类黄酮（2.26 和 2.31mgQE/g 提取物）、产量（13.76 和 16.25 %）和蛋白质（56.52 和 54.08 mg BSA/g）水平。与索氏提取物相比，油性提取物中类胡萝卜素和必需脂肪酸含量较高，而 PLE 提取物中阿魏酸、4-氨基苯甲酸和槲皮素含量较高。总还原糖（TRS）含量表明芝麻饼是生产生物乙醇的良好生物质。连续工艺（SFE + PLE）能有效地从芝麻饼中回收两种生物活性馏分，有助于提高这种副产品的价值。

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引用次数: 0

Aqueous-organic and aqueous-vapor interfacial phenomena for three phase systems containing CO2, CH4, n-butanol, n-dodecane and H2O at saturation conditions 饱和状态下含 CO2、CH4、正丁醇、正十二烷和 H2O 的三相体系的水-有机和水-蒸汽界面现象

IF 3.4 3区工程技术 Q2 CHEMISTRY, PHYSICAL

Journal of Supercritical Fluids

Pub Date : 2024-09-30 DOI: 10.1016/j.supflu.2024.106420

R. Villablanca-Ahues , R. Nagl , T. Zeiner , P. Jaeger

A fundamental understanding of the interfacial properties at elevated pressure is essential for processes in the context of the energy transition, such as the storage of CO₂, H₂ or CH₄. Systems in such processes have traces of impurities. This work aims to systematically investigate these multi-component systems through simplified vapor-liquid-liquid systems comprising H₂O, (n-butanol or n-dodecane), and (CO₂ or CH₄). The model systems are theoretically investigated using the density gradient theory and the PCP-SAFT. The interfacial tension and saturated phase density of the model systems are experimentally measured by the pendant drop and the oscillating tube method, respectively. Good agreement between the theoretical and experimental results is found. It was found that the pure and binary systems of these mixtures can be described well by the introduced model, delivering high quality predictions.

从根本上了解高压下的界面特性对于能源转型过程（如二氧化碳、H2 或 CH4 的储存）至关重要。这些过程中的系统都含有微量杂质。这项研究旨在通过由 H2O、（正丁醇或正十二烷）和（CO2 或 CH4）组成的简化汽-液-液系统，系统地研究这些多组分系统。利用密度梯度理论和 PCP-SAFT 对模型体系进行了理论研究。通过垂滴法和振荡管法分别对模型体系的界面张力和饱和相密度进行了实验测量。结果表明，理论和实验结果之间具有良好的一致性。研究发现，引入的模型可以很好地描述这些混合物的纯系统和二元系统，并提供高质量的预测结果。

引用次数: 0

Supercritical CO2 impregnation of pink pepper essential oil in gelatin-siloxane cryogel for biomedical applications 超临界二氧化碳浸渍粉红胡椒精油在明胶-硅氧烷低温凝胶中的生物医学应用

IF 3.4 3区工程技术 Q2 CHEMISTRY, PHYSICAL

Journal of Supercritical Fluids

Pub Date : 2024-09-30 DOI: 10.1016/j.supflu.2024.106419

Ulisses Silva do Nascimento , Thayná dos Santos Borges , Carolina Kafka Neves , Ariane Moracci Yoshitake , Elisete Vieira do Nascimento , Christiane Bertachini Lombello , Bruno Guzzo da Silva , Lígia Passos Maia-Obi

The supercritical CO₂ impregnation of pink pepper essential oil (EO) can bring its bioactive properties to a biomaterial in a green approach, making it multifunctional. Aiming to obtain a gelatin-siloxane cryogel loaded with pink pepper EO for biomedical applications and to understand the impact of the impregnation conditions, gelatin was crosslinked with (3-glycidoxypropyl)trimethoxysilane and lyophilized, and the impregnation was studied using a design of experiments with conditions from 10 to 30 MPa and 35–60 °C. The cryogel synthesis was confirmed by FTIR, %gel and TGA. Its biocompatibility was demonstrated through SEM, water uptake and cytotoxicity studies. It was shown that, due to the influence on the solubility of the EO in scCO₂, varying pressure and temperature influences the impregnation, which showed {20 MPa; 35 °C} as its best condition. Therefore, a cryogel suitable for implantation with potential to reduce side effects related with infection and inflammation was obtained.

对粉红胡椒精油（EO）进行超临界二氧化碳浸渍可将其生物活性特性以绿色方法注入生物材料，使其具有多功能性。为了获得负载粉红胡椒精油的明胶-硅氧烷低温凝胶用于生物医学应用，并了解浸渍条件的影响，研究人员用（3-缩水甘油氧丙基）三甲氧基硅烷交联明胶并将其冻干，然后在 10 至 30 兆帕和 35 至 60 °C的条件下采用实验设计法研究了浸渍过程。傅立叶变换红外光谱（FTIR）、凝胶百分比（%gel）和热重分析（TGA）证实了冷冻凝胶的合成。通过扫描电子显微镜、吸水率和细胞毒性研究证明了其生物相容性。研究表明，由于环氧乙烷在 scCO2 中的溶解度会受到影响，因此不同的压力和温度会影响浸渍效果。因此，我们获得了一种适合植入的低温凝胶，它有可能减少与感染和炎症有关的副作用。

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引用次数: 0

Evaluation of the reaction order and kinetic modeling of Domanic oil shale upgrading at supercritical water conditions 超临界水条件下多曼尼克油页岩升级反应顺序和动力学模型评估

IF 3.4 3区工程技术 Q2 CHEMISTRY, PHYSICAL

Journal of Supercritical Fluids

Pub Date : 2024-09-29 DOI: 10.1016/j.supflu.2024.106418

Guillermo Félix , Richard Djimasbe , Alexis Tirado , Mikhail A. Varfolomeev , Jorge Ancheyta

Two different kinetic models were developed for the kinetic study of Domanic oil shale conversion in the supercritical water. The oil shale reaction order was evaluated with a three-lump reaction scheme taking into account oil shale, gases, and synthetic oil. Contrary to the commonly reported first-order, it was found that a higher order (2.5) is more suitable for the conversion of oil shale at supercritical water conditions. The main reaction mechanism and predictions were obtained using a more detailed reaction network (five-lump model), which precisely estimates the experimental yield of all compounds contemplated. The statistical analysis suggested that the estimated kinetic parameters were suitably optimized, as well as the sensitivity analysis confirmed that these are the optimal values. The conversion of organic matter into gas and coke through free radical reactions exhibits larger rates using supercritical water. Low temperature (380 °C) and short reaction times favor the yield of synthetic oil because when these conditions are exceeded secondary cracking reactions provoke the generation of gases. Gas production is mainly carried out by the conversion of organic matter for brief reaction times and the transformation of carbonates for extended periods.

针对超临界水中多曼尼克油页岩转化的动力学研究，开发了两种不同的动力学模型。在考虑到油页岩、气体和合成油的三块反应方案下，对油页岩反应阶数进行了评估。与通常报告的一阶相反，研究发现高阶（2.5）更适合油页岩在超临界水条件下的转化。使用更详细的反应网络（五块模型）获得了主要反应机理和预测结果，该网络可精确估算所有预期化合物的实验产率。统计分析表明，估计的动力学参数经过适当优化，敏感性分析也证实这些参数是最佳值。使用超临界水，通过自由基反应将有机物转化为气体和焦炭的速率更高。低温（380 °C）和短反应时间有利于合成油的产出，因为当超过这些条件时，二次裂解反应会引发气体的产生。气体的产生主要是通过有机物的转化（反应时间短）和碳酸盐的转化（反应时间长）进行的。

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引用次数: 0

Influence of solvent selection and RESS processing conditions on formation of a praziquantel-malonic acid cocrystal in supercritical CO2 溶剂选择和 RESS 处理条件对在超临界二氧化碳中形成吡喹酮-丙二酸共晶体的影响

IF 3.4 3区工程技术 Q2 CHEMISTRY, PHYSICAL

Journal of Supercritical Fluids

Pub Date : 2024-09-29 DOI: 10.1016/j.supflu.2024.106417

Lauren A. MacEachern , Grace O’Connor , Jamileh Shojaeiarani , Mahmoud Mirmehrabi , Azadeh Kermanshahi-pour

Praziquantel (PZQ) is an anthelmintic drug with low solubility, therefore cocrystallization and particle size reduction is desirable to improve bioavailability. In this study, a PZQ-malonic acid cocrystal was micronized by rapid expansion of supercritical solution (RESS). Due to low solubility in scCO₂, four cosolvents were screened as RESS modifiers. While addition of acetone or THF yielded mixtures of PZQ and its cocrystal, MeOH and EtOH produced pure cocrystal. Impact of pressure (15–30 MPa), temperature (35–55 °C), and cosolvent loading (3–10 volumes) on phase-purity, yield, and particle size were investigated. Adding cosolvent to RESS facilitated dissolution of cocrystal formers in scCO₂ and crystallization of the cocrystal with yields up to 68.5 wt% and particle size as low as 600 nm. Results show that for APIs with low solubility in scCO₂, cosolvent-modified RESS is a suitable approach for simultaneous crystallization and micronization.

吡喹酮 (PZQ) 是一种溶解度较低的抗蠕虫药物，因此需要通过共晶体化和缩小粒度来提高生物利用度。本研究采用超临界溶液快速膨胀法（RESS）对 PZQ-丙二酸共晶体进行了微粉化。由于 PZQ 在 scCO2 中的溶解度较低，因此筛选了四种共溶剂作为 RESS 改性剂。加入丙酮或四氢呋喃会产生 PZQ 及其共晶体的混合物，而加入 MeOH 和 EtOH 则会产生纯共晶体。研究了压力（15-30 兆帕）、温度（35-55 °C）和共溶剂添加量（3-10 体积）对相纯度、产量和粒度的影响。在 RESS 中添加共溶剂可促进共晶体形成剂在 scCO2 中的溶解和共晶体的结晶，其产率高达 68.5 wt%，粒度低至 600 nm。结果表明，对于在 scCO2 中溶解度较低的原料药，共溶剂改性 RESS 是一种同时结晶和微粉化的合适方法。

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引用次数: 0

Utilizing cocoa bean husk residues from supercritical extraction for biofuel production through hydrothermal liquefaction 通过水热液化利用超临界萃取的可可豆壳残渣生产生物燃料

IF 3.4 3区工程技术 Q2 CHEMISTRY, PHYSICAL

Journal of Supercritical Fluids

Pub Date : 2024-09-24 DOI: 10.1016/j.supflu.2024.106416

Seung Eun Lee , Ji Sun Lim , Young-Kwon Park , Bonggeun Shong , Hong-shik Lee

This study aimed to develop an efficient method for converting residual biomass into biofuel through a process that combines supercritical fluid extraction and hydrothermal liquefaction. The study analyzed the compositional changes in the biomass residues using various co-solvents and assessed their potential for biofuel production. After hydrothermal liquefaction, the liquid biofuel produced showed a decrease in the H to C ratio from 1.7 to 1.6 and a reduction in the O to C ratio from 0.5 to 0.2, compared to the unprocessed feedstock, indicating a favorable alteration in elemental composition for biofuel production. Notably, residues extracted with supercritical CO₂ and ethanol had the lowest yield, while those extracted with CO₂ and water achieved the highest energy recovery at 101.5 %. These findings suggest that integrating supercritical fluid extraction with hydrothermal liquefaction is an environmentally sustainable and efficient approach, significantly advancing the development of sustainable biofuels.

本研究旨在通过超临界流体萃取和热液液化相结合的工艺，开发一种将残留生物质转化为生物燃料的高效方法。研究分析了使用各种助溶剂的生物质残留物的成分变化，并评估了其生产生物燃料的潜力。与未经加工的原料相比，水热液化后生产出的液体生物燃料的 H C 比值从 1.7 降至 1.6，O C 比值从 0.5 降至 0.2，这表明元素组成的改变有利于生物燃料的生产。值得注意的是，用超临界二氧化碳和乙醇萃取的残渣产量最低，而用二氧化碳和水萃取的残渣能量回收率最高，达到 101.5%。这些研究结果表明，将超临界流体萃取与水热液化相结合是一种环境可持续的高效方法，可极大地推动可持续生物燃料的发展。

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引用次数: 0

Fabrication of stable slippery lubricant-infused porous surface on polymethyl methacrylate/thermoplastic polyurethane by supercritical CO2 foaming 用超临界二氧化碳发泡法在聚甲基丙烯酸甲酯/热塑性聚氨酯上制造稳定的注入润滑剂的多孔滑面

IF 3.4 3区工程技术 Q2 CHEMISTRY, PHYSICAL

Journal of Supercritical Fluids

Pub Date : 2024-09-23 DOI: 10.1016/j.supflu.2024.106415

Shaowei Xing, Yishen Zhao, Chenxu Tian, Cuifang Lv, Meijiang Lin, Yao Wang, Guangxian Li, Xia Liao

The development of sustainable and efficient methods to prepare slippery lubricant-infused porous surface (SLIPS) is a profound work. In this study, using bilayer polymers restricting foaming mutually, bimodal cells were prepared through bilayer poly(methyl methacrylate) (PMMA). At the same time, uniform cells were prepared by bilayer PMMA /thermoplastic polyurethane (TPU). The prepared porous surfaces exhibited a high porosity (57 % or more). TPU as dispersed phase increased the cell density of the PMMA/TPU surface with a maximum cell density of 5.5 × 10⁷ cells/cm² and an average cell size of 1.0 μm. SLIPS prepared on PMMA/TPU surface with high porosity and uniform microcellular had better stability, and the sliding angle (SA) remained less than 10° after centrifugal rotation at 8000 r/min. Therefore, this work provides an approach to improve the surface cell density and produce SLIPS sustainably and efficiently.

开发可持续的高效方法来制备注入润滑剂的光滑多孔表面（SLIPS）是一项意义深远的工作。本研究利用双层聚合物相互限制发泡的特性，通过双层聚甲基丙烯酸甲酯（PMMA）制备了双峰细胞。同时，通过双层聚甲基丙烯酸甲酯（PMMA）/热塑性聚氨酯（TPU）制备了均匀细胞。制备的多孔表面具有很高的孔隙率（57% 或更高）。作为分散相的热塑性聚氨酯提高了 PMMA/TPU 表面的细胞密度，最大细胞密度为 5.5 × 107 cells/cm2，平均细胞尺寸为 1.0 μm。在具有高孔隙率和均匀微孔的 PMMA/TPU 表面制备的 SLIPS 具有更好的稳定性，在 8000 r/min 的离心旋转后，滑动角（SA）仍小于 10°。因此，这项工作提供了一种提高表面细胞密度和可持续高效制备 SLIPS 的方法。

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引用次数: 0

Response surface optimization for supercritical carbon dioxide extraction of Korarima (Aframomum corrorima) seed oil and its antibacterial activity evaluation 超临界二氧化碳萃取科拉利马（Aframomum corrorima）种子油及其抗菌活性评价的响应面优化

IF 3.4 3区工程技术 Q2 CHEMISTRY, PHYSICAL

Journal of Supercritical Fluids

Pub Date : 2024-09-19 DOI: 10.1016/j.supflu.2024.106411

Mulugeta Guta, Huijun Tan, Yaping Zhao

Oils extracted from natural plants are valuable resources because of their diverse biocidal activity against microorganisms. This paper reports, for the first time, supercritical CO₂ extraction of oil from Korarima (Aframomum corrorima) seeds and its antibacterial activity evaluation. The influences of pressure, temperature, and extraction time on the yield of supercritical CO₂-extracted oil (scCO₂-extracted oil) were optimized using the Response Surface Methodology. Under the optimal extraction conditions of 46 °C, 15.5 MPa, and 147 min, the extraction yield reached 1.60±0.04 %, consistent with the theoretical value of 1.58 %. The compositions of the scCO₂-extracted oil were identified by GC-MS, primarily consisting of nerolidol (33.97–41.20 %), geraniol (23.08–24.50 %), and α-terpinene (8.90–9.06 %). The oil exhibited significant antibacterial activity against Staphylococcus. aureus with a minimum inhibitory concentration of 1 mg·mL⁻¹. This study highlights the potential applications of supercritical CO₂ extraction technology for extracting Korarima seed oil and its use as an antibacterial ingredient in cosmetics and pharmaceuticals.

从天然植物中萃取的油具有多种抗微生物的杀菌活性，因此是一种宝贵的资源。本文首次报道了超临界二氧化碳萃取Korarima（Aframomum corrorima）种子油及其抗菌活性评价。采用响应面法优化了压力、温度和萃取时间对超临界二氧化碳萃取油（scCO2-萃取油）产量的影响。在 46 °C、15.5 兆帕、147 分钟的最佳萃取条件下，萃取率达到 1.60±0.04 %，与理论值 1.58 % 一致。经 GC-MS 鉴定，scCO2 萃取油的成分主要包括橙花叔醇（33.97-41.20 %）、香叶醇（23.08-24.50 %）和α-萜品烯（8.90-9.06 %）。这种精油对金黄色葡萄球菌具有明显的抗菌活性，最低抑菌浓度为 1 毫克/毫升-1。这项研究强调了超临界 CO2 萃取技术在萃取 Korarima 种子油以及将其用作化妆品和药品中的抗菌成分方面的潜在应用。

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引用次数: 0

Experimental investigation of the pressure drop of CO2 flow at supercritical pressures in a heated 4 mm smooth pipe with different orientations 超临界压力下二氧化碳流在不同方向的 4 毫米光滑加热管中的压降实验研究

IF 3.4 3区工程技术 Q2 CHEMISTRY, PHYSICAL

Journal of Supercritical Fluids

Pub Date : 2024-09-18 DOI: 10.1016/j.supflu.2024.106407

Konstantinos Theologou, Rainer Mertz, Jörg Starflinger

The application of supercritical fluids as an alternative heat transfer medium in thermal processes is becoming increasingly important, whereby the understanding of their pressure drop characteristics is essential for the process and component design. With a total of 96 experiments, this publication shows a systematic analysis of the pressure drop of CO₂ flow at supercritical pressures in a heated smooth pipe with an inner diameter of 4 mm, at a pressure of 7.75 MPa, mass fluxes up to 2000 kg/m²s and heat fluxes up to 235 kW/m². The hydrostatic pressure drop accounts for between 4 % and 24 % of the total pressure drop and the pressure drop due to flow acceleration for between 12 % and 30 %, with the frictional pressure drop accounting for the largest percentage. It was found that the Filonenko correlation can predict the pipe friction pressure drop in the investigated parameter range with a mean absolute deviation of 7 %.

超临界流体作为一种替代传热介质在热工过程中的应用正变得越来越重要，因此了解其压降特性对于工艺和部件设计至关重要。本出版物共进行了 96 次实验，系统分析了内径为 4 毫米、压力为 7.75 兆帕、质量流量高达 2000 千克/平方米、热流量高达 235 千瓦/平方米的加热光滑管道中超临界压力下的二氧化碳流压降。静水压降占总压降的 4% 至 24%，流动加速度造成的压降占 12% 至 30%，其中摩擦压降所占比例最大。研究发现，Filonenko 相关性可以预测调查参数范围内的管道摩擦压降，平均绝对偏差为 7%。

引用次数: 0

Effect of supercritical CO2 drying variables and gel composition on the textural properties of cellulose aerogels 超临界二氧化碳干燥变量和凝胶成分对纤维素气凝胶纹理特性的影响

IF 3.4 3区工程技术 Q2 CHEMISTRY, PHYSICAL

Journal of Supercritical Fluids

Pub Date : 2024-09-18 DOI: 10.1016/j.supflu.2024.106414

Noelia D. Machado , María L. Goñi , Nicolás A. Gañán

Cellulose aerogels are interesting platforms for biomedical and drug delivery applications, due to their biocompatibility, biodegradability, water absorption capacity, and good textural properties. Supercritical CO₂ drying has been proven as an efficient technology for obtaining aerogels and preserving the porous structure. In this work, the effect of relevant process variables (CO₂ density, depressurization rate, and intermediate depressurization mode) and gel composition on the textural properties of cellulose aerogels is studied. Experiments are performed in batch-mode, and aerogel monoliths are characterized in terms of apparent density, porosity, specific surface area, and crystalline morphology. Water uptake in different buffer solutions is also evaluated. The use of thiourea in the gel formation leads to lower porosity. On the other hand, higher porosity and surface area are obtained when depressurization is slow and the system is only partially depressurized between drying cycles. Aerogels showed a good and fast water uptake capacity, regardless of the pH (200–500 %).

纤维素气凝胶具有生物相容性、生物可降解性、吸水能力和良好的质地特性，是生物医学和药物输送应用的有趣平台。超临界二氧化碳干燥已被证明是获得气凝胶并保持其多孔结构的有效技术。在这项工作中，研究了相关工艺变量（二氧化碳密度、减压速率和中间减压模式）和凝胶成分对纤维素气凝胶质构特性的影响。实验以间歇模式进行，气凝胶单体在表观密度、孔隙率、比表面积和结晶形态方面均有特征。此外，还评估了气凝胶在不同缓冲溶液中的吸水性。在凝胶形成过程中使用硫脲会导致孔隙率降低。另一方面，如果减压速度较慢，且系统在两次干燥循环之间只进行部分减压，则孔隙率和比表面积会更高。无论酸碱度如何（200-500 %），气凝胶都具有良好而快速的吸水能力。

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