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Facile preparation of conductive silicone rubber composite foams with tunable cell morphologies and absorption-dominant characteristics 轻松制备具有可调细胞形态和吸收主导特性的导电硅橡胶复合泡沫
IF 3.4 3区 工程技术 Q2 CHEMISTRY, PHYSICAL Pub Date : 2024-07-07 DOI: 10.1016/j.supflu.2024.106346

Flexible silicone rubber (SR) foams with tunable cellular morphologies were fabricated via supercritical CO2 foaming. Conductive carbon black (CB) modified at a low cost and with high complex viscosity was preferentially selected. The effects of the pore size and void fraction on the electrical conductivity and dielectric permittivity of the SR/CB composite foams were carefully investigated. The pore size of the foams affected the specific shielding effectiveness (SSE) and absorption coefficient (A), whereas the variation in the void fraction did not generate evident changes. In comparison with its solid counterpart, a foam with a pore diameter of 59.9 μm showed a 50 % decrease in density, 31.6 % increase in absorptivity, and 95.7 % increase in SSE, demonstrating a considerable electromagnetic interference shielding effectiveness (EMI SE). Decreases in the pore size and void fraction of the foams improved compression modulus and strength. In addition, sample preparation process was simplified, making industrial production easier.

通过超临界二氧化碳发泡制造了具有可调蜂窝形态的柔性硅橡胶(SR)泡沫。优先选择了成本低、复合粘度高的改性导电炭黑(CB)。研究人员仔细研究了孔径和空隙率对 SR/CB 复合泡沫的导电性和介电常数的影响。泡沫的孔径会影响特定屏蔽效能(SSE)和吸收系数(A),而空隙率的变化不会产生明显的变化。与固体泡沫相比,孔径为 59.9 μm 的泡沫密度降低了 50%,吸收率提高了 31.6%,SSE 提高了 95.7%,显示出相当高的电磁干扰屏蔽效能(EMI SE)。泡沫孔径和空隙率的减少提高了压缩模量和强度。此外,还简化了样品制备过程,使工业生产更加容易。
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引用次数: 0
Selective extraction of carnosic acid, carnosol, and rosmarinic acid from Rosmarinus officinalis L. using supercritical fluid and their antioxidant activity 利用超临界流体从迷迭香中选择性提取肉豆蔻酸、肉豆蔻醇和迷迭香酸及其抗氧化活性
IF 3.4 3区 工程技术 Q2 CHEMISTRY, PHYSICAL Pub Date : 2024-07-02 DOI: 10.1016/j.supflu.2024.106344
Meryem Boufetacha , Abdelilah Ayad , Nicolas Thiebault , Nadia Boussetta , Elkhadir Gharibi , Mohammed Benali

Rosmarinus officinalis L. is one of the most widely exploited medicinal plants for its bioactive compounds, including rosmarinic acid (RA), carnosic acid (CA) and carnosol (CAR). This study aims to selectively extract these compounds, using supercritical fluids extraction with carbon dioxide and ethanol as co-solvents, based on the Hansen solubility parameters approach. This approach predicted that CA and CAR are highly soluble in the supercritical fluid. However, a weak interaction was predicted between RA and this fluid. The experimental findings indicated the highest amounts of RA and CA were observed at 150 bar and 80°C, resulting in yields of 3.43 mg/g dry weight (DW), and 18.9 mg/g DW, respectively. Favourable extraction conditions for CAR were recorded at 250 bar and 40°C, with a content of 19.1 mg/g DW. Evaluation of antioxidant activity using DPPH tests revealed that extracts obtained at 250 bar at 40 and 80°C rich in CAR have a stronger antioxidant power.

迷迭香(Rosmarinus officinalis L.)是一种被广泛利用的药用植物,其生物活性化合物包括迷迭香酸(RAs)、肉毒碱(CA)和肉毒酚(CAR)。本研究以汉森溶解度参数法为基础,以二氧化碳和乙醇为助溶剂,采用超临界流体萃取法选择性地提取这些化合物。该方法预测 CA 和 CAR 在超临界流体中的溶解度很高。然而,根据预测,RA 与该流体之间的相互作用较弱。实验结果表明,在 150 巴和 80 摄氏度的条件下,RA 和 CA 的含量最高,产量分别为 3.43 毫克/克干重(DW)和 18.9 毫克/克干重。在 250 巴和 40 摄氏度的条件下,CAR 的提取效果较好,含量为 19.1 毫克/克干重。使用 DPPH 试验对抗氧化活性进行评估后发现,在 250 bar、40 和 80°C 条件下提取的富含 CAR 的提取物具有更强的抗氧化能力。
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引用次数: 0
A comparative analysis of density-based and neural network modeling for predicting the solubility of organic compounds in supercritical carbon dioxide 基于密度和神经网络建模预测有机化合物在超临界二氧化碳中溶解度的对比分析
IF 3.4 3区 工程技术 Q2 CHEMISTRY, PHYSICAL Pub Date : 2024-07-02 DOI: 10.1016/j.supflu.2024.106345
Mohammad Mahdi Barzegar, Feridun Esmaeilzadeh, Ali Zandifar

This study investigates the estimation of solute solubility in supercritical carbon dioxide (SC-CO2) within a pressure and temperature range of 80 bar to 490.29 bar and 308 K to 423 K. We propose a novel empirical model that establishes a correlation between relevant parameters and the targeted solubility. A feature importance algorithm facilitated the development of this empirical model. The model’s accuracy is comprehensively evaluated using 40 published experimental datasets, with an average absolute relative deviation (AARD) of 9.9 %. It demonstrates superior performance compared to 12 previously established models. Furthermore, a fine-tuned artificial neural network (ANN) is developed to harness the unique capabilities of machine learning techniques. The ANN outperforms the proposed model, achieving a significantly lower AARD% of 4.38. This outcome emphasizes the potential of machine learning techniques, particularly ANNs, for achieving superior accuracy.

本研究探讨了超临界二氧化碳(SC-CO)中溶质溶解度的估算方法,其压力和温度范围分别为 80 巴至 490.29 巴和 308 K 至 423 K。我们提出了一个新的经验模型,该模型建立了相关参数与目标溶解度之间的相关性。特征重要性算法促进了这一经验模型的开发。利用 40 个已发表的实验数据集对该模型的准确性进行了全面评估,平均绝对相对偏差 (AARD) 为 9.9%。与之前建立的 12 个模型相比,该模型表现出更优越的性能。此外,还开发了一种微调人工神经网络(ANN),以利用机器学习技术的独特能力。人工神经网络的性能优于所提出的模型,AARD% 明显降低到 4.38。这一结果凸显了机器学习技术,特别是人工神经网络在实现更高精度方面的潜力。
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引用次数: 0
Effect of stirring and KOH/NaOH ratio on phase formation in hydrothermal synthesis of KNbO3-NaNbO3 particles 水热合成 KNbO3-NaNbO3 粒子过程中搅拌和 KOH/NaOH 比率对相形成的影响
IF 3.4 3区 工程技术 Q2 CHEMISTRY, PHYSICAL Pub Date : 2024-06-30 DOI: 10.1016/j.supflu.2024.106340
Ellawala K. Chandima Pradeep, Alexandre Chauvel, Cenk Abdurrahmanoglu, Ragnar Kiebach, Astri Bjørnetun Haugen

This study investigates the hydrothermal synthesis of KNbO3-NaNbO3 particles, which contains compositions of interest as lead-free piezoelectric materials. Precursor solutions containing Nb2O5, NaOH/KOH were hydrothermally reacted at 190 0C for 15 hours using either a conventional reactor or a reactor with stirring. For 50 % KOH or lower, the product was cubic or elongated cuboid/belt-shaped NaNbO3, whereas solely KOH resulted in hexagonal plate-like KNbO3. When 75 % KOH was used, the product was a mixture of large K5Na3Nb6O19·9 H2O hexagonal plates and smaller NaNbO3 cubes. We hypothesized this phase segregation was induced by highly concentrated microenvironments, and stirring would prevent that. Accordingly, stirring hydrothermal treatment of 75 % KOH solution produced only K5Na3Nb6O19·H2O hexagonal plates, which could be transformed to K0.7Na0.3NbO3 by calcination. By reducing the hydrothermal treatment time to 1 – 6 hours we isolated reaction intermediates, and based on them propose a kinetics-controlled mechanism for hydrothermal reactions of Nb2O5 and KOH/NaOH.

本研究探讨了 KNbO3-NaNbO3 粒子的水热合成,其中包含可用作无铅压电材料的成分。含有 Nb2O5、NaOH/KOH 的前驱体溶液在 190 0C 温度下,使用传统反应器或带搅拌的反应器进行 15 小时的水热反应。当使用 50% 或更低的 KOH 时,生成物为立方体或细长的立方体/带状 NaNbO3,而仅使用 KOH 则生成六方板状 KNbO3。当使用 75% 的 KOH 时,生成物是大的 K5Na3Nb6O19-9 H2O 六方板和较小的 NaNbO3 立方体的混合物。我们假设这种相分离是由高浓度微环境引起的,而搅拌可以防止这种情况。因此,对 75% KOH 溶液进行搅拌水热处理后,只产生了 K5Na3Nb6O19-H2O 六方板,煅烧后可转化为 K0.7Na0.3NbO3。通过将水热处理时间缩短至 1 - 6 小时,我们分离出了反应中间产物,并在此基础上提出了 Nb2O5 和 KOH/NaOH 水热反应的动力学控制机制。
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引用次数: 0
Amphoteric SnO2 nanoparticles via pH-controlled continuous flow solvothermal synthesis 通过 pH 值控制的连续流溶热合成技术制备两性氧化锡纳米粒子
IF 3.4 3区 工程技术 Q2 CHEMISTRY, PHYSICAL Pub Date : 2024-06-26 DOI: 10.1016/j.supflu.2024.106341
Aref Mamakhel , Magnus Kløve , Martin Bondesgaard , Troels L. Christiansen , Steen Uttrup Pedersen , Jørgen Skibsted , Bo Brummerstedt Iversen

Amphoteric oxides can be challenging to produce in phase pure form due to their sensitivity to the pH of the reaction mixture. The high-pressure, high-temperature reaction conditions of hydrothermal processes make the pH difficult to control. Here we report a simple approach to obtain nanoparticles of amphoteric oxides, where cheap metal nitrate precursors are reacted in alcohol (2-propanol) water mixtures (25 vol%:75 vol%) to maintain a neutral pH under solvothermal conditions. Phase pure SnO2 nanoparticles were synthesized in a continuous flow solvothermal reactor at 250 °C, 300 °C, 350 °C and 400 °C with sizes ranging from 3 nm to 7 nm. The nanoparticles were characterized using powder X-ray diffraction, transmission electron microscopy, energy dispersive X-ray spectroscopy, Raman spectroscopy, 119Sn MAS NMR spectroscopy, Brunauer-Emmett-Teller nitrogen adsorption, UV–VIS, and as anode material in CR2032 Li-ion battery cells. To demonstrate generality, amphoteric oxides ZnO, Bi2O3, Cr2O3 and γ-AlOOH were also synthesized.

两性氧化物对反应混合物的 pH 值非常敏感,因此生产纯相两性氧化物具有挑战性。水热法的高压高温反应条件使得 pH 值难以控制。在这里,我们报告了一种获得两性氧化物纳米颗粒的简单方法,即在溶热条件下,将廉价的金属硝酸盐前体在醇(2-丙醇)水混合物(25 vol%:75 vol%)中进行反应,以保持中性 pH 值。在 250 ℃、300 ℃、350 ℃ 和 400 ℃ 温度下,在连续流动溶热反应器中合成了相纯的氧化锡纳米粒子,其尺寸范围为 3 nm 至 7 nm。使用粉末 X 射线衍射、透射电子显微镜、能量色散 X 射线光谱、拉曼光谱、Sn MAS NMR 光谱、Brunauer-Emmett-Teller 氮吸附、紫外-可见光谱对纳米粒子进行了表征,并将其作为 CR2032 锂离子电池的阳极材料。为了证明其通用性,还合成了两性氧化物 ZnO、BiO、CrO 和 γ-AlOOH。
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引用次数: 0
Measurement and modeling of the electrical conductivity of organic electrolyte solutions and their mixtures with compressed CO2 有机电解质溶液及其与压缩二氧化碳混合物电导率的测量与建模
IF 3.4 3区 工程技术 Q2 CHEMISTRY, PHYSICAL Pub Date : 2024-06-26 DOI: 10.1016/j.supflu.2024.106338
Marvin Dorn , Lukas Franke , Paul Figiel , Sabine Kareth , Eckhard Weidner , Christoph Held , Marcus Petermann

The electrochemical carbon dioxide reduction reaction (CO2RR) is of increasing importance for the development of a closed carbon cycle. Here, electrolytes are often used to increase the electrical conductivity and thus the current density. In addition, the use of compressed CO2 and electrolyte-containing organic solvents suppresses hydrogen evolution. However, the electrical conductivity of CO2-saturated electrolyte solutions is mostly unknown. Therefore, their electrical conductivity was investigated in this work at different electrolyte concentrations, pressures (up to 150 bar) and temperatures (298.15 K and 343.15 K). In addition, the simplified Mean Spherical Approximation (MSA-simple) model, supported by ePC-SAFT for density modeling, was used to successfully model the conductivity. The results show that CO2-saturated electrolyte solutions generally exhibit lower conductivities than CO2-free electrolyte solutions. However, at very low electrolyte and CO2 concentrations, the conductivities were higher in CO2-saturated electrolyte solutions than in CO2-free electrolyte solutions, which is a new finding in the literature.

电化学二氧化碳还原反应(CO2RR)对于开发封闭式碳循环的重要性与日俱增。在这种情况下,通常使用电解质来增加导电性,从而提高电流密度。此外,使用压缩的 CO 和含电解质的有机溶剂可抑制氢的演化。然而,CO 饱和电解质溶液的电导率大多不为人知。因此,本研究对不同电解质浓度、压力(最高 150 巴)和温度(298.15 K 和 343.15 K)下的电导率进行了研究。此外,在 ePC-SAFT 的密度建模支持下,使用简化的平均球形近似(MSA-simple)模型成功地建立了电导率模型。结果表明,CO 饱和电解质溶液的电导率通常低于不含 CO 的电解质溶液。然而,在电解质和 CO 浓度很低的情况下,CO 饱和电解质溶液的电导率要高于无 CO 的电解质溶液,这在文献中是一个新发现。
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引用次数: 0
Effect of supercritical carbon dioxide on pore structure and methane adsorption of shale with different particle sizes 超临界二氧化碳对不同粒径页岩的孔隙结构和甲烷吸附的影响
IF 3.4 3区 工程技术 Q2 CHEMISTRY, PHYSICAL Pub Date : 2024-06-26 DOI: 10.1016/j.supflu.2024.106343
Liang Wang , Yuechen Zhao , Minxuan Liu , Zihang Song , Yiwei Sun , Sijia Ni , Shenguang Fu , Rongkun Pan

Supercritical carbon dioxide (SCCO2) fracturing significantly enhances shale gas recovery, which is influenced by particle size. We soaked shale in SCCO2 and investigated the impact of SCCO2 on different particle sizes. Large-particle shales showed the largest percentage changes in specific surface area and total pore volume (54.11 %, 87.87 %; 58.59 %, 76.32 %) followed by small-particle size shales. This trend was also observed in other pore structure parameters. The particle-size effect is: Large-particle shale, with abundant microfractures, enhances SCCO2 flow and pore alteration. Small-particle shale's high specific surface area facilitates SCCO2 penetration. Medium-particle shale is less affected due to balanced interactions of these factors. Methane is primarily found in large and medium pores and microfractures. Methane adsorption in shale mainly involves multi-layer adsorption. Following SCCO2 treatment, pore fractures narrowed, increasing the proportion of methane molecules adsorbed as a single-layer. This study is crucial for evaluating the fracturing effects on shale gas wells.

超临界二氧化碳(SCCO2)压裂法能显著提高页岩气的采收率,而页岩气的采收率受颗粒大小的影响。我们将页岩浸泡在 SCCO2 中,并研究了 SCCO2 对不同粒径的影响。大颗粒页岩的比表面积和总孔隙度的百分比变化最大(54.11 %、87.87 %;58.59 %、76.32 %),其次是小颗粒页岩。其他孔隙结构参数也呈现出这种趋势。颗粒大小的影响是大颗粒页岩具有丰富的微裂隙,可增强 SCCO2 流动和孔隙改变。小颗粒页岩的高比表面积有利于 SCCO2 的渗透。中颗粒页岩受到的影响较小,这是因为这些因素之间的相互作用达到了平衡。甲烷主要存在于大、中孔隙和微裂缝中。甲烷在页岩中的吸附主要涉及多层吸附。经 SCCO2 处理后,孔隙裂缝变窄,增加了单层吸附甲烷分子的比例。这项研究对于评估页岩气井的压裂效果至关重要。
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引用次数: 0
Liposomes and niosomes production by a supercritical CO2 assisted process for topical applications: A comparative study 通过超临界二氧化碳辅助工艺生产局部应用的脂质体和niosomes:比较研究
IF 3.4 3区 工程技术 Q2 CHEMISTRY, PHYSICAL Pub Date : 2024-06-26 DOI: 10.1016/j.supflu.2024.106342
Lucia Baldino, Domenico Riccardi, Ernesto Reverchon

A supercritical CO2 assisted process was used to perform a comparative study between liposomes and niosomes. Process operating conditions were fixed at 100 bar and 40 °C, and the produced vesicles were characterized in terms of mean diameter, size distribution, ζ-potential, and stability over time. Mean diameters of liposomes and niosomes were similar (130 ± 37 nm for liposomes and 141 ± 36 nm for niosomes) and both systems were stable after 1 month from production. Ascorbic acid (AA) was loaded in both kinds of formulation. AA encapsulation efficiency was equal to 92 % and 99 % for liposomes and niosomes, respectively, and DPPH-activity was larger than 90 % in both vesicular systems. Drug release tests revealed that AA was released in 120 min and 240 min from liposomes and niosomes, respectively, due to a different compactness of the vesicle bilayer.

利用超临界二氧化碳辅助工艺对脂质体和niosomes进行了比较研究。工艺操作条件固定为 100 巴和 40 °C,生产出的囊泡在平均直径、大小分布、ζ电位和随时间变化的稳定性方面都有特征。脂质体和niosomes的平均直径相似(脂质体为130 ± 37 nm,niosomes为141 ± 36 nm),两种体系在生产1个月后都很稳定。两种制剂都含有抗坏血酸(AA)。脂质体和niosomes的AA包封效率分别为92%和99%,两种囊泡体系的DPPH活性均大于90%。药物释放测试表明,由于囊泡双分子层的紧密度不同,AA分别在120分钟和240分钟内从脂质体和niosomes中释放出来。
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引用次数: 0
Towards a new approach in chiral resolution: Pressurized-CO2 assisted preferential cocrystallization 手性解析的新方法:加压-CO2 辅助优先共晶体化
IF 3.4 3区 工程技术 Q2 CHEMISTRY, PHYSICAL Pub Date : 2024-06-24 DOI: 10.1016/j.supflu.2024.106339
Joséphine de Meester , Patrick Layrisse , Mathieu Marchivie , Laurent Collard , Guillaume Wery , Clément Brandel , Yohann Cartigny , Pascale Subra-Paternault , Tom Leyssens , Christelle Harscoat-Schiavo

We here report the first occurrence of a preferential cocrystallization process assisted by compressed carbon dioxide. Our study focuses on the Nefiracetam-Mandelic acid conglomerate forming system. The cocrystal conglomerate was successfully crystallized using compressed CO2 as antisolvent, and acetone, ethyl acetate, or isobutanol as solvents for starting solutions in the so-called GAS process. We then focus on acetone to successfully perform preferential cocrystallization supported by compressed CO2. A critical step in the design of the process is the adaptation of the set-up to allow the introduction of enantiopure seeding inside the reactor. Based on the use of seeded rings, we test several seeding configurations to enhance enantioseparation through the simultaneous crystallization of both enantiomers in two different areas of the reactor.

我们在此报告了首次出现的由压缩二氧化碳辅助的优先共晶过程。我们的研究重点是奈非拉西坦-扁桃酸结晶体系。在所谓的 GAS 过程中,以压缩二氧化碳作为反溶剂,以丙酮、乙酸乙酯或异丁醇作为起始溶液的溶剂,成功地结晶出了共晶体凝聚体。然后,我们将重点放在丙酮上,在压缩 CO 的支持下成功实现了优先共晶。该工艺设计的关键步骤是调整装置,以便在反应器内引入对映体纯种。在使用种子环的基础上,我们测试了几种种子配置,通过两种对映体在反应器的两个不同区域同时结晶来提高对映体分离效果。
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引用次数: 0
Encapsulation of Arthrospira platensis polyphenolic extract using supercritical emulsion-based process 利用超临界乳液法封装节肢动物多酚提取物
IF 3.4 3区 工程技术 Q2 CHEMISTRY, PHYSICAL Pub Date : 2024-06-21 DOI: 10.1016/j.supflu.2024.106335
Chiara Bufalini , Ida Palazzo , Alessandro Alberto Casazza , Pier Francesco Ferrari , Roberta Campardelli , Giuseppe Firpo , Patrizia Perego , Ernesto Reverchon

Arthrospira platensis polyphenolic natural extracts have several benefits for human health. Due to their instability and reduced shelf-life, these extracts are usually encapsulated. This work analyzed the supercritical emulsion extraction (SEE) process for the production of polymeric nanoparticles loaded with A. platensis polyphenolic extracts. The objective of this work was to evaluate a powdered encapsulation system to overcome the drawbacks of liquid systems, which are those mainly used for microalgae extract stabilization. An optimization study was performed investigating different process parameters and comparing the obtained particles in terms of particle size distribution, morphology, and encapsulation efficiency. The process permitted the successfull production of loaded polymeric nanoparticles with an encapsulation efficiency up to 74 % in the best operating conditions. The SEE process allowed a better control of morphology and particle size distribution of the nanometric particles operating in a continuous mode.

Arthrospira platensis 多酚天然提取物对人体健康有多种益处。由于其不稳定性和较短的保质期,这些提取物通常被封装起来。本研究分析了超临界乳液萃取(SEE)工艺,用于生产装载有板蓝根节肢动物多酚提取物的聚合物纳米颗粒。这项工作的目的是评估一种粉末封装系统,以克服液体系统(主要用于稳定微藻提取物)的缺点。研究人员对不同的工艺参数进行了优化研究,并从粒度分布、形态和封装效率等方面对获得的颗粒进行了比较。在最佳操作条件下,该工艺成功地生产出了负载聚合物纳米粒子,封装效率高达 74%。SEE 工艺可以更好地控制以连续模式运行的纳米颗粒的形态和粒度分布。
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引用次数: 0
期刊
Journal of Supercritical Fluids
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