Search results for: hydrothermal decarboxylation

Authors: Sam Derakhshan Deilami, Iain N. Kings, Lynne E. Macaskie, Brajendra K. Sharma, Anthony V. Bridgwater, Joseph Wood

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This paper reports the application of a bacteria-supported palladium catalyst to the hydrodeoxygenation (HDO) of pyrolysis bio-oil, towards producing an upgraded transport fuel. Biofuels are key to the timely replacement of fossil fuels in order to mitigate the emissions of greenhouse gases and depletion of non-renewable resources. The process is an essential step in the upgrading of bio-oils derived from industrial by-products such as agricultural and forestry wastes, the crude oil from pyrolysis containing a large amount of oxygen that requires to be removed in order to create a fuel resembling fossil-derived hydrocarbons. The bacteria supported catalyst manufacture is a means of utilizing recycled metals and second life bacteria, and the metal can also be easily recovered from the spent catalysts after use. Comparisons are made between bio-Pd, and a conventional activated carbon supported Pd/C catalyst. Bio-oil was produced by fast pyrolysis of beechwood at 500 C at a residence time below 2 seconds, provided by Aston University. 5 wt % BioPd/C was prepared under reducing conditions, exposing cells of E. coli MC4100 to a solution of sodium tetrachloropalladate (Na2PdCl4), followed by rinsing, drying and grinding to form a powder. Pd/C was procured from Sigma-Aldrich. The HDO experiments were carried out in a 100 mL Parr batch autoclave using ~20g bio-crude oil and 0.6 g bio-Pd/C catalyst. Experimental variables investigated for optimization included temperature (160-350C) and reaction times (up to 5 h) at a hydrogen pressure of 100 bar. Most of the experiments resulted in an aqueous phase (~40%) and an organic phase (~50-60%) as well as gas phase (<5%) and coke (<2%). Study of the temperature and time upon the process showed that the degree of deoxygenation increased (from ~20 % up to 60 %) at higher temperatures in the region of 350 C and longer residence times up to 5 h. However minimum viscosity (~0.035 Pa.s) occurred at 250 C and 3 h residence time, indicating that some polymerization of the oil product occurs at the higher temperatures. Bio-Pd showed a similar degree of deoxygenation (~20 %) to Pd/C at lower temperatures of 160 C, but did not rise as steeply with temperature. More coke was formed over bio-Pd/C than Pd/C at temperatures above 250 C, suggesting that bio-Pd/C may be more susceptible to coke formation than Pd/C. Reactions occurring during bio-oil upgrading include catalytic cracking, decarbonylation, decarboxylation, hydrocracking, hydrodeoxygenation and hydrogenation. In conclusion, it was shown that bio-Pd/C displays an acceptable rate of HDO, which increases with residence time and temperature. However some undesirable reactions also occur, leading to a deleterious increase in viscosity at higher temperatures. Comparisons are also drawn with earlier work on the HDO of Chlorella derived bio-oil manufactured from micro-algae via hydrothermal liquefaction. Future work will analyze the kinetics of the reaction and investigate the effect of bi-metallic catalysts.

Keywords: bio-oil, catalyst, palladium, upgrading

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Authors: Nirmala Deenadayalu, Kwanele B. Mazibuko, Lethiwe D. Mthembu

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Sugarcane bagasse is the residue obtained after the extraction of sugar from the sugarcane. The main aim of this work was to produce catechol from sugarcane bagasse. The optimization of catechol production was investigated using a Box-Behnken design of experiments. The sugarcane bagasse was heated in a Parr reactor at a set temperature. The reactions were carried out at different temperatures (100-250) °C, catalyst loading (1% -10% KOH (m/v)) and reaction times (60 – 240 min) at 17 bar pressure. The solid and liquid fractions were then separated by vacuum filtration. The liquid fraction was analyzed for catechol using high-pressure liquid chromatography (HPLC) and characterized for the functional groups using Fourier transform infrared spectroscopy (FTIR). The optimized condition for catechol production was 175 oC, 240 min, and 10 % KOH with a catechol yield of 79.11 ppm. Since the maximum time was 240 min and 10 % KOH, a further series of experiments were conducted at 175 oC, 260 min, and 20 % KOH and yielded 2.46 ppm catechol, which was a large reduction in catechol produced. The HPLC peak for catechol was obtained at 2.5 min for the standards and the samples. The FTIR peak at 1750 cm⁻¹ was due to the C=C vibration band of the aromatic ring in the catechol present for both the standard and the samples. The peak at 3325 cm⁻¹ was due to the hydrogen-bonded phenolic OH vibration bands for the catechol. The ANOVA analysis was also performed on the set of experimental data to obtain the factors that most affected the amount of catechol produced.

Keywords: catechol, sugarcane bagasse, lignin, hydrothermal liquefaction

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Authors: Neumoin Anton Ivanovich, Opra Denis Pavlovich

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Materials based on titanium oxide compounds are widely used in such areas as solar energy, photocatalysis, food industry and hygiene products, biomedical technologies, etc. Demand for them has also formed in the battery industry (an example of this is the commercialization of Li4Ti5O12), where much attention has recently been paid to the development of next-generation systems and technologies, such as sodium-ion batteries. This dictates the need to search for new materials with improved characteristics, as well as ways to obtain them that meet the requirements of scalability. One of the ways to solve these problems can be the creation of nanomaterials that often have a complex of physicochemical properties that radically differ from the characteristics of their counterparts in the micro- or macroscopic state. At the same time, it is important to control the texture (specific surface area, porosity) of such materials. In view of the above, among other methods, the hydrothermal technique seems to be suitable, allowing a wide range of control over the conditions of synthesis. In the present study, a method was developed for the preparation of mesoporous nanostructured sodium trititanate (Na2Ti3O7) with a hierarchical architecture. The materials were synthesized by hydrothermal processing and exhibit a complex hierarchically organized two-layer architecture. At the first level of the hierarchy, materials are represented by particles having a roughness surface, and at the second level, by one-dimensional nanotubes. The products were found to have high specific surface area and porosity with a narrow pore size distribution (about 6 nm). As it is known, the specific surface area and porosity are important characteristics of functional materials, which largely determine the possibilities and directions of their practical application. Electrochemical impedance spectroscopy data show that the resulting sodium trititanate has a sufficiently high electrical conductivity. As expected, the synthesized complexly organized nanoarchitecture based on sodium trititanate with a porous structure can be practically in demand, for example, in the field of new generation electrochemical storage and energy conversion devices.

Keywords: sodium trititanate, hierarchical materials, mesoporosity, nanotubes, hydrothermal synthesis

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Authors: Chiu-Hsuan Lee, Min-Hao Yuan, Kun-Cheng Lin, Qiao-Yin Tsai, Yun-Jie Lu, Yi-Jhen Wang, Hsin-Yi Lin, Chih-Hua Hsu, Jia-Rong Jhou, Si-Ying Li, Yi-Hung Chen, Je-Lueng Shie

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Raw food waste has a high-water content. If it is incinerated, it will increase the cost of treatment. Therefore, composting or energy is usually used. There are mature technologies for composting food waste. Odor, wastewater, and other problems are serious, but the output of compost products is limited. And bakelite is mainly used in the manufacturing of integrated circuit boards. It is hard to directly recycle and reuse due to its hard structure and also difficult to incinerate and produce air pollutants due to incomplete incineration. In this study, supercritical hydrothermal and subcritical glycolysis thermal conversion technology is used to convert biomass wastes of bakelite and raw kitchen wastes to carbon materials and biofuels. Batch carbonization tests are performed under high temperature and pressure conditions of solvents and different operating conditions, including wet and dry base mixed biomass. This study can be divided into two parts. In the first part, bakelite waste is performed as dry-based industrial waste. And in the second part, raw kitchen wastes (lemon, banana, watermelon, and pineapple peel) are used as wet-based biomass ones. The parameters include reaction temperature, reaction time, mass-to-solvent ratio, and volume filling rates. The yield, conversion, and recovery rates of products (solid, gas, and liquid) are evaluated and discussed. The results explore the benefits of synergistic effects in thermal glycolysis dehydration and carbonization on the yield and recovery rate of solid products. The purpose is to obtain the optimum operating conditions. This technology is a biomass-negative carbon technology (BNCT); if it is combined with carbon capture and storage (BECCS), it can provide a new direction for 2050 net zero carbon dioxide emissions (NZCDE).

Keywords: biochar, raw food waste, bakelite, supercritical hydrothermal, subcritical glycolysis, biofuels

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Authors: I. Ben Kaddour, S. Larbaoui

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Since their first synthesis, the Silicoaluminophosphates materials have proved their efficiency as a good adsorbent and catalyst in several environmental and energetic applications. In this work, the photocatalytic hydrogen production from water splitting reactions has been conducted under visible radiations in the presence of a series of iron and/or titanium-containing microporous silico-alumino-phosphates materials synthesized by hydrothermal method, using triethylamine as an organic structuring agent to obtain the AFI structure type. These photo-catalysts were then characterized by various physicochemical methods to determine their structural, textural and morphological properties such as X-ray diffraction (XRD), Fourier transformed infrared spectroscopy (FTIR), scanning electron microscopy (SEM) coupled with X rays microanalysis, nitrogen adsorption measurements, UV-visible diffuse reflectance spectroscopy (UV-Vis-DRS), and X-rays photoelectron spectroscopy (XPS) and the analysis revealed that these materials have significant photocatalytic properties. The hydrogen production process has been followed by photoelectrochemical characterization (PEC). The results showed that hydrogen is the only gas produced, and the reaction takes place in the conduction band where water is reduced to hydrogen. The electron recombination has also been avoided, as holes are entrapped using hole scavengers. In addition, these catalysts have been shown to remain stable during reuse for up to five cycles.

Keywords: photocatalysis, SAPO-5, hydrothermal synthesis, hydrogen production

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Authors: Luís F. da Silva, Ariadne C. Catto, Osmando F. Lopes, Khalifa Aguir, Valmor R. Mastelaro, Caue Ribeiro, Elson Longo

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Gas detection is important for controlling industrial, and vehicle emissions, agricultural residues, and environmental control. In last decades, several semiconducting oxides have been used to detect dangerous or toxic gases. The excellent gas-sensing performance of these devices have been observed at high temperatures (~250 °C), which forbids the use for the detection of flammable and explosive gases. In this way, ultraviolet light activated gas sensors have been a simple and promising alternative to achieve room temperature sensitivity. Among the semiconductor oxides which exhibit a good performance as gas sensor, the zinc oxide (ZnO) and tin oxide (SnO2) have been highlighted. Nevertheless, their poor selectivity is the main disadvantage for application as gas sensor devices. Recently, heterostructures combining these two semiconductors (ZnO-SnO2) have been studied as an alternative way to enhance the gas sensor performance (sensitivity, selectivity, and stability). In this work, we investigated the influence of mass ratio Zn:Sn on the properties of ZnO-SnO2 nanocomposites prepared by hydrothermal treatment for 4 hours at 200 °C. The crystalline phase, surface, and morphological features were characterized by X-ray diffraction (XRD), high-resolution transmission electron (HR-TEM), and X-ray photoelectron spectroscopy (XPS) measurements. The gas sensor measurements were carried out at room-temperature under ultraviolet (UV) light irradiation using different ozone levels (0.06 to 0.61 ppm). The XRD measurements indicate the presence of ZnO and SnO2 crystalline phases, without the evidence of solid solution formation. HR-TEM analysis revealed that a good contact between the SnO2 nanoparticles and the ZnO nanorods, which are very important since interface characteristics between nanostructures are considered as challenge to development new and efficient heterostructures. Electrical measurements proved that the best ozone gas-sensing performance is obtained for ZnO:SnO2 (50:50) nanocomposite under UV light irradiation. Its sensitivity was around 6 times higher when compared to SnO2 pure, a traditional ozone gas sensor. These results demonstrate the potential of ZnO-SnO2 heterojunctions for the detection of ozone gas at room-temperature when irradiated with UV light irradiation.

Keywords: hydrothermal, zno-sno2, ozone sensor, uv-activation, room-temperature

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Authors: Charmaine Lamiel, Van Hoa Nguyen, Marjorie Baynosa, Jae-Jin Shim

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The depletion of non-renewable sources had led to the continuous development of various energy storage systems in order to cope with the world’s demand in energy. Supercapacitors have attracted considerable attention because they can store more energy than conventional capacitors and have higher power density than batteries. The combination of carbon-based material and metal chalcogenides are now being considered in response to the search for active electrode materials exhibiting high electrochemical performance. In this study, a hierarchical mesoporous carbon sphere@nickel cobalt sulfide (CS@Ni-Co-S) core-shell was synthesized using a simple hydrothermal method. The CS@Ni-Co-S core-shell microstructures exhibited a high capacitance of 724.4 F g−1 at 2 A g−1 in a 6 M KOH electrolyte. Good specific retention of 86.1% and high Coulombic efficiency of 97.9% was obtained after 2000 charge-discharge cycles. The electrode exhibited a high energy density of 58.0 Wh kg−1 (1440 W kg−1) and high power density of 7200 W kg−1 (34.2 Wh kg−1). The reaction involved green synthesis without further sulfurization or post-heat treatment. Through this study, a cost-effective and facile synthesis of CS@Ni-Co-S as an active electrode showed favorable electrochemical performance.

Keywords: carbon sphere, electrochemical, hydrothermal, nickel cobalt sulfide, supercapacitor

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Authors: Ghodratollah Rostami Paydar

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The Baba-Ali and Galali iron deposits are located in northwest Hamedan and the Iranian Sanandaj-Sirjan geological structural zone. The host rocks of these deposits are metavolcanosedimentary successions of Songhor stratigraphic series with permo-trriassic age. Field investigation, ore geometry, textures and structures and paragenetic sequence of minerals, all indicate that the ore minerals are crystallized in four stages: primary volcanosedimentary stage, secondary regional metamorphism with formation of ductile shear zones, contact metamorphism and metasomatism stage and the finally late hydrothermal mineralization within uplift and exposure. Totally 29 samples of sulfide, oxide-silicate and carbonate minerals of iron orees and gangue has been purified for stable isotope analysis. The isotope ratio data assure that occurrence of dynamothermal metamorphism in these areas typically involves a lengthy period of time, which results in a tendency toward isotopic homogenization specifically in O and H stable isotopes and showing the role of metamorphic waters in mineralization process. Measurement of δ34S (CDT) in first generation of pyrite is higher than another ones, so it confirms the volcanogenic origin of primary iron mineralization. δ13C data measurements in Galali carbonate country rocks show a marine origin. δ18O in magnetite and skarn forming silicates, δ18O and δ13C in limestone and skarn calcite and δ34S in sulphides are all consistent with the interaction of a magmatic-equilibrated fluid with Galali limestone, and a dominantly magmatic source for S. All these data imply skarn formation and mineralisation in a magmatic-hydrothermal system that maintained high salinity to relatively late stages resulting in the formation of the regional Na metasomatic alteration halo. Late stage hydrothermal quartz-calcite veinlets are important for gold mineralization, but the economic evaluation is required to detailed geochemical studies.

Keywords: iron, polygenetic, stable isotope, BabaAli, Galali

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Authors: Natasha Khan, Muhammad Arif

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The Chakdara granite gneiss is an extension of Swat granite gneisses. It is characterized by biotite bands and the occurrence of fluorite and blue beryl. Younger phases (quartzofeldspathic veins) occur within gneisses are characterized by various mineral phases that include beryl, biotite, phlogopite, annite, muscovite, ilmenite-pyrophanite, monazite, zircon, apatite, magnetite and minor amounts of sphene, rutile, and ulvöspinel. The present paper is an attempt to address the detailed mineral chemistry and genesis of minerals occurring in these younger phases. These quartzofeldspathic veins are assumed to be of hydrothermal origin on the basis of Th2O content in monazite, Zr/Hf ratio in zircon, REE enrichment, and Ce/Y ratio of allanite. Biotite in the present study is characterized by high F content. Muscovite is phengitic and contains very high amounts of Fe as compared to the normal muscovites. The Th2O content for monazite is low (0.81-1.56 wt. %) like those of hydrothermal origin. The Zr/Hf ratio in zircon is variable for different analyses but mostly falls in the range of ~ 41 and above. Allanite is generally unaltered and characterized by LREE enrichment. The properties of beryl and columbite in the present study show pegmatitic features.

Keywords: Beryl, Chakdarra granite gneiss, micas, quartzofeldspathic veins

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Authors: K. Saravanan, K. A.Rameshkumar, P. Maadeswaran

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The depletion of fossil resources and the rise in global temperatures are two of the most important concerns we confront today. There are numerous renewable energy sources like solar power, tidal power, wind energy, radiant energy, hydroelectricity, geothermal energy, and biomass available to generate the needed energy demand. Engineers and scientists around the world are facing a massive barrier in the development of storage technologies for the energy developed from renewable energy sources. The development of electrochemical capacitors as a future energy storage technology is at the forefront of current research and development. This is due to the fact that the electrochemical capacitors have a significantly higher energy density, a faster charging-discharging rate, and a longer life span than capacitors, and they also have a higher power density than batteries, making them superior to both. In this research, electrochemical capacitors using the Nd2O3/Mn3O4/ N-rGO electrode material is chosen since the of hexagonal and tetragonal crystal structures of Nd2O3 and Mn3O4 and also has cycling stability of 68% over a long time at 50mVs-1 and a high coulombic efficiency of 99.64% at 5 Ag-1. This approach may also be used to create novel electrode materials with improved electrochemical and cyclic stability for high-performance supercapacitors.

Keywords: Nd2O3/Mn3O4/N-rGO, nanocomposites, hydrothermal method, electrode material, specific capacitance, use of supercapacitors

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Authors: Getachew Kuma Watiro

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The need for solar energy is constantly increasing and it is widely available on the earth’s surface. Photovoltaic technology is one of the most capable of all viable energy technology and is seen as a promising approach to the control era as it is readily available and has zero carbon emissions. Inexpensive and versatile solar cells have achieved the conversion efficiency and long life of dye-sensitized solar cells, improving the conversion efficiency from the sun to electricity. DSSCs have received a lot of attention for Various potential commercial uses, such as mobile devices and portable electronic devices, as well as integrated solar cell modules. The systematic reviews were used to show the critical impact of additive C-dots in the Dye-Sensitized solar cell for energy application technology. This research focuses on the following methods to synthesize nanoparticles such as facile, polyol, calcination, and hydrothermal technique. In addition to these, there are additives C-dots by the Hydrothermal method. This study deals with the progressive development of DSSC in photovoltaic technology. The applications of single and heterojunction structure technology devices were used (ZnO, NiO, SnO2, and NiO/ZnO/N719) and applied some additives C-dots (ZnO/C-dots /N719, NiO/C-dots /N719, SnO2 /C-dots /N719 and NiO/ZnO/C-dots/N719) and the effects of C-dots were reviewed. More than all, the technology of DSSC with C-dots enhances efficiency. Finally, recommendations have been made for future research on the application of DSSC with the use of these additives.

Keywords: dye-sensitized solar cells, heterojunction’s structure, carbon dot, conversion efficiency

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Authors: Sarai Guerrero, Lijia Liu

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Zinc gallogermanate (ZGGO) is a persistent phosphor that can emit in the near infrared (NIR) range once dopped with Cr³⁺ enabling its use for in-vivo deep-tissue bio-imaging. Such a property also allows for its application in cancer diagnosis and therapy. Given this, work into developing a synthetic procedure that can be done using common laboratory instruments and equipment as well as understanding ZGGO overall, is in demand. However, the ZGGO nanoparticles must have a size compatible for cell intake to occur while still maintaining sufficient photoluminescence. The nanoparticle must also be made biocompatible by functionalizing the surface for hydrophilic solubility and for high particle uniformity in the final product. Additionally, most research is completed on doped ZGGO, leaving a gap in understanding the base form of ZGGO. It also leaves a gap in understanding how doping affects the synthesis of ZGGO. In this work, the first step of optimizing the particle size via the crystalline size of ZGGO was done with undoped ZGGO using the organic acid, oleic acid (OA) for organic ligand-assisted biphasic hydrothermal synthesis. The effects of this synthesis procedure on ZGGO’s crystallinity were evaluated using Powder X-Ray Diffraction (PXRD). OA was selected as the capping ligand as experiments have shown it beneficial in synthesizing sub-10 nm zinc gallate (ZGO) nanoparticles as well as palladium nanocrystals and magnetite (Fe₃O₄) nanoparticles. Later it is possible to substitute OA with a different ligand allowing for hydrophilic solubility. Attenuated Total Reflection Fourier-Transform Infrared (ATR-FTIR) was used to investigate the surface of the nanoparticle to investigate and verify that OA had capped the nanoparticle. PXRD results showed that using this procedure led to improved crystallinity, comparable to the high-purity reagents used on the ZGGO nanoparticles. There was also a change in the crystalline size of the ZGGO nanoparticles. ATR-FTIR showed that once capped ZGGO cannot be annealed as doing so will affect the OA. These results point to this new procedure positively affecting the crystallinity of ZGGO nanoparticles. There are also repeatable implying the procedure is a reliable source of highly crystalline ZGGO nanoparticles. With this completed, the next step will be working on substituting the OA with a hydrophilic ligand. As these ligands effect the solubility of the nanoparticle as well as the pH that the nanoparticles can dissolve in, further research is needed to verify which ligand is best suited for preparing ZGGO for bio-imaging.

Keywords: biphasic hydrothermal synthesis, crystallinity, oleic acid, zinc gallogermanate

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Authors: Kun Liang Ang, Eng Toon Saw, Wei He, Xuecheng Dong, Seeram Ramakrishna

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Ester solvents are widely used in pharmaceutical, printing and flavor industry due to their good miscibility, low toxicity, and high volatility. Through pervaporation, these ester solvents can be recovered from industrial wastewater. While metal-doped silicalite 1 zeolite membranes are commonly used in organic solvent recovery in the pervaporation process, these ceramic membranes suffer from low membrane permeation flux, mainly due to the high thickness of the metal-doped zeolite membrane. Herein, a simple method of fabricating an ultrathin tin-silicalite 1 membrane supported on alumina tube is reported. This ultrathin membrane is able to achieve high permeation flux and separation factor for an ester in a diluted aqueous solution. Nanosized tin-Silicalite 1 seeds which are smaller than 500nm has been formed through hydrothermal synthesis. The sn-Silicalite 1 seeds were then seeded onto alumina tube through dip coating, and the tin-Silicalite 1 membrane was then formed by hydrothermal synthesis in an autoclave through secondary growth method. Multiple membrane synthesis factors such as seed size, ceramic substrate surface pore size selection, and secondary growth conditions were studied for their effects on zeolite membrane growth. The microstructure, morphology and the membrane thickness of tin-Silicalite 1 zeolite membrane were examined. The membrane separation performance and stability will also be reported.

Keywords: ceramic membrane, pervaporation, solvent recovery, Sn-MFI zeolite

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Authors: Thiago Ribeiro de Alencar, Jacyro Gramulia Junior, Patricia Teixeira Leite

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The area of the electricity sector that deals with energy needs by the hydroelectric in a coordinated manner is called Operation Planning of Hydrothermal Power Systems (OPHPS). The purpose of this is to find a political operative to provide electrical power to the system in a given period, with reliability and minimal cost. Therefore, it is necessary to determine an optimal schedule of generation for each hydroelectric, each range, so that the system meets the demand reliably, avoiding rationing in years of severe drought, and that minimizes the expected cost of operation during the planning, defining an appropriate strategy for thermal complementation. Several optimization algorithms specifically applied to this problem have been developed and are used. Although providing solutions to various problems encountered, these algorithms have some weaknesses, difficulties in convergence, simplification of the original formulation of the problem, or owing to the complexity of the objective function. An alternative to these challenges is the development of techniques for simulation optimization and more sophisticated and reliable, it can assist the planning of the operation. Thus, this paper presents the development of a computational tool, namely Hydro-IA for solving optimization problem identified and to provide the User an easy handling. Adopted as intelligent optimization technique is Genetic Algorithm (GA) and programming language is Java. First made the modeling of the chromosomes, then implemented the function assessment of the problem and the operators involved, and finally the drafting of the graphical interfaces for access to the User. The results with the Genetic Algorithms were compared with the optimization technique nonlinear programming (NLP). Tests were conducted with seven hydroelectric plants interconnected hydraulically with historical stream flow from 1953 to 1955. The results of comparison between the GA and NLP techniques shows that the cost of operating the GA becomes increasingly smaller than the NLP when the number of hydroelectric plants interconnected increases. The program has managed to relate a coherent performance in problem resolution without the need for simplification of the calculations together with the ease of manipulating the parameters of simulation and visualization of output results.

Keywords: energy, optimization, hydrothermal power systems, artificial intelligence and genetic algorithms

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Authors: Bagnoud-Velásquez Mariluz, Damergi Eya, Grandjean Dominique, Frédéric Vogel, Ludwig Christian

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The sustainability of algae to biofuel processes is seriously affected by the energy intensive production of fertilizers. Large amounts of nitrogen and phosphorus are required for a large-scale production resulting in many cases in a negative impact of the limited mineral resources. In order to meet the algal bioenergy opportunity it appears crucial the promotion of processes applying a nutrient recovery and/or making use of renewable sources including waste. Hydrothermal (HT) conversion is a promising and suitable technology for microalgae to generate biofuels. Besides the fact that water is used as a “green” reactant and solvent and that no biomass drying is required, the technology offers a great potential for nutrient recycling. This study evaluated the possibility to treat the water HT effluent by the growth of microalgae while producing renewable algal biomass. As already demonstrated in previous works by the authors, the HT aqueous product besides having N, P and other important nutrients, presents a small fraction of organic compounds rarely studied. Therefore, extracted heteroaromatic compounds in the HT effluent were the target of the present research; they were profiled using GC-MS and LC-MS-MS. The results indicate the presence of cyclic amides, piperazinediones, amines and their derivatives. The most prominent nitrogenous organic compounds (NOC’s) in the extracts were carefully examined by their effect on microalgae, namely 2-pyrrolidinone and β-phenylethylamine (β-PEA). These two substances were prepared at three different concentrations (10, 50 and 150 ppm). This toxicity bioassay used three different microalgae strains: Phaeodactylum tricornutum, Chlorella sorokiniana and Scenedesmus vacuolatus. The confirmed IC50 was for all cases ca. 75ppm. Experimental conditions were set up for the growth of microalgae in the aqueous phase by adjusting the nitrogen concentration (the key nutrient for algae) to fit that one established for a known commercial medium. The values of specific NOC’s were lowered at concentrations of 8.5 mg/L 2-pyrrolidinone; 1mg/L δ-valerolactam and 0.5 mg/L β-PEA. The growth with the diluted HT solution was kept constant with no inhibition evidence. An additional ongoing test is addressing the possibility to apply an integrated water cleanup step making use of the existent hydrothermal catalytic facility.

Keywords: hydrothermal process, microalgae, nitrogenous organic compounds, nutrient recovery, renewable biomass

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Authors: Melanie Francois, Gilles Caboche, Frederic Demoisson, Francois Maeght, Maria Paola Carpanese, Lionel Combemale, Pascal Briois

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Finding new clean, and efficient way for energy production is one of the actual global challenges. Advances in fuel cell technology have shown that, for few years, Protonic Ceramic Fuel Cell (PCFC) has attracted much attention in the field of new hydrogen energy thanks to their lower working temperature, possible higher efficiency, and better durability than classical SOFC. On the contrary of SOFC, where O²⁻ oxygen ion is the charge carrier, PCFC works with H⁺ proton as a charge carrier. Consequently, the lower activation energy of proton diffusion compared to the one of oxygen ion explains those benefits and allows PCFC to work in the 400-600°C temperature range. Doped-BaCeO₃ is currently the most chosen material for this application because of its high protonic conductivity; for example, BaCe₀.₉Y₀.₁O₃ δ exhibits a total conductivity of 1.5×10⁻² S.cm⁻¹ at 600°C in wet H₂. However, BaCeO₃ based perovskite has low stability in H₂O and/or CO₂ containing atmosphere, which limits their practical application. On the contrary, BaZrO₃ based perovskite exhibits good chemical stability but lower total conductivity than BaCeO₃ due to its larger grain boundary resistance. By substituting zirconium with 20% of yttrium, it is possible to achieve a total conductivity of 2.5×10⁻² S.cm⁻¹ at 600°C in wet H₂. However, the high refractory property of BaZr₀.₈Y₀.₂O₃-δ (noted BZY20) causes problems to obtain a dense membrane with large grains. Thereby, using a synthesis process that gives fine particles could allow better sinterability and thus decrease the number of grain boundaries leading to a higher total conductivity. In this work, BaZr₀.₈Y₀.₂O₃-δ have been synthesized by classical batch hydrothermal device and by a continuous hydrothermal device developed at ICB laboratory. The two variants of this process are able to work in supercritical conditions, leading to the formation of nanoparticles, which could be sintered at a lower temperature. The as-synthesized powder exhibits the right composition for the perovskite phase, impurities such as BaCO₃ and YO-OH were detected at very low concentration. Microstructural investigation and densification rate measurement showed that the addition of 1 wt% of ZnO as sintering aid and a sintering at 1550°C for 5 hours give high densified electrolyte material. Furthermore, it is necessary to heat the synthesized powder prior to the sintering to prevent the formation of secondary phases. It is assumed that this thermal treatment homogenizes the crystal structure of the powder and reduces the number of defects into the bulk grains. Electrochemical impedance spectroscopy investigations in various atmospheres and a large range of temperature (200-700°C) were then performed on sintered samples, and the protonic conductivity of BZY20 has been highlighted. Further experiments on half-cell, NiO-BZY20 as anode and BZY20 as electrolyte, are in progress.

Keywords: hydrothermal synthesis, impedance measurement, Y-doped BaZrO₃, proton conductor

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Authors: Zehui Du, Chaiwat Prapainainar, Paisan Kongkachuichay, Paweena Prapainainar

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The aim of this work was to obtain small crystalline size and high crystallinity of mordenites and analcimes, by modifying the aging time, agitation, water content, crystallization temperature and crystallization time. Two different hydrothermal methods were studied. Both methods used Na2SiO3 as the silica source, NaAlO2 as the aluminum source, and NaOH as the alkali source. The first method used HMI as the template while the second method did not use the template. Mordenite crystals with spherical shape and bimodal in size of about 1 and 5 µm were obtained from the first method using conditions of 24 hr aging time, 170°C and 24 hr crystallization. Modernites with high crystallinity were formed using agitation system in the crystallization process. It was also found that the aging time of 2 hr and 24 hr did not much affect the formation of mordenite crystals. Analcime crystals were formed in spherical shape and facet on surface with the size between 13-15 µm by the second method using the conditions of 30 minutes aging time, 170°C and 24 hr crystallization without calcination. By increasing water content, the crystallization process was slowed down and resulted in smaller analcime crystals. Larger size of analcime crystals were observed when the samples were calcined at 300°C and 580°C. Higher calcination temperature led to higher crystal growth and resulted in larger crystal size. Finally, mordenite and analcime was used as fillers in zeolite/Nafion composite membrane to solve the fuel cross over problem in direct alcohol fuel cell.

Keywords: analcime, hydrothermal synthesis, mordenite, zeolite

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Authors: Manish Saha, Manish Kumar Niranjan, Saket Asthana

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The K₀.₅Na₀.₅NbO₃ (KNN) system has emerged as one of the most promising lead-free piezoelectric over the years. In this work, we perform a comprehensive investigation of electronic structure, lattice dynamics and dielectric/ferroelectric properties of the room temperature phase of KNN by combining ab-initio DFT-based theoretical analysis and experimental characterization. We assign the symmetry labels to KNN vibrational modes and obtain ab-initio polarized Raman spectra, Infrared (IR) reflectivity, Born-effective charge tensors, oscillator strengths etc. The computed Raman spectrum is found to agree well with the experimental spectrum. In particular, the results suggest that the mode in the range ~840-870 cm-¹ reported in the experimental studies is longitudinal optical (LO) with A_1 symmetry. The Raman mode intensities are calculated for different light polarization set-ups, which suggests the observation of different symmetry modes in different polarization set-ups. The electronic structure of KNN is investigated, and an optical absorption spectrum is obtained. Further, the performances of DFT semi-local, metal-GGA and hybrid exchange-correlations (XC) functionals, in the estimation of KNN band gaps are investigated. The KNN bandgap computed using GGA-1/2 and HSE06 hybrid functional schemes are found to be in excellant agreement with the experimental value. The COHP, electron localization function and Bader charge analysis is also performed to deduce the nature of chemical bonding in the KNN. The solid-state reaction and hydrothermal methods are used to prepare the KNN ceramics, and the effects of grain size on the physical characteristics these ceramics are examined. A comprehensive study on the impact of different synthesis techniques on the structural, electrical, and photocatalytic properties of ferroelectric ceramics KNN. The KNN-S prepared by solid-state method have significantly larger grain size as compared to that for KNN-H prepared by hydrothermal method. Furthermore, the KNN-S is found to exhibit higher dielectric, piezoelectric and ferroelectric properties as compared to KNN-H. On the other hand, the increased photocatalytic activity is observed in KNN-H as compared to KNN-S. As compared to the hydrothermal synthesis, the solid-state synthesis causes an increase in the relative dielectric permittivity (ε^') from 2394 to 3286, remnant polarization (P_r) from 15.38 to 20.41 μC/cm^², planer electromechanical coupling factor (k_p) from 0.19 to 0.28 and piezoelectric coefficient (d_33) from 88 to 125 pC/N. The KNN-S ceramics are also found to have a lower leakage current density, and higher grain resistance than KNN-H ceramic. The enhanced photocatalytic activity of KNN-H is attributed to relatively smaller particle sizes. The KNN-S and KNN-H samples are found to have degradation efficiencies of RhB solution of 20% and 65%, respectively. The experimental study highlights the importance of synthesis methods and how these can be exploited to tailor the dielectric, piezoelectric and photocatalytic properties of KNN. Overall, our study provides several bench-mark important results on KNN that have not been reported so far.

Keywords: lead-free piezoelectric, Raman intensity spectrum, electronic structure, first-principles calculations, solid state synthesis, photocatalysis, hydrothermal synthesis

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Authors: Nabat Gojaeva, Mikayil Naghiyev, Sultan Jafarov, Gular Mikayilova

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Chovdar ore area is located in the contact of Dashkesan caldera and Shamkir horst-graben uplift, which comprises the central part of Lok-Karabakh Island arcs of South Caucasus metallogenic province in terms of regional tectonics. One of the main structural features of formation of the Mereh and Aghyokhush group of low sulfidation epithermal gold deposits, locating in the north peripheric part of the ore area, is involving the crossing areas of ore-hosting and ore-forming Pan-Caucasian-direction structurally-compound faults with the meridional, rhombically shaped faults. In addition, another significant feature is the temporally two- or three-stage ore formation. In the first stage -an early phase of Upper Bathonian age, sulfides are the dominant minerals, in the second stage- late ‘productive’ phase of Upper Bathonian age, mainly gold mineralization is formed. Also, in the Upper Jurassic – Lower Cretaceous ages, rarely-encountered Cu-polymetallic ore formations are documented. Finally, in the last stage, the re-dislocation of ore-formation is foreseen in the previously-formed mineralization areas. The faults in the strike and dip directions formed shearing, brecciation, sulfide mineralization aureoles, and hydrothermal alteration zones in the wall rocks along with the local depression blocks. The geological-structural analysis of the area shows that multiple and various morphogenetic volcano-tectonically fault systems have developed in the area. These fault systems have played a trap role for ore-formation in the intersected parts of faults mentioned above. Thus, in the referred parts, mostly predominance of felsic volcanism and metasomatic alteration (silicification, argillitic, etc.) of wall rocks, as well as the products of this volcanism, account for the inclusion of hydrothermal ore-forming fluids along these faults. It is possible to determine temporally and lithological-structural connection between the ore-formation along with local depression blocks and faults as borders for products of felsic volcanism of Upper Cretaceous-Lesser Jurassic ages, in the results of the replacement of hydrothermal alteration zones with relatively low-temperature metasomatic alterations while moving from the felsic parts to the margins, and due to being non-ore bearing intermediate and intermediate-felsic magmatic facies.

Keywords: Aghyokhush, fault, gold deposit, Mereh

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Authors: Brizita Djordjevic, Bojana Vidovic, Milica Zrnic, Uros Cakar, Ivan Stankovic, Davor Korcok, Sladjana Sobajic

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Histamine is a biogenic amine, which is formed by enzymatic decarboxylation from the amino acid histidine. It can be found in foods such as fish and fish products, meat and fermented meat products, cheese, wine and beer. The presence of histamine in these foods can indicate microbiological spoilage or poor manufacturing processes. The consumption of food containing large amounts of histamine can have toxicological consequences. In 62 food products (31 canned fish products, 19 wines and 12 cheeses) from the market of Serbia the content of histamine was determined using enzyme-linked immunosorbent assay (ELISA) test kit according to the manufacturer's instructions (Immunolab GmbH, Kassel, Germany). The detection limits of this assay were 20 µg/kg for fish and cheese and 4 µg/L for wine. The concentration of histamine varied between 0.16-207 mg/kg in canned fish products, 0.03-1.47 mg/kg in cheeses and 0.01- 0.18 mg/L in wines. In all analyzed canned fish products the results obtained for the histamine were below the limits set by European and national legislation, so they can be considered acceptable and safe for the health consumers. The levels of histamine in analyzed cheeses and wines were very low and did not pose safety concerns.

Keywords: cheese, enzyme-linked immunosorbent assay, histamine, fish products, wine

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Authors: Atef Y. Shenouda, Anton A. Momchilov

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Graphene and CdO with different stoichiometric ratios of Cd(CH₃COO)₂ and graphene samples were prepared by hydrothermal reaction. The crystalline phases of pure CdO and 3CdO:1graphene were identified by X-ray diffraction (XRD). The particle morphology was studied with SEM. Furthermore, impedance measurements were applied. Galvanostatic measurements for the cells were carried out using potential limits between 0.01 and 3 V vs. Li/Li⁺. The current cycling intensity was 10⁻⁴ A. The specific discharge capacity of 3CdO-1G cell was about 450 Ah.Kg⁻¹ up to more than 100 cycles.

Keywords: CdO, graphene, negative electrode, lithium battery

Procedia PDF Downloads 123

Authors: Vera Marcantonio, Marcello De Falco, Mauro Capocelli, Álvaro Amado-Fierro, Teresa A. Centeno, Enrico Bocci

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Concerns about energy security, energy prices, and climate change led scientific research towards sustainable solutions to fossil fuel as renewable energy sources coupled with hydrogen as an energy vector and carbon capture and conversion technologies. Among the technologies investigated in the last decades, biomass gasification acquired great interest owing to the possibility of obtaining low-cost and CO₂ negative emission hydrogen production from a large variety of everywhere available organic wastes. Upstream and downstream treatment were then studied in order to maximize hydrogen yield, reduce the content of organic and inorganic contaminants under the admissible levels for the technologies which are coupled with, capture, and convert carbon dioxide. However, studies which analyse a whole process made of all those technologies are still missing. In order to fill this lack, the present paper investigated the coexistence of hydrothermal carbonization (HTC), sorption enhance gasification (SEG), hot gas cleaning (HGC), and CO₂ conversion by dielectric barrier discharge (DBD) plasma reactor for H₂ production from biomass waste by means of Aspen Plus software. The proposed model aimed to identify and optimise the performance of the plant by varying operating parameters (such as temperature, CaO/biomass ratio, separation efficiency, etc.). The carbon footprint of the global plant is 2.3 kg CO₂/kg H₂, lower than the latest limit value imposed by the European Commission to consider hydrogen as “clean”, that was set to 3 kg CO₂/kg H₂. The hydrogen yield referred to the whole plant is 250 gH₂/kgBIOMASS.

Keywords: biomass gasification, hydrogen, aspen plus, sorption enhance gasification

Procedia PDF Downloads 43

Authors: Marcin Zielinski, Marcin Debowski, Paulina Rusanowska, Magda Dudek

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As a result of sonification, the destruction of complex biomass structures results in an increase in the biogas yield from the conditioned material. First, the amount of organic matter released into the solution due to disintegration was determined. This parameter was determined by changes in the carbon content in liquid phase of the conditioned substrate. The amount of carbon in the liquid phase increased with the prolongation of the sonication time to 16 min. Further increase in the duration of sonication did not cause a statistically significant increase in the amount of organic carbon in the liquid phase. The disintegrated material was then used for respirometric measurements for determination of the impact of the conditioning process used on methane fermentation effectiveness. The relationship between the amount of energy introduced into the lignocellulosic substrate and the amount of biogas produced has been demonstrated. Statistically significant increase in the amount of biogas was observed until sonication of 16 min. Further increase in energy in the conditioning process did not significantly increase the production of biogas from the treated substrate. The biogas production from the conditioned substrate was 17% higher than from the reference biomass at that time. The ultrasonic disintegration method did not significantly affect the observed biogas composition. In all series, the methane content in the produced biogas from the conditioned substrate was similar to that obtained with the raw substrate sample (51.1%). Another method of substrate conditioning was hydrothermal depolymerization. This method consists in application of increased temperature and pressure to substrate. These phenomena destroy the structure of the processed material, the release of organic compounds to the solution, which should lead to increase the amount of produced biogas from such treated biomass. The hydrothermal depolymerization was conducted using an innovative microwave heating method. Control measurements were performed using conventional heating. The obtained results indicate the relationship between depolymerization temperature and the amount of biogas. Statistically significant value of the biogas production coefficients increased as the depolymerization temperature increased to 150°C. Further raising the depolymerization temperature to 180°C did not significantly increase the amount of produced biogas in the respirometric tests. As a result of the hydrothermal depolymerization obtained using microwave at 150°C for 20 min, the rate of biogas production from the Sida silage was 780 L/kg VS, which accounted for nearly 50% increase compared to 370 L/kg VS obtained from the same silage but not depolymerised. The study showed that by microwave heating it is possible to effectively depolymerized substrate. Significant differences occurred especially in the temperature range of 130-150ºC. The pre-treatment of Sida hermaphrodita silage (biogas substrate) did not significantly affect the quality of the biogas produced. The methane concentration was about 51.5% on average. The study was carried out in the framework of the project under program BIOSTRATEG funded by the National Centre for Research and Development No. 1/270745/2/NCBR/2015 'Dietary, power, and economic potential of Sida hermaphrodita cultivation on fallow land'.

Keywords: disintegration, biogas, methane fermentation, Virginia fanpetals, biomass

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Authors: Atef Y. Shenouda, Fei Xu

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Cu₃SbS₃ (CAS) was synthesized by direct solid-state reaction from elementary Cu, Sb, & S and hydrothermal reaction using thioacetamide (TAM). Crystal structure and morphology for the prepared phases of Cu₃SbS₃ were studied via X-ray diffraction (XRD) and field emission scanning electron microscope (FESEM). The band gap energies are 2 and 2.2 eV for the prepared samples. The two samples are as anode for Na ion storage. They show high initial capacity to 490 mAh/g. Na cell prepared from TAM sample shows 280 mAh/g after 25 cycles vs. 60 mAh/g for elemental sample.

Keywords: Cu3SbS3, sodium batteries, thioacetamide, sulphur sources

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Authors: Doaa Hamdi, Ahmed Hashem

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The present study aims at integrating the ASTER data and Landsat 8 data to discriminate and map alteration and/or mineralization zones in addition to delineating different lithological units of Humr Akarim Granites area. The study area is located at 24º9' to 24º13' N and 34º1' to 34º2'45"E., covering a total exposed surface area of about 17 km². The area is characterized by rugged topography with low to moderate relief. Geologic fieldwork and petrographic investigations revealed that the basement complex of the study area is composed of metasediments, mafic dikes, older granitoids, and alkali-feldspar granites. Petrographic investigations revealed that the secondary minerals in the study area are mainly represented by chlorite, epidote, clay minerals and iron oxides. These minerals have specific spectral signatures in the region of visible near-infrared and short-wave infrared (0.4 to 2.5 µm). So that the ASTER imagery processing was concentrated on VNIR-SWIR spectrometric data in order to achieve the purposes of this study (geologic mapping of hydrothermal alteration zones and delineate possible radioactive potentialities). Mapping of hydrothermal alterations zones in addition to discriminating the lithological units in the study area are achieved through the utilization of some different image processing, including color band composites (CBC) and data transformation techniques such as band ratios (BR), band ratio codes (BRCs), principal component analysis(PCA), Crosta Technique and minimum noise fraction (MNF). The field verification and petrographic investigation confirm the results of ASTER imagery and Landsat 8 data, proposing a geological map (scale 1:50000).

Keywords: remote sensing, petrography, mineralization, alteration detection

Procedia PDF Downloads 129

Authors: Daniel F. Sava, Anton Ficai, Bogdan S. Vasile, Georgeta Voicu, Ecaterina Andronescu

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The energy crisis and environmental contamination are very serious problems, therefore searching for better and sustainable renewable energy is a must. It is predicted that the global energy demand will double until 2050. Solar water splitting and photocatalysis are considered as one of the solutions to these issues. The use of oxide semiconductors for solar water splitting and photocatalysis started in 1972 with the experiments of Fujishima and Honda on TiO2 electrodes. Since then, the evolution of nanoscience and characterization methods leads to a better control of size, shape and properties of materials. Although the past decade advancements are astonishing, for these applications the properties have to be controlled at a much finer level, allowing the control of charge-carrier lives, energy level positions, charge trapping centers, etc. Graphene has attracted a lot of attention, since its discovery in 2004, due to the excellent electrical, optical, mechanical and thermal properties that it possesses. These properties make it an ideal support for photocatalysts, thus graphene composites with oxide semiconductors are of great interest. We present in this work the synthesis and characterization of graphene-related materials and oxide semiconductors and their different composites. These materials can be used in constructing devices for different applications (batteries, water splitting devices, solar cells, etc), thus showing their application flexibility. The synthesized materials are different morphologies and sizes of TiO2, ZnO and Fe2O3 that are obtained through hydrothermal, sol-gel methods and graphene oxide which is synthesized through a modified Hummer method and reduced with different agents. Graphene oxide and the reduced form could also be used as a single material for transparent conductive films. The obtained single materials and composites were characterized through several methods: XRD, SEM, TEM, IR spectroscopy, RAMAN, XPS and BET adsorption/desorption isotherms. From the results, we see the variation of the properties with the variation of synthesis parameters, size and morphology of the particles.

Keywords: composites, graphene, hydrothermal, renewable energy

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Authors: Iris Vural Gursel, Andrea Ramirez

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Effective utilization of lignin is an important mean for developing economically profitable biorefineries. Current literature suggests that large amounts of lignin will become available in second generation biorefineries. New conversion technologies will, therefore, be needed to carry lignin transformation well beyond combustion to produce energy, but towards high-value products such as chemicals and transportation fuels. In recent years, significant progress on catalysis has been made to improve transformation of lignin, and new catalytic processes are emerging. In this work, a techno-economic assessment of two of these novel conversion routes and comparison with more established lignin pyrolysis route were made. The aim is to provide insights into the potential performance and potential hotspots in order to guide the experimental research and ease the commercialization by early identifying cost drivers, strengths, and challenges. The lignin conversion routes selected for detailed assessment were: (non-catalytic) lignin pyrolysis as the benchmark, direct hydrodeoxygenation (HDO) of lignin and hydrothermal lignin depolymerisation. Products generated were mixed oxygenated aromatic monomers (MOAMON), light organics, heavy organics, and char. For the technical assessment, a basis design followed by process modelling in Aspen was done using experimental yields. A design capacity of 200 kt/year lignin feed was chosen that is equivalent to a 1 Mt/y scale lignocellulosic biorefinery. The downstream equipment was modelled to achieve the separation of the product streams defined. For determining external utility requirement, heat integration was considered and when possible gasses were combusted to cover heating demand. The models made were used in generating necessary data on material and energy flows. Next, an economic assessment was carried out by estimating operating and capital costs. Return on investment (ROI) and payback period (PBP) were used as indicators. The results of the process modelling indicate that series of separation steps are required. The downstream processing was found especially demanding in the hydrothermal upgrading process due to the presence of significant amount of unconverted lignin (34%) and water. Also, external utility requirements were found to be high. Due to the complex separations, hydrothermal upgrading process showed the highest capital cost (50 M€ more than benchmark). Whereas operating costs were found the highest for the direct HDO process (20 M€/year more than benchmark) due to the use of hydrogen. Because of high yields to valuable heavy organics (32%) and MOAMON (24%), direct HDO process showed the highest ROI (12%) and the shortest PBP (5 years). This process is found feasible with a positive net present value. However, it is very sensitive to the prices used in the calculation. The assessments at this stage are associated with large uncertainties. Nevertheless, they are useful for comparing alternatives and identifying whether a certain process should be given further consideration. Among the three processes investigated here, the direct HDO process was seen to be the most promising.

Keywords: biorefinery, economic assessment, lignin conversion, process design

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Authors: W. Ketren, J. Wannapeera, Z. Heishun, A. Ryuichi, K. Toshiteru, M. Kouichi, O. Hideaki

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Degradative solvent extraction is the method developed for biomass upgrading by dewatering and fractionation of biomass under the mild condition. However, the conversion mechanism of the degradative solvent extraction method has not been fully understood so far. The rice straw was treated in 1-methylnaphthalene (1-MN) at a different solvent-treatment temperature varied from 250 to 350 ^oC with the residence time for 60 min. The liquid membrane-Fourier Transform Infrared Spectroscopy (FTIR) technique is applied to study the processing mechanism in-depth without separation of the solvent. It has been found that the strength of the oxygen-hydrogen stretching  (3600-3100 cm^-1) decreased slightly with increasing temperature in the range of 300-350 ^oC. The decrease of the hydroxyl group in the solvent soluble suggested dehydration reaction taking place between 300 and 350 ^oC. FTIR spectra in the carbonyl stretching region (1800-1600 cm^-1) revealed the presence of esters groups, carboxylic acid and ketonic groups in the solvent-soluble of biomass. The carboxylic acid increased in the range of 200 to 250 ^oC and then decreased. The prevailing of aromatic groups showed that the aromatization took place during extraction at above 250 ^oC. From 300 to 350 ^oC, the carbonyl functional groups in the solvent-soluble noticeably decreased. The removal of the carboxylic acid and the decrease of esters into the form of carbon dioxide indicated that the decarboxylation reaction occurred during the extraction process.

Keywords: biomass waste, degradative solvent extraction, mechanism, upgrading

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Authors: Karen Fuchs, Michael Prokein, Nils Mölders, Manfred Renner, Eckhard Weidner

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Due to the high CO₂ emissions, the energy consumption for the production of sand-lime bricks is of great concern. Especially the production of quicklime from limestone and the energy consumption for hydrothermal curing contribute to high CO₂ emissions. Hydrothermal curing is carried out under a saturated steam atmosphere at about 15 bar and 200°C for 12 hours. Therefore, we are investigating the opportunity to replace quicklime and sand in the production of building materials with different types of slag as calcium-rich waste from steel production. We are also investigating the possibility of substituting conventional hydrothermal curing with CO₂ curing. Six different slags (Linz-Donawitz (LD), ferrochrome (FeCr), ladle (LS), stainless steel (SS), ladle furnace (LF), electric arc furnace (EAF)) provided by "thyssenkrupp MillServices & Systems GmbH" were ground at "Loesche GmbH". Cylindrical blocks with a diameter of 100 mm were pressed at 12 MPa. The composition of the blocks varied between pure slag and mixtures of slag and sand. The effects of pressure, temperature, and time on the CO₂ curing process were studied in a 2-liter high-pressure autoclave. Pressures between 0.1 and 5 MPa, temperatures between 25 and 140°C, and curing times between 1 and 100 hours were considered. The quality of the CO₂-cured blocks was determined by measuring the compressive strength by "Ruhrbaustoffwerke GmbH & Co. KG." The degree of carbonation was determined by total inorganic carbon (TIC) and X-ray diffraction (XRD) measurements. The pH trends in the cross-section of the blocks were monitored using phenolphthalein as a liquid pH indicator. The parameter set that yielded the best performing material was tested on all slag types. In addition, the method was scaled to steel slag-based building blocks (240 mm x 115 mm x 60 mm) provided by "Ruhrbaustoffwerke GmbH & Co. KG" and CO₂-cured in a 20-liter high-pressure autoclave. The results show that CO₂ curing of building blocks consisting of pure wetted LD slag leads to severe cracking of the cylindrical specimens. The high CO₂ uptake leads to an expansion of the specimens. However, if LD slag is used only proportionally to replace quicklime completely and sand proportionally, dimensionally stable bricks with high compressive strength are produced. The tests to determine the optimum pressure and temperature show 2 MPa and 50°C as promising parameters for the CO₂ curing process. At these parameters and after 3 h, the compressive strength of LD slag blocks reaches the highest average value of almost 50 N/mm². This is more than double that of conventional sand-lime bricks. Longer CO₂ curing times do not result in higher compressive strengths. XRD and TIC measurements confirmed the formation of carbonates. All tested slag-based bricks show higher compressive strengths compared to conventional sand-lime bricks. However, the type of slag has a significant influence on the compressive strength values. The results of the tests in the 20-liter plant agreed well with the results of the 2-liter tests. With its comparatively moderate operating conditions, the CO₂ curing process has a high potential for saving CO₂ emissions.

Keywords: CO₂ curing, carbonation, CCU, steel slag

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Authors: Jiajun Duan, Yang Li, Jianan Gao, Runzi Cao, Enxiang Shang, Wen Zhang

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Reactive oxygen species (ROS) generation is considered as an important photoaging mechanism of microplastics (MPs) and nanoplastics (NPs). To elucidate the ROS-induced MP/NP aging processes in water under UV365 irradiation, we examined the effects of surface coatings, polymer types, and grain sizes on ROS generation and photoaging intermediates. Bare polystyrene (PS) NPs generated hydroxyl radicals (•OH) and singlet oxygen (¹O₂), while coated PS NPs (carboxyl-modified PS (PS-COOH), amino-modified PS (PS-NH₂)) and PS MPs generated fewer ROS due to coating scavenging or size effects. Polypropylene, polyethylene, polyvinyl chloride, polyethylene terephthalate, and polycarbonate MPs only generated •OH. For aromatic polymers, •OH addition preferentially occurred at benzene rings to form monohydroxy polymers. Excess •OH resulted in H abstraction, C-C scission, and phenyl ring opening to generate aliphatic ketones, esters, aldehydes, and aromatic ketones. For coated PS NPs, •OH preferentially attacked the surface coatings to result in decarboxylation and deamination reactions. For aliphatic polymers, •OH attack resulted in the formation of carbonyl groups from peracid, aldehyde, or ketone via H abstraction and C-C scission. Moreover, ¹O₂ might participate in phenyl ring opening for PS NPs and coating degradation for coated PS NPs. This study facilitates understanding the ROS-induced weathering process of NPs/MPs in water under UV irradiation.

Keywords: microplastics, nanoplastics, photoaging, reactive oxygen species, surface coating

Procedia PDF Downloads 132