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Although CO2 geological storage (CGS) is thought to be one of the most promising technologies to sequester the anthropogenic CO2 to mitigate the climate change, implementation of the method is still challenging due to lack of fundamental understanding of controls of wettability, which is responsible for residual trapping of the gas and its flow dynamics. One of the key parameters that controls the wetting state is the zeta potential, ζ, at rock‐water and CO2‐water interfaces. ζ in systems comprising rocks, carbonated aqueous solutions and immiscible supercritical CO2 have not been measured prior to this study, where we detail the experimental protocol that enables measuring ζ in such systems, and report novel experimental data on the multi‐phase ζ. We also demonstrate for the first time that ζ of supercritical CO2‐water interface is negative with a magnitude greater that 14 mV. Moreover, our experimental results suggest that presence of multi‐valent cations in tested solutions causes a shift of wettability toward intermediate‐wet state. We introduce a new parameter that combines multi‐phase ζ and relative permeability endpoints to characterize the wetting state and residual supercritical CO2 saturation. Based on these results, we demonstrate that ζ measurements could serve as a powerful experimental method for predicting CGS efficiency and/or for designing injection of aqueous solutions with bespoke composition prior to implementing CGS to improve the residual CO2 trapping in sandstone formations. Plain Language Summary Extensive research has been conducted in the field of CO2 geological storage (CGS). However, among a multitude of parameters that affect the efficiency of CGS, the system's wettability has been investigated empirically rather than from first principles. Fundamentally, wettability controls distribution of injected CO2 and reservoir fluids in the pore space, as well as the flow dynamics of all fluids in target formations. One of the main forces controlling the wetting state is related to electrostatic interaction between rock‐water and CO2‐water interfaces, and the zeta potential is a property that describes these interactions. With the zeta potential dependence on the partial CO2 pressure, water pH and chemical composition, and mineralogy, wettability can be characterized and/or modified prior to CO2 injection using this interfacial property, thus enabling optimization of residual CO2 trapping and significantly improving overall CGS efficiency. We have designed and for the first time carried out coreflooding experiments combined with single‐ and multi‐phase zeta potential measurements at CGS conditions. We have introduced the normalized zeta potential which comprises two independent wettability indicators, and report a correlation between this property, the residual CO2 saturation and wettability. Our results explain the underlying mechanisms of dependence of CO2 saturation on experimental conditions. Relationship between the interfacial rock‐water (ζr–w), supercritical CO2‐water (ζc–w), macroscopic multiphase (ζm–p) zeta potential and the wetting state of quartz‐supercritical CO2‐aqueous solution systems.

Macroalgae are one of potential sources for carotenoids, such as fucoxanthin, which are consumed by humans and animals. This carotenoid has been applied in both the pharmaceutical and food industries. In this study, extraction of fucoxanthin from wet brown seaweed Undaria pinnatifida (water content was 93.2%) was carried out with a simple method using liquefied dimethyl ether (DME) as an extractant in semi-continuous flow-type system. The extraction temperature and absolute pressure were 25 °C and 0.59 MPa, respectively. The liquefied DME was passed through the extractor that filled by U. pinnatifida at different time intervals. The time of experiment was only 43 min. The amount of fucoxanthin could approach to 390 μg/g dry of wet U. pinnatifida when the amount of DME used was 286 g. Compared with ethanol Soxhlet and supercritical CO2 extraction, which includes drying and cell disruption, the result was quite high. Thus, DME extraction process appears to be a good method for fucoxanthin recovery from U. pinnatifida with improved yields.

The process of supercritical CO 2 extraction of aromatic and medicinal plants represents a revolutionary advancement in the field of natural compound extraction. By harnessing the unique properties of carbon dioxide in its supercritical state. This review critically evaluates the supercritical CO 2 extraction process for aromatic and medicinal plants, aiming to assess its efficiency, selectivity, and environmental impact thoroughly. By meticulously analysing its potential as an innovative solution in the industry, the study delves into the technique’s capacity to generate high-quality extracts while significantly reducing the ecological footprint associated with traditional extraction methods. Supercritical CO 2 extraction represents a substantial advancement in natural compound extraction, offering unparalleled precision and purity. By circumventing the use of harmful solvents commonly employed in conventional methods, it presents a sustainable alternative for the extraction of valuable compounds from aromatic and medicinal plants. This environmentally conscious approach aligns with the growing demand for eco-friendly practices within the industry, providing a promising avenue for sustainable resource utilization. Through a comprehensive examination of its benefits and limitations, this review seeks to contribute to a deeper understanding of supercritical CO 2 extraction’s role in shaping the future of the aromatic and medicinal plant sector. By shedding light on its potential applications and implications, this study aims to inform decision-makers and researchers alike about the transformative potential of this innovative extraction technique.

In this article, highly porous and transparent silicon oxycarbide (SiOC) gels are synthesized from Bis(Triethoxysilyl) methane (BTEM). The gels are synthesized by the sol-gel technique followed by both ambient pressure and supercritical drying. Then, the portion of wet gels have been pyrolyzed in a hydrogen atmosphere at 800 and 1100 °C. The FT-IR spectroscopy analysis and nitrogen sorption results indicate the successful synthesis of Si-O-Si bonds and the formation of mesopores. From a hysteresis loop, the SiOC ceramics showed the H1 type characteristic with well-defined cylindrical pore channels for the aerogel and the H2 type for the ambigel samples, indicating that the pores are distorted due to the capillary stress. The produced gels are mesoporous materials having high surface areas with a maximum of 1140 m2/g and pore volume of 2.522 cm3/g obtained from BTEM aerogels. The pyrolysis of BTEM aerogels at 800 °C results in the production of a bulk and transparent sample with a slightly pale white color, while BTEM xerogels are totally transparent and colorless at the same temperature. At 1100 °C, all the aerogels become opaque brown, confirming the formation of free carbon and crystalline silicon.

Silk sericin (SS), a by-product of the textile industry, has gained significant attention for its biomedical potential due to its biocompatibility and regenerative potential. However, the literature lacks information on SS processing methods and the resulting physicochemical properties. This study represents the first step in protocol optimization and standardization. In the present work, different processing techniques were studied and compared on SS extracted from boiling water: evaporation, rotary evaporation, lyophilization, and dialysis, which presented a recovery yield of approximately 27–32%. The goal was to find the most promising process to concentrate extracted SS solutions, and to ensure that the SS structure was highly preserved. As a result, a new cryo-lyophilization methodology was proposed. The proposed method allows for the preservation of the amorphous structure, which offers significant advantages including complete dissolution in water and PBS, an increase in storage stability, and the possibility of scaling-up, making it highly suitable for industrial and biomedical applications. The second part of the work focused on addressing another challenge in SS processing: efficient and non-destructive sterilization. Supercritical CO2 (scCO2) has been gaining momentum in the last years for sterilizing sensitive biopolymers and biological materials due to its non-toxicity and mild processing conditions. Thus, scCO2 technology was validated as a mild technique for the terminal sterilization of SS. In this way, it was possible to engineer a sequential cryo-lyophilization/scCO2 sterilization process which was able to preserve the original properties of this natural silk protein. Overall, we have valorized SS into a sterile, off-the-shelf, bioactive, and water-soluble material, with the potential to be used in the biomedical, pharmaceutical, or cosmetic industries.

The use of clean technologies in the development of bioactive plant extracts has been encouraged, but it is necessary to verify the cytotoxicity and cytoprotection for food and pharmaceutical applications. Therefore, the objective of this work was to obtain the experimental data of the supercritical sequential extraction of murici pulp, to determine the main bioactive compounds obtained and to evaluate the possible cytotoxicity and cytoprotection of the extracts in models of HepG2 cells treated with H2O2. The murici pulp was subjected to sequential extraction with supercritical CO2 and CO2+ethanol, at 343.15 K, and 22, 32, and 49 MPa. Higher extraction yields were obtained at 49 MPa. The oil presented lutein (224.77 µg/g), oleic, palmitic, and linoleic, as the main fatty acids, and POLi (17.63%), POO (15.84%), PPO (13.63%), and LiOO (10.26%), as the main triglycerides. The ethanolic extract presented lutein (242.16 µg/g), phenolic compounds (20.63 mg GAE/g), and flavonoids (0.65 mg QE/g). The ethanolic extract showed greater antioxidant activity (122.61 and 17.14 µmol TE/g) than oil (43.48 and 6.04 µmol TE/g). Both extracts did not show cytotoxicity and only murici oil showed a cytoprotective effect. Despite this, the results qualify both extracts for food/pharmaceutical applications.

Abelmoschus manihot (L.) Medic has been used for many years in Chinese traditional medicine. In this study, supercritical CO2 plus a modifier was utilized to extract flavonoids from the flowers of Abelmoschus manihot (L.) Medic. The effects of temperature (40 °C–60 °C), pressure (10–30 MPa) and different concentrations of ethanol as modifier (60%–90%, ethanol:water, v/v) on major flavonol content and the antioxidant activity of the extracts were studied by response surface methodology (RSM) using a Box-Behnken design. The flavonol content was calculated as the sum of the concentrations of seven major flavonoids, namely rutin, hyperin, isoquercetin, hibifolin, myricetin, quercetin-3′-O-glucoside and quercetin, which were simultaneously determined by a HPLC method. The antioxidant activity was evaluated by a 2,2-diphenyl-1-picrylhydarzyl (DPPH) free radical-scavenging assay. The results showed that three factors and their interactions could be well fitted to second-order polynomial models (p < 0.05). At the optimal extraction conditions for flavonol content (20 MPa, 52 °C, and 85% ethanol content), the yield of flavonoids was 41.96 mg/g and the IC50 value was 0.288 mg/mL, respectively, suggesting the extract has high antioxidant activity. Furthermore, the anti-adipogenic activity of the extract on the 3T3-L1 cell line was investigated. The results indicated that it can downregulate PPARγ and C/EBPα expression at mRNA. In summary, in this study, we have established a cost-effective method for the extraction of flavonoids from the flowers of Abelmoschus manihot (L.) Medic using supercritical fluid extraction and the extracts exhibited potent antioxidant and anti-adipogenic effects, suggesting a possible therapeutic approach for the prevention and treatment of obesity.

Astaxanthin and lutein, antioxidants used in nutraceutics and cosmetics, can be extracted from several microalgal species. In this work, investigations on astaxanthin and lutein extraction from Haematococcus pluvialis (H. pluvialis) in the red phase were carried out by means of the supercritical fluid extraction (SFE) technique, in which CO2 supercritical fluid was used as the extracting solvent with ethanol as the co-solvent. The experimental activity was performed using a bench-scale reactor in semi-batch configuration with varying extraction times (20, 40, 60, and 80 min), temperatures (50, 65, and 80 °C) and pressures (100, 400, and 550 bar). Moreover, the performance of CO2 SFE with ethanol was compared to that without ethanol. The results show that the highest astaxanthin and lutein recoveries were found at 65 °C and 550 bar, with ~18.5 mg/g dry weight (~92%) astaxanthin and ~7.15 mg/g dry weight (~93%) lutein. The highest astaxanthin purity and the highest lutein purity were found at 80 °C and 400 bar, and at 65 °C and 550 bar, respectively.

Aerogels from natural polymers are endowed with attractive textural and biological properties for biomedical applications due to their high open mesoporosity, low density, and reduced toxicity. Nevertheless, the lack of macroporosity in the aerogel structure and of a sterilization method suitable for these materials restrict their use for regenerative medicine purposes and prompt the research on getting ready-to-implant dual (macro + meso)porous aerogels. In this work, zein, a family of proteins present in materials for tissue engineering, was evaluated as a sacrificial porogen to obtain macroporous starch aerogels. This approach was particularly advantageous since it could be integrated in the conventional aerogel processing method without extra leaching steps. Physicochemical, morphological, and mechanical characterization were performed to study the effect of porogen zein at various proportions (0:1, 1:2, and 1:1 zein:starch weight ratio) on the properties of the obtained starch-based aerogels. From a forward-looking perspective for its clinical application, a supercritical CO2 sterilization treatment was implemented for these aerogels. The sterilization efficacy and the influence of the treatment on the aerogel final properties were evaluated mainly in terms of absence of microbial growth, cytocompatibility, as well as physicochemical, structural, and mechanical modifications.

Quantitative electrolyte extraction from lithium ion batteries (LIB) is of great interest for recycling processes. Following the generally valid EU legal guidelines for the recycling of batteries, 50 wt % of a LIB cell has to be recovered, which cannot be achieved without the electrolyte; hence, the electrolyte represents a target component for the recycling of LIBs. Additionally, fluoride or fluorinated compounds, as inevitably present in LIB electrolytes, can hamper or even damage recycling processes in industry and have to be removed from the solid LIB parts, as well. Finally, extraction is a necessary tool for LIB electrolyte aging analysis as well as for post-mortem investigations in general, because a qualitative overview can already be achieved after a few minutes of extraction for well-aged, apparently “dry” LIB cells, where the electrolyte is deeply penetrated or even gellified in the solid battery materials.