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  • 1.
    Abrahamsson, Filip
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Leaching of Pyrrhotite from Nickel Concentrate2017Independent thesis Advanced level (professional degree), 20 credits / 30 HE creditsStudent thesis
    Abstract [en]

    Non-oxidative acid leaching of pyrrhotite from Kevitsa’s Ni-concentrate and methods to recover by-products, have been investigated. Selective dissolution of pyrrhotite (Fe1-xS, 0<x<0.25) can enrich the content of the valuable metals, such as Ni and Co, in the final concentrate and will reduce the amount of Fe and S sent to the smelters. The pyrometallurgical smelting of leached concentrate will thus give less formation of smelter by-products in form of slag and SO2. The leaching was studied through an experimental design plan with parameter settings of  38.8% to 57.8% H2SO4 and temperatures from 60 to 100°C. The best results were obtained in experiments carried out at the lower experimental range. Leaching at 60°C with an initial acid concentration of 38.8% H2SO4 was found sufficient to selectively dissolve most of the pyrrhotite; leaving an enriched solid residue. A QEMSCAN analysis of the solid residue confirmed that most of the pyrrhotite had been dissolved and showed that pentlandite was still the main Ni-mineral. Chemical assays showed that more than 95% of the Ni, Co, and Cu remained in the final residue.

       The utilized leaching process generates by-products, in the form of large quantities of Fe2+ in solution and gaseous H2S. To recover Fe2+, crystallization of iron(ii) sulfate (FeSO4∙nH2O) from leach solution through cooling have been studied. The crystallized crystals were further dehydrated into the monohydrate (FeSO4∙H2O) through a strong sulfuric acid treatment (80%H2SO4). XRD analysis confirmed that FeSO4∙H2O was the main phase in the final crystals, and a chemical analysis showed a Fe content of about 30%, 1.5% Mg, 0.4% Ca, and 0.2% Ni.

       The possibility to leach the concentrate by circulating the acidic solution from the crystallization stage has been tested. The recirculation of the solution showed no negative effects, as the recoveries of elements and chemical assays of the final solid residue were found to be similar to the obtained assay when the concentrate was leached in a fresh solution.

  • 2.
    Agthe, Michael
    et al.
    Department of Materials and Environmental Chemistry, Arrhenius Laboratory, Stockholm University.
    Wetterskog, Erik
    Department of Materials and Environmental Chemistry, Arrhenius Laboratory, Stockholm University.
    Mouzon, Johanne
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Salazar-Alvarez, German
    Department of Materials and Environmental Chemistry, Arrhenius Laboratory, Stockholm University.
    Bergström, Lennart Magnus
    Department of Materials and Environmental Chemistry, Arrhenius Laboratory, Stockholm University.
    Dynamic growth modes of ordered arrays and mesocrystals during drop-casting of iron oxide nanocubes2014In: CrystEngComm, ISSN 1466-8033, E-ISSN 1466-8033, Vol. 16, no 8, p. 1443-1450Article in journal (Refereed)
    Abstract [en]

    The growth modes of self-assembled mesocrystals and ordered arrays from dispersions of iron oxide nanocubes with a mean edge length of 9.6 nm during controlled solvent removal have been investigated with a combination of visible light video microscopy, atomic force microscopy and scanning electron microscopy. Mesocrystals with translational and orientational order of sizes up to 10 μm are formed spontaneously during the final, diffusion-controlled, drop-casting stage when the liquid film is very thin and the particle concentration is high. Convection-driven deposition of ordered nanocube arrays at the edge of the drying droplet is a manifestation of the so called coffee-ring effect. Dendritic growth or fingering of rapidly growing arrays of ordered nanocubes could also be observed in a transition regime as the growth front moves from the initial three-phase contact line towards the centre of the original droplet.

  • 3.
    Aguilar, Wilson
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Study of the Synthesis of ZSM-5 from Inexpensive Raw Materials2014Licentiate thesis, comprehensive summary (Other academic)
    Abstract [en]

    ZSM-5 is an aluminosilicate with high silica ratio with suitable properties for catalysis, ion exchange, adsorption and membrane applications. ZSM-5 is usually produced industrially from concentrated systems in which there is formation of an amorphous gel phase. Typical syntheses of ZSM-5 require sources of silicon and aluminium, a mineralizer and an organic molecule as so-called templating agent. The silicon and aluminum sources widely used for the synthesis are pure reagent chemicals and in particular quaternary ammonium compounds like tetrapropyl ammonium hydroxides (TPA-OH), are employed as templating agents. Unfortunately, these compounds are rather expensive. Demand for inexpensive sources of aluminosilicates for the synthesis of ZSM-5 has increased during the last two decades. Natural raw materials such as kaolin clay and diatomaceous earth (diatomite) are two potential inexpensive sources of silica and alumina. Moreover, the molecule n-butylamine (NBA) has been reported as a low-cost templating agent to replace the quaternary ammonium compounds. The aim of this work was to show for the first time that leached metakaolinite or diatomite in combination with sodium hydroxide and n-butylamine could be used as inexpensive raw materials for the synthesis of ZSM-5 without using an additional source of silica. After synthesis optimization, both sources of aluminosilicate were found to behave differently during the course of synthesis and led to slightly different products. The chemical composition of the raw materials and the products were determined using inductively coupled plasma-sector field mass spectrometry (ICP-SFMS). Crystallinity was examined by X-ray diffractometry (XRD), the morphology was studied by extreme-high-resolution scanning electron microscopy (XHR-SEM) and the specific surface area was estimated from nitrogen adsorption data by the BET method. The chemical composition of individual crystals was determined by energy dispersive spectrometry (EDS). Dealumination of the raw materials by acid leaching made it possible to reach appropriate SiO2/Al2O3 ratios and reduced the amount of impurities. The final ZSM-5 products had a SiO2/Al2O3 ratio in the range 20 – 40. The use of leached diatomite allowed reaching higher yield of ZSM-5 crystals within comparable synthesis times. However, low amounts of mordenite were formed, which was related to the high calcium content of diatomite. Another considerable advantage of diatomite over kaolin is that diatomite does not require heat treatment at high temperature to convert the kaolin to reactive metakaolin. Further characterization of the system by XHR-SEM and EDS at low voltage was carried out in order to understand the nucleation and early growth of the ZSM-5 zeolite crystals. The observations with unprecedented detail strongly suggest that nucleation and the succeeding growth occurs on the gel surface. The growth rates in the various crystallographic directions already at an early stage are such that the shape of the growing crystals resembles that of the final crystals. However, as the early growth is interface mediated, the growth rate along the gel particles is high and the gel particles will become partially embedded inside the growing crystals at an early stage. The Si and Al nutrients are probably transported along the solid/liquid interface and possibly through the liquid in the form of nanoparticles detaching from the gel. The organic template was initially contained in the liquid. However, it remains unclear at which stage the template becomes incorporated in the solid material. EDS at low voltage was also used to gain compositional information about the sodium/calcium ion exchanged products and extraneous phases when kaolin and Bolivian montmorillonite clay were used for the synthesis of zeolite A by alkali fusion. In order to evaluate the cation exchange capacity (CEC) of the synthesized zeolite, ICP-SFMS and EDS were compared. The EDS method used in this work resulted in (Na,Ca)/Al ratios in equivalent moles very close to 1.0 as expected and was therefore found more reliable than ICP-SFMS to measure cation exchange capacity for zeolite A. To summarize, the present work shows that it was possible to synthesize well-crystallized ZSM-5 zeolite from inexpensive raw materials such as leached metakaolin or leached diatomite, sodium hydroxide and n-butyl amine. Furthermore, the crystallization mechanism evidenced in this system might be more general and also apply for other concentrated systems, e.g. those using TPA as structure-directing. Finally, this work displays that EDS at low voltage can provide valuable local compositional information in the field of zeolite synthesis.

  • 4.
    Aguilar, Wilson
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering. Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Cardenas, Edgar
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering. Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Mouzon, Johanne
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering. Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Dendritic growth of NBA-ZSM-5In: Microporous and Mesoporous Materials, ISSN 1387-1811, E-ISSN 1873-3093Article in journal (Other academic)
    Abstract [en]

    Crystallization of ZSM-5 zeolite from a gel using n-butylamine as structure-directing agent was studied. Extreme high-resolution transmission and scanning electron microscopy showed the presence of dendritic features that are present at the crystal surface during most of the reaction time that become smoother towards completion of the crystallization. In addition, a web that likely stems from the gel, comprised of alumina-rich nanoparticles between the dendrites at the surface of the crystals was also identified. When the gel is not in direct contact with the crystal surface, dendrites and the web are not observed, and the crystals grow faster. Thus, the alumina-rich web retards the crystal growth and cause the formation of dendritic features.

  • 5.
    Aguilar, Wilson
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Garcia, Gustavo
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Mouzon, Johanne
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Comparison between leached metakaolin and leached diatomaceous earth as raw materials for the synthesis of ZSM-52014In: SpringerPlus, E-ISSN 2193-1801, Vol. 3, no 1Article in journal (Refereed)
    Abstract [en]

    Inexpensive raw materials have been used to prepare ZSM-5 zeolites with SiO2/Al2O3 molar ratios in the range 20 - 40. Kaolin or Bolivian diatomaceous earth was used as aluminosilicate raw materials and sodium hydroxide and n-butylamine were used as mineralizing agents and template. Dealumination of the raw materials by acid leaching made it possible to reach appropriate SiO2/Al2O3 ratios and to reduce the amount of iron and other impurities. After mixing the components and aging, hydrothermal treatment was carried out and the products were recovered The results clearly show for the first time that well-crystallized ZSM-5 can be directly prepared from leached metakaolin or leached diatomaceous earth using sodium hydroxide and n-butylamine as mineralizing agents and template under appropriate synthesis conditions. A longer induction time prior to crystallization was observed for reaction mixtures prepared from leached diatomaceous earth, probably due to slower digestion of the fossilized diatom skeletons as compared with that for microporous leached metakaolin. The use of leached diatomaceous earth allowed higher yield of ZSM-5 crystals within comparable synthesis times. However, low amounts of Mordenite formed, which was related to the high calcium content of diatomaceous earth. Another considerable advantage of diatomaceous earth over kaolin is that diatomaceous earth does not require heat treatment at high temperature for metakaolinization.

  • 6.
    Aguilar-Mamani, Wilson
    et al.
    Department of Chemistry, Faculty of Science and Technology, San Simon University, UMSS, Cochabamba.
    Akhtar, Farid
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Material Science.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Mouzon, Johanne
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Solution-mediated growth of NBA-ZSM-5 crystals retarded by gel entrapment2018In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 487, p. 57-64Article in journal (Refereed)
    Abstract [en]

    The synthesis of flat tablet-shaped ZSM-5 crystals from a gel using metakaolin as aluminosilicate source and n-butyl amine as structure directing agent was investigated. The evolution inside the solid phase was characterized by X-ray diffraction, scanning electron microscopy, energy dispersive spectroscopy, thermogravimetry and mass spectrometry. A kinetic study indicated that the nucleation of the majority crystals occurred concurrently with the formation of the gel upon heating the starting liquid suspension. Microstructural evidences undeniably showed that the gel precipitated on ZSM-5 crystals and mineral impurities originating from kaolin. As a result, crystal growth was retarded by gel entrapment, as indicated by the configuration and morphology of the embedded crystals. The results presented herein are harmonized with a solution-mediated nucleation and growth mechanism. Our observations differ from the autocatalytic model that suggests that the nuclei rest inside the gel until released when the gel is consumed. Our results show instead that it is crystals that formed in an early stage before entrapment inside the gel that rest inside the gel until exposed at the gel surface. These results illustrate the limitation of the classical method used in the field to determine nucleation profiles when the crystals become trapped inside the gel.

  • 7.
    Aguilar-Mamani, Wilson
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering. Department of Chemistry, Faculty of Science and Technology, San Simon University, Cochabamba, Bolivia.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Mouzon, Johanne
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Internal structure of a gel leading to NBA-ZSM-5 single crystals2018In: Journal of porous materials, ISSN 1380-2224, E-ISSN 1573-4854, Vol. 25, no 6, p. 1551-1559Article in journal (Refereed)
    Abstract [en]

    Porous gel structures are formed during the synthesis of the zeolite ZSM-5 due to the reaction between a source of aluminosilicate, sodium hydroxide, water and a structure directing agent, such as e.g. tetrapropylammonium (TPA) or n-butylamine (NBA). In the present work, the formation of the gel in a heterogeneous system leading to the crystallization of NBA-ZSM-5 zeolite from leached metakaolin was studied extensively. The solid and liquid phases obtained after separation were analyzed by inductively coupled plasma sector field mass spectrometry, dynamic light scattering, extreme high resolution-scanning electron microscopy, energy dispersive spectroscopy, high resolution-transmission electron microscopy, X-ray diffraction and nitrogen gas adsorption. The main gel phase formed after hydrothermal treatment exhibited a sponge-like structure resembling those forming in (Na, TPA)-ZSM-5-based systems. For the first time, the walls of the main gel were shown to be inhomogenous and to possess a biphasic internal structure consisting of a mesoporous skeleton of aluminosilicate nanoparticles embedded in a silicate-rich soluble matrix of soft matter. The data presented in this paper is of primary importance to understand the mechanism by which the gel is consumed and contributes to the growth process of the zeolite crystals.

  • 8.
    Aiello, R.
    et al.
    University of Calabria.
    Artioli, G.
    University of Milan.
    Carotenuto, L.
    MARS Center, Naples.
    Colella, C.
    University of Naples.
    Norby, P.
    University of Oslo.
    Sterte, Johan
    Zeolite synthesis in microgravity2005In: Topical teams in life & physical sciences: towards new research applications, Noordwijk, Netherlands: ESTEC , 2005, p. 78-85Chapter in book (Other academic)
    Abstract [en]

    The results of activities performed by the members of the Topical Team on 'Zeolites synthesis in microgravity' are discussed. A method was developed using a two-temperature synthesis procedure to distinguish between the nucleation and growth phase of the crystallization. The experiments have investigated the possibility of suppressing secondary nucleation by imposing a temperature gradient. Optical thickness of the solution has been monitored by interferometry. The Team, on the basis of findings, has elaborated a research program on zeolite film deposition that includes microgravity experimentation.

  • 9.
    Akhtar, Farid
    et al.
    Department of Materials and Environmental Chemistry, Stockholm University.
    Ojuva, Arto
    Stockholm University, Department of Materials and Environmental Chemistry.
    Mouzon, Johanne
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Bergström, Lennart M.
    Department of Materials and Environmental Chemistry, Stockholm University.
    All-Zeolite Membranes2010Conference paper (Refereed)
  • 10.
    Akhtar, Farid
    et al.
    Stockholm University, Department of Materials and Environmental Chemistry.
    Ojuva, Arto
    Stockholm University, Department of Materials and Environmental Chemistry.
    Wirawan, Kompiang
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Bergström, Lennart
    Stockholm University, Department of Materials and Environmental Chemistry.
    Hierarchically porous binder-free silicalite-1 discs: a novel support for all-zeolite membranes2011In: Journal of Materials Chemistry, ISSN 0959-9428, E-ISSN 1364-5501, Vol. 21, no 24, p. 8822-8828Article in journal (Refereed)
    Abstract [en]

    Thermal expansion mismatch between the zeolite film and the support is an important cause for the formation of defects and cracks during the fabrication and use of zeolite membranes. We have studied how silicalite-1 discs with a permeability comparable to commercially available alumina supports can be produced by pulsed current processing (PCP) as a novel substrate for all-zeolite membranes. Hierarchically porous and mechanically strong membrane supports where the surface area and crystallography of the silicalite-1 particles were maintained could be obtained by carefully controlling the thermal treatment during PCP consolidation. In situ X-ray diffraction and dilatometry showed that the coefficient of thermal expansion (CTE) of the silicalite-1 substrate was negative in the temperature range 200-800 degrees C while the commonly used alumina substrate displayed a positive CTE. The critical temperature variation, Delta T, and thicknesses for crack-free supported zeolite films with a negative CTE were estimated using a fracture energy model. Zeolite films with a thickness of 1 mu m can only sustain a relatively modest Delta T of 100 degrees when supported onto alumina substrates while the all-zeolite membranes can support temperature variations above 500 degrees

  • 11.
    Akhtar, Farid
    et al.
    Department of Materials and Environmental Chemistry, Stockholm University.
    Ojuva, Arto
    Stockholm University, Department of Materials and Environmental Chemistry.
    Wirawan, Kompiang
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Bergström, Lennart
    Department of Materials and Environmental Chemistry, Stockholm University.
    PCP procesing of Zeolite supports for all-zeolite membranes2011Conference paper (Refereed)
  • 12.
    Akhtar, Farid
    et al.
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Material Science.
    Sjöberg, Erik
    Korelskiy, Danil
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Rayson, Mark
    Department of Chemistry, The University of Surrey, Guildford.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Bergström, Lennart
    Department of Materials and Environmental Chemistry, Stockholm University.
    Preparation of graded silicalite-1 substrates for all-zeolite membranes with excellent CO2/H2 separation performance2015In: Journal of Membrane Science, ISSN 0376-7388, E-ISSN 1873-3123, Vol. 493, p. 206-211Article in journal (Refereed)
    Abstract [en]

    raded silicalite-1 substrates with a high gas permeability and low surface roughness have been produced by pulsed current processing of a thin coating of a submicron silicalite-1 powder onto a powder body of coarser silicalite-1 crystals. Thin zeolite films have been hydrothermally grown onto the graded silicalite-1 support and the all-zeolite membranes display an excellent CO2/H2 separation factor of 12 at 0 °C and a CO2 permeance of 21.3×10-7 mol m-2 s-1 Pa-1 for an equimolar CO2/H2 feed at 505 kPa and 101 kPa helium sweep gas. Thermal cracking estimates based on calculated surface energies and measured thermal expansion coefficients suggest that all-zeolite membranes with a minimal thermal expansion mismatch between the graded substrate and the zeolite film should remain crack-free during thermal cycling and the critical calcination step.

  • 13.
    Andersson, Anna
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    CFD optimization of photochemical UV reactors for VOC degradation2017Independent thesis Advanced level (professional degree), 20 credits / 30 HE creditsStudent thesis
    Abstract [en]

    In 2016 the World Health Organization released a report on Ambient Air Pollution, in this it was stated that one out of every nine deaths all around the world in 2012 were due to air-pollution-related conditions. Urban air pollution involves a broad range of compounds from many diverse sources. Volatile Organic Compounds (VOCs) are some of the important compounds. Almost all VOCs are known to have effect on human health, many of them are carcinogenic. VOCs also contribute to the ground level photochemical smog and the reduction of the stratospheric ozone layer. Therefore, it is important to control the emissions of VOCs from industries and restaurants.

    Today most big scale VOC removal is done by thermal or catalytic incineration. While smaller scale air purification is done by using adsorbing materials such as activated carbon. Both these methods have their drawbacks. A promising technology, which is also environmentally friendly, is UV reactors.

    This thesis is a collaboration with the company Centriair, a company developing and selling UV reactors mainly for odor removal. The UV reactors which are in use today show acceptable performance, with a conversion of 50-60%. However, they have yet to be optimized to get the most out of the reactors. The aim was to try to reach an as high conversion of VOCs as possible in a prototype scale compared to a reference reactor, also in prototype scale. The reactors were simulated using the Computational Fluid Dynamic (CFD) software COMSOL Multiphysics® 5.2a. The simulation was based on earlier lab scale experiments with UV reactors.

    The conclusion from doing this thesis is that the most important challenge with a UV reactor up-scaling and optimization is the dark zones and the bypassing effect given by these. It is very important that the irradiation reaches the whole reactor and that all gas is affected by it. It is also important that the gas is given time to stay by the light sources as long as possible. Two reactors in this thesis had very high conversion results and thus showed potential of being very effective UV reactors. These two reactors showed conversion results of 45% respective 61% higher than the reference reactor used by Centriair today.

  • 14.
    Andersson, Charlotte
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering.
    Factors affecting MFI membrane quality2007Doctoral thesis, comprehensive summary (Other academic)
    Abstract [en]

    Zeolites are crystalline aluminosilicates with molecular sieving properties and are widely used in industrial applications such as catalysis, sorption and ion-exchange. Zeolite membranes are highly interesting due to their capability to continuously separate molecules under severe conditions. The MFI zeolite structure has suitable pore diameter for many applications, and its thermal and chemical stability is high. In order to obtain high performance MFI membranes, a thin and defect free film is needed for high flux and high selectivity. In this thesis, parameters affecting quality of zeolite membranes have been investigated. Different MFI-zeolite membranes were prepared using seed crystals and hydrothermal synthesis. Thereafter, membranes were characterized using scanning electron microscopy, single gas permeation measurements, porosimetry and separation experiments. The effect of grain boundaries was investigated by preparing membranes with small crystal size. It was found that a high amount of grain boundaries reduced the quality of the membranes. In another study, the effect of exposure to aqueous solutions was found to increase the amount of non-zeolitic pores in the membrane, and thus it decreased the quality of the membrane. However, no such effect was found for ethanol that was identified as a safe rinsing media. Membranes with different Si/Al ratio were also prepared and evaluated. It was observed that the Si/Al ratio of a MFI membrane influences the performance of the membrane. It was found that an increase of aluminium makes the membrane more polar which leads to an improved adsorption of, and selectivity for polar molecules. The effect of support invasion was also evaluated and the regularity and extension of the support invasion was observed to affect membrane quality. The effect of heating rate during calcination was investigated and no correlation between heating rate and membrane quality was observed. Calcination of membranes was studied in-situ by high temperature synchrotron radiation and a model for crack formation was postulated. In summary, this work has shown that in order to obtain high quality membranes, the amount of grain boundaries, the film thickness and support invasion should be controlled. To obtain the best performance of the membranes the Si/Al ratio should be chosen with respect to the application. Finally, water exposure affects the lifetime of the MFI membranes in certain applications.

  • 15.
    Andersson, Charlotte
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering.
    Properties of molecular sieve membranes2004Licentiate thesis, comprehensive summary (Other academic)
    Abstract [en]

    Zeolites are crystalline aluminosilicates with molecular sieving properties and are widely used in industry for catalysis, sorption and ion-exchange applications. Zeolite membranes are commercially interesting since this technology may be employed for continuous separation of molecules under severe conditions. MFI zeolite has suitable pore diameter for many applications and relatively high thermal and chemical stability. Zeolite films in membranes must be thin, to obtain a high flux and free from defects for high selectivity. Many parameters are affecting the properties of zeolite films and in this thesis some of them are investigated. MFI zeolite membranes were prepared using seed crystals and hydrothermal synthesis and characterized with scanning electron microscopy, single gas permeation measurements, porosimetry and separation experiments. Membranes grown in one or several steps with seeding in-between the synthesis steps were compared. It was observed that membranes comprised of small crystals and consequently high concentration of grain boundaries had low separation performance. Grain boundaries could also be opened by extensive rinsing, which reduced membrane quality. The influence of the calcination rate on the performance of zeolite membranes of a particular type was also studied. It was demonstrated that the calcination rate does not affect the membrane quality.

  • 16. Andersson, Charlotte
    et al.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Effects of exposure to water and ethanol on silicalite-1 membranes2008In: Journal of Membrane Science, ISSN 0376-7388, E-ISSN 1873-3123, Vol. 313, no 1-2, p. 120-126Article in journal (Refereed)
    Abstract [en]

    The effects of long exposures to ethanol, water and 0.1 M aqueous solutions of ammonia, sodium hydroxide, tetrapropylammonium hydroxide (TPAOH) and hydrochloric acid on thin TPA-silicalite-1 membranes were studied. Single gas permeation experiments, porosimetry and scanning electron microscopy were used to characterize the membranes. It was found that a short exposure (24 h) will only dissolve synthesis residues and will not affect membrane quality negatively. The only medium that had an effect after 24 h was sodium hydroxide, which almost dissolved the film completely. After exposing TPA-silicalite-1 membranes for 30 days in the various liquids, the membrane quality decreased in the order ethanol < 0.1 M hydrochloric acid < 0.1 M TPAOH < water < 0.1 M ammonia < 0.1 M sodium hydroxide due to dissolution of the silicalite-1 crystals. This study has shown that prolonged exposure to aqueous solutions will lead to dissolution of silicalite-1 crystals causing an increase in micro- and mesopores in the film. The amount and size of the pores will depend on the pH of the aqueous medium. Higher pH gives a higher dissolution and hence more non-zeolitic pores in the silicalite-1 film. Ethanol has no effect on the dissolution of the zeolite film even after 30 days. This finding has an effect in membrane preparation and in several membrane applications such as pervaporation and separation of hydrocarbons isomer mixtures.

  • 17. Andersson, Charlotte
    et al.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Jareman, Fredrik
    Luleå tekniska universitet.
    Sterte, Johan
    Silicalite-1 membranes with small crystal size2004In: Recent advances in the science and technology of zeolites and related materials. Part A: proceedings of the 14th International Zeolite Conference, Amsterdam: Elsevier, 2004, p. 626-631Conference paper (Refereed)
    Abstract [en]

    Silicalite-1 membranes with small crystal size were prepared using a multiseeding method, where the support was repeatedly seeded and exposed to a short hydrothermal treatment up to five times. The film were characterized using SEM, single gas permeation, porosimetry and mixture separation experiment Films with three or four layers were of high quality i.e with minor defects according to the porosimetry experiments but showed poor separation of binary mixtures. This result may be attributed to the small crystal size and/or large amount of grain boundaries in the films.

  • 18.
    Andersson, Joel
    et al.
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Machine Elements.
    Larsson, Roland
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Machine Elements.
    Almqvist, Andreas
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Machine Elements.
    Grahn, Mattias
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Minami, Ichiro
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Machine Elements.
    Semi-deterministic chemo-mechanical model of boundary lubrication2012In: Faraday discussions (Online), ISSN 1359-6640, E-ISSN 1364-5498, Vol. 156, p. 343-360Article in journal (Refereed)
    Abstract [en]

    A model for tribofilm growth is developed. The model is used in combination with numerical contact mechanics tools to enable evaluation of the combined effects of chemistry and contact mechanics. The model is tuned with experimental data and is thereafter applied to rough surfaces. The growth of the tribofilm is evaluated for 3 different contact cases and short-term tribofilm growth behaviour is analyzed. The results show how tribofilms grow in patches. The model is expected to be used as a tool for analysis of the interaction between rough surfaces.

  • 19.
    Andersson, Sofia
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Influence of metal ions on lignin-based carbon fiber quality2017Independent thesis Advanced level (professional degree), 20 credits / 30 HE creditsStudent thesis
    Abstract [en]

    Carbon fiber is a lightweight, versatile material with many current and potential applications. To be able to expand the market for carbon fiber composites in other areas than special applications the production costs must be reduced. One way of accomplishing this could be to use a less expensive raw material where lignin is a good example as it can be provided at lower cost, is renewable and abundantly available compared to commercially used raw materials today.

    So far, the mechanical properties of lignin-based carbon fibers are inferior relative to commercial carbon fibers. For lignin-based carbon fibers to enter the commercial market more research is necessary to gain knowledge of the conversion of lignin to carbon fiber. The LightFibre project investigates the possibilities to produce carbon fibers based on a mixture of softwood kraft lignin and cellulose. The kraft lignin is isolated from black liquor in the kraft/sulfate process with the LignoBoost process. This master thesis project was conducted within in the LightFibre project and evaluated whether metal ions generally present in kraft lignin had an influence on the final carbon fiber quality in terms of mechanical properties and morphology. The mechanical properties were determined with tensile testing, the morphology by scanning electron microscopy (SEM) and the relative abundance of studied elements with electron dispersive spectroscopy (EDS).

    The influence of the chosen metal ions was tested by impregnation of dry-jet wet spun prefibers based on 70 wt.% softwood kraft lignin and 30 wt.% dissolving pulp cellulose. The fibers were impregnated in room temperature with solutions containing Na2SO4, K2SO4, MgSO4, FeSO4 and Al2(SO4)3 salts where the cations were the focus in these trials. The concentrations used for impregnation were 0.2 and 1M of the cations.

    The obtained mechanical properties of the carbon fibers of the samples impregnated with different metal ions did not deviate significantly from the reference which had a tensile strength of 870 MPa and tensile modulus of 68 GPa. The analysis of morphology with SEM showed no defects or damage of any of the fibers. Therefore, it was concluded that the impregnated metal ions: K+, Na+, Al3+, Mg2+ and Fe2+ at the obtained levels in the fibers cause no effects on the fibers during the stabilization and carbonization that affects the mechanical performance of final carbon fiber.  The amount of potassium in one of the samples was estimated to 0.1 wt.%.

    From the results of this study it may be suggested that the general recommendation of <0.1 wt.% ash in lignin can be exceeded, for dry-jet wet-spun kraft lignin/cellulose-based carbon fibers.

  • 20. Anthonis, Marc Henry
    et al.
    Bons, Anton-Jan
    Deckman, H. W.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Lai, Wenyih F.
    Peters, J.A.J.
    Crystalline molecular sieve layers and processes for their manufacturePatent (Other (popular science, discussion, etc.))
    Abstract [en]

    A process is described for the manufacture of crystalline molecular sieve layers with good para-xylene over meta-xylene selectivity's good para-xylene permeances and selectivities. The process requires impregnation of the support prior to hydrothermal synthesis using the seeded method and may be undertaken with pre-impregnation masking. The crystalline molecular sieve layer has a selectivity (.alpha..sub.x) for para-xylene over meta-xylene of 2 or greater and a permeance (Q.sub.x) for para-xylene of 3.27.times.10.sup.-8 mole(px)/m.sup.2.s.Pa(px) or greater measured at a temperature of .gtoreq.250.degree. C. and an aromatic hydrocarbon partial pressure of .gtoreq.10.times.10.sup.3 Pa.

  • 21.
    Antonopoulou, Io
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Development of biocatalytic processes for selective antioxidant production2018Doctoral thesis, comprehensive summary (Other academic)
    Abstract [en]

    Feruloyl esterases (FAEs, EC 3.1.1.73) represent a subclass of carboxylic acid esterases that under normal conditions catalyze the hydrolysis of the ester bond between hydroxycinnamic acids (ferulic acid, sinapic acid, caffeic acid, p-coumaric acid) and sugar residues in plant cell walls. Based on their specificity towards monoferulates and diferulates, substitutions on the phenolic ring and on their amino acid sequence identity, they have been classified into four types (A-D) while phylogenetic analysis has resulted in classification into thirteen subfamilies (SF1-13). Under low water content, these enzymes are able to catalyze the esterification of hydroxycinnamic acids or the transesterification of their esters (donor) with alcohols or sugars (acceptor) resulting in compounds with modified lipophilicity, having a great potential for use in the tailor-made modification of natural antioxidants for cosmetic, cosmeceutical and pharmaceutical industries. The work described in this thesis focused on the selection,characterization and application of FAEs for the synthesis of bioactive esters with antioxidant activity in non-conventional media. The basis of the current classification systems was investigated in relation with the enzymes’ synthetic and hydrolytic abilities while the developed processes were evaluated for their efficiency and sustainability.

    Paper I was dedicated to the screening and evaluation of the synthetic abilities of 28 fungal FAEs using acceptors of different lipophilicity at fixed conditions in detergentless microemulsions. It was revealed that FAEs classified in phylogenetic subfamilies related to acetyl xylan esterases (SF5 and 6) showed increased transesterification rates and selectivity. In general, FAEs showed preference on more hydrophilic alcohol acceptors and in descending order to glycerol > 1-butanol > prenol. Homology modeling and small molecule docking simulations were employed as tools for the identification of a potential relationship between the predicted surface and active site properties of selected FAEs and the transesterification selectivity.

    Papers II- IV focused on the characterization of eight promising FAEs and the optimization of reaction conditions for the synthesis of two bioactive esters (prenyl ferulate and L-arabinose ferulate) in detergentless microemulsions. The effect of the medium composition, the donor and acceptor concentration, the enzyme load, the pH, the temperature and the agitation on the transesterification yield and selectivity were investigated. It was observed that the acceptor concentration and enzyme load were crucial parameters for selectivity. Fae125 (Type A, SF5) iiexhibited highest prenyl ferulate yield (81.1%) and selectivity (4.685) converting 98.5% of VFA to products after optimization at 60 mM VFA, 1.5 M prenol, 0.04 mg FAE mL-1, 40oC, 24 h, 53.4:43.4:3.2 v/v/v n-hexane: t-butanol: 100 mM MOPS-NaOH pH 8.0. On the other hand, FaeA1 (Type A, SF5) showed highest L-arabinose ferulate yield (52.2 %) and selectivity (1.120) at 80 mM VFA, 55 mM L-arabinose, 0.02 mg FAE mL-1, 50oC, 8 h, 19.8: 74.7: 5.5 v/v/v n-hexane: t-butanol: 100 mM MOPS-NaOH pH 8.0.

    In paper V, the effect of reaction media on the enzyme stability and transesterification yield and selectivity was studied in different solvents for the synthesis of two bioactive esters: prenyl ferulate and L-arabinose ferulate. The best performing enzyme (Fae125) was used in the optimization of reaction conditions in the best solvent (n-hexane) via response surface methodology. Both bioconversions were best described by a two-factor interaction model while optimal conditions were determined as the ones resulting in highest yield and selectivity.Highest prenyl ferulate yield (87.5%) and selectivity (7.616) were observed at 18.56 mM prenol mM-1VFA, 0.04 mg FAE mL-1, 24.5 oC, 24.5 h, 91.8: 8.2 v/v n-hexane: 100 mM sodium acetate pH 4.7. Highest L-arabinose ferulate yield (56.2%) and selectivity (1.284) were observed at 2.96 mM L-arabinose mM-1VFA, 0.02 mg FAE mL-1, 38.9 oC, 12 h, 90.5: 5.0: 4.5 v/v/v n-hexane: dimethyl sulfoxide: 100 mM sodium acetate pH 4.7. The enzyme could be reused for six consecutive reaction cycles maintaining 66.6% of its initial synthetic activity. The developed bioconversions showed exceptional biocatalyst productivities (> 300 g product g-1FAE) and the waste production was within the range of pharmaceutical processes.

    Paper VI focused on the investigation of the basis of the type A classification of a well-studied FAE from Aspergillus niger(AnFaeA) by comparing its activity towards methyl and arabinose hydroxycinnamic acid esters. For this purpose, L-arabinose ferulateand caffeate were synthesized enzymatically. kcat/Kmratios revealed that AnFaeA hydrolyzed arabinose ferulate 1600 times and arabinose caffeate 6.5 times more efficiently than methyl esters. This study demonstrated that short alkyl chain hydroxycinnamate esters which are used nowadays for FAE classification can lead to activity misclassification, while L-arabinose esters could potentially substitute synthetic esters in classification describing more adequately the enzyme specificitiesin the natural environment.

  • 22.
    Antonopoulou, Io
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Use of feruloyl esterases for chemoenzymatic synthesis of bioactive compounds2017Licentiate thesis, comprehensive summary (Other academic)
    Abstract [en]

    Feruloyl esterases (FAEs, EC 3.1.1.73) represent a subclass of carboxylic acid esterases that under normal conditions catalyze the hydrolysis of the ester bond between hydroxycinnamic acids (ferulic acid, sinapic acid, caffeic acid, p-coumaric acid) and arabinose residues in plant cell walls. Based on their specificity towards monoferulates and diferulates, substitutions on the phenolic ring and on their amino acid sequence identity, they have been classified into four types (A-D). The use of FAEs as accessory enzymes for the degradation of lignocellulosic biomass and their synergism with other hemicellulases has been studied for application in many industries, such as the food, the biofuel and the paper pulp industry. In the recent years, the use of FAEs as biosynthetic tools has been underlined. Under low water content, these enzymes are able to catalyze the esterification of hydroxycinnamic acids or the transesterification of their esters resulting in compounds with altered lipophilicity, revealing a great potential for tailor-made modification of natural antioxidants for use in cosmetic, cosmeceutical and pharmaceutical industries.

    The first part of the thesis is focused on the optimization of reaction conditions for the synthesis of two bioactive esters: prenyl ferulate and L-arabinose ferulate using 5 FAEs (FaeA1, FaeA2, FaeB1, FaeB2 and MtFae1a) from Myceliophthora thermophila in detergentless microemulsions. Reaction conditions were optimized investigating parameters such as the medium composition, the substrate concentration, the enzyme load, the pH, the temperature and the agitation. Regarding the synthesis of prenyl ferulate, FaeB2 offered the highest transesterification yield (71.5±0.2%) after 24 h of incubation at 30oC using 60 mM vinyl ferulate (VFA), 1 M prenol and 0.02 mg FAE/mL in a mixture comprising of 53.4: 43.4: 3.2 v/v/v n-hexane: t-butanol: 100 mM MOPS-NaOH pH 6.0. At these conditions, the competitive hydrolysis was 4-7 fold minimized. Regarding the synthesis of L-arabinose ferulate, FaeA1 offered highest transesterification yield (35.9±2.96%) after 8 h of incubation at 50oC using 80 mM VFA, 55 mM L-arabinose and 0.02 mg FAE/mL in a mixture of 19.8: 74.7: 5.5 v/v/v n-hexane: t-butanol: 100 mM MOPS-NaOH pH 8.0. It was revealed that the type B FAEs from M. thermophila show higher preference to more lipophilic acceptors like prenol, while the type A FaeA1 was more efficient in the synthesis of the more hydrophilic L-arabinose ferulate.

    The second part of the thesis is focused on the investigation of the basis of the type A classification of a well-studied FAE from Aspergillus niger (AnFaeA) by comparing its activity towards methyl and arabinose hydroxycinnamate esters. For this purpose, L-arabinose ferulate and caffeate were synthesized enzymatically. kcat/Km ratios revealed that AnFaeA hydrolyzed arabinose ferulate 1600 times and arabinose caffeate 6.5 times more efficiently than methyl esters. This study demonstrated that short alkyl chain hydroxycinnamate esters which are used nowadays for FAE classification can lead to activity misclassification, while L-arabinose esters could potentially substitute synthetic esters in classification.

  • 23.
    Antonopoulou, Io
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Dilokpimol, Adiphol
    Fungal Physiology, Westerdijk Fungal Biodiversity Institute & Fungal Molecular Physiology, Utrecht University.
    Iancu, Laura
    Dupont Industrial Biosciences.
    Mäkelä, Miia R.
    Department of Microbiology, University of Helsink.
    Varriale, Simona
    Department of Chemical Sciences, University of Naples “Federico II”.
    Cerullo, Gabriella
    Department of Chemical Sciences, University of Naples “Federico II”.
    Hüttner, Silvia
    Department of Biology and Biological Engineering, Division of Industrial Biotechnology, Chalmers University of Technology.
    Uthoff, Stefan
    Institut für Molekulare Mikrobiologie und Biotechnologie, Westfälische Wilhelms-Universität Münster.
    Jütten, Peter
    Taros Chemicals GmbH & Co KG.
    Piechot, Alexander
    Taros Chemicals GmbH & Co KG.
    Steinbüchel, Alexander
    nstitut für Molekulare Mikrobiologie und Biotechnologie, Westfälische Wilhelms-Universität Münster.
    Olsson, Lisbeth
    Department of Biology and Biological Engineering, Division of Industrial Biotechnology, Chalmers University of Technology.
    Faraco, Vincenza
    Department of Chemical Sciences, University of Naples “Federico II”.
    Hildén, Kristiina
    Department of Microbiology, University of Helsinki.
    de Vries, Ronald
    Fungal Physiology, Westerdijk Fungal Biodiversity Institute & Fungal Molecular Physiology, Utrecht University.
    Rova, Ulrika
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Christakopoulos, Paul
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    The Synthetic Potential of Fungal Feruloyl Esterases: A Correlation with Current Classification Systems and Predicted Structural Properties2018In: Catalysts, ISSN 2073-4344, Vol. 8, no 6, article id 242Article in journal (Refereed)
    Abstract [en]

    Twenty-eight fungal feruloyl esterases (FAEs) were evaluated for their synthetic abilities in a ternary system of n-hexane: t-butanol: 100 mM MOPS-NaOH pH 6.0 forming detergentless microemulsions. Five main derivatives were synthesized, namely prenyl ferulate, prenyl caffeate, butyl ferulate, glyceryl ferulate, and l-arabinose ferulate, offering, in general, higher yields when more hydrophilic alcohol substitutions were used. Acetyl xylan esterase-related FAEs belonging to phylogenetic subfamilies (SF) 5 and 6 showed increased synthetic yields among tested enzymes. In particular, it was shown that FAEs belonging to SF6 generally transesterified aliphatic alcohols more efficiently while SF5 members preferred bulkier l-arabinose. Predicted surface properties and structural characteristics were correlated with the synthetic potential of selected tannase-related, acetyl-xylan-related, and lipase-related FAEs (SF1-2, -6, -7 members) based on homology modeling and small molecular docking simulations.

  • 24.
    Antonopoulou, Io
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Hunt, Cameron
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Cerullo, Gabriella
    Department of Chemical Sciences, University of Naples "Federico II".
    Varriale, Simona
    Department of Chemical Sciences, University of Naples “Federico II”.
    Gerogianni, Alexandra
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Faraco, Vincenza
    Department of Chemical Sciences, University of Naples "Federico II".
    Rova, Ulrika
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Christakopoulos, Paul
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Tailoring the specificity of the type C feruloyl esterase FoFaeC from Fusarium oxysporum towards methyl sinapate by rational redesign based on small molecule docking simulations2018In: PLoS ONE, ISSN 1932-6203, E-ISSN 1932-6203, Vol. 13, no 5, article id e0198127Article in journal (Refereed)
    Abstract [en]

    The type C feruloyl esterase FoFaeC from Fusarium oxysporum is a newly discovered enzyme with high potential for use in the hydrolysis of lignocellulosic biomass but it shows low activity towards sinapates. In this work, small molecule docking simulations were employed in order to identify important residues for the binding of the four model methyl esters of hydroxycinnamic acids, methyl ferulate/caffeate/sinapate/p-coumarate, to the predicted structure of FoFaeC. Subsequently rational redesign was applied to the enzyme’ active site in order to improve its specificity towards methyl sinapate. A double mutation (F230H/T202V) was considered to provide hydrophobic environment for stabilization of the methoxy substitution on sinapate and a larger binding pocket. Five mutant clones and the wild type were produced in Pichia pastoris and biochemically characterized. All clones showed improved activity, substrate affinity, catalytic efficiency and turnover rate compared to the wild type against methyl sinapate, with clone P13 showing a 5-fold improvement in catalytic efficiency. Although the affinity of all mutant clones was improved against the four model substrates, the catalytic efficiency and turnover rate decreased for the substrates containing a hydroxyl substitution.

  • 25.
    Antonopoulou, Io
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Spanopoulos, Athanasios
    Biotechnology Laboratory, School of Chemical Engineering, National Technical University of Athens, 5 Iroon Polytechniou Str, Zografou Campus, Athens, Greece.
    Matsakas, Leonidas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Single cell oil and ethanol production by the oleaginous yeast Trichosporon fermentans utilizing dried sweet sorghum stalks2020In: Renewable energy, ISSN 0960-1481, E-ISSN 1879-0682, Vol. 146, p. 1609-1617Article in journal (Refereed)
    Abstract [en]

    The ability of the oleaginous yeast Trichosporon fermentans to efficiently produce lipids when cultivated in dried sweet sorghum was evaluated. First, lipid production was evaluated in synthetic media mimicking the composition of sweet sorghum stalks and optimized based on the nitrogen source and C: N ratio. Under optimum conditions, the lipid production reached 3.66 g/L with 21.91% w/w lipid content by using a mixture of sucrose, glucose and fructose and peptone at C: N ratio 160. Cultivation on pre-saccharified sweet sorghum stalks offered 1.97 g/L, while it was found that sweet sorghum stalks can support yeast growth and lipid production without the need for external nitrogen source addition. At an attempt to increase the carbon source concentration for optimizing lipid production, the Crabtree effect was observed in T. fermentans. To this end, the yeast was evaluated for its potential to produce ethanol under anaerobic conditions in synthetic media and sweet sorghum. The ethanol concentration at 100 g/L glucose was 40.31 g/L, while utilizing sweet sorghum by adding a distinct saccharification step and external nitrogen source offered ethanol concentration equal to 23.5 g/L. To the authors’ knowledge, this is the first time that the Crabtree effect is observed in T. fermentans.

  • 26.
    Antzutkin, Oleg
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Kota, Hanumantha Rao
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Ikumapayi, Fatai
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Holmgren, Allan
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Gunneriusson, Lars
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Johansson, Björn
    New Boliden AB.
    Berggren, Andreas
    New Boliden AB.
    Larsson, Anna-Carin
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Öberg, Sven
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Mathematical Science.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Mouzon, Johanne
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Bhuiyan, Iftekhar Uddin
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Forsmo, Seija
    LKAB.
    Interactions in multi-component mineral systems2011Conference paper (Other academic)
  • 27.
    Antzutkin, Oleg
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Kota, Hanumantha Rao
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Ikumapayi, Fatai
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Johansson, Björn
    New Boliden AB.
    Berggren, Andreas
    New Boliden AB.
    Larsson, Anna-Carin
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Holmgren, Allan
    Öberg, Sven
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Mathematical Science.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Mouzon, Johanne
    Bhuiyan, Iftekhar Uddin
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Forsmo, Seija
    LKAB.
    Interactions in multi-component mineral systems2010Conference paper (Other academic)
  • 28.
    Arkhipov, Victor P.
    et al.
    Kazan National Research Technological University.
    Idiyatullin, Zhamil Sh
    Kazan National Research Technological University.
    Potapova, Elisaveta
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Antzutkin, Oleg
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Filippov, Andrei
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Micelles and aggregates of oxyethylated isononylphenols and their extraction properties near cloud point2014In: Journal of Physical Chemistry B, ISSN 1520-6106, E-ISSN 1520-5207, Vol. 118, no 20, p. 5480-5487Article in journal (Refereed)
    Abstract [en]

    We used nuclear magnetic resonance (NMR) spectroscopy and dynamic light scattering (DLS) techniques to study the structural and dynamic properties of micellar solutions of nonionic surfactants of a homologous series of oxyethylated isononylphenols - C9H19C6H 4O(C2H4O)nH, where n = 6, 8, 9, 10, or 12 - in a wide range of temperatures, including cloud points. The radii of the micelles and aggregates, as well as their compositions at different concentrations of surfactant, were determined. Using aqueous phenol solutions as a model, we studied the process of cloud point extraction with oxyethylated isononylphenols

  • 29.
    Arkhipov, Victor
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Potapova, Elisaveta
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Antzutkin, Oleg
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Filippov, Andrei
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Micelle structure and molecular self-diffusion in isononylphenol ethoxylate–water systems2013In: Magnetic Resonance in Chemistry, ISSN 0749-1581, E-ISSN 1097-458X, Vol. 51, no 7, p. 424-430Article in journal (Refereed)
    Abstract [en]

    The structure and dynamic properties of micellar solutions of nonionic surfactants of a series of isononylphenol ethoxylates, C9H19C6H4O(C2H4O)nH (where n = 6,8,9,10, and 12), were studied by NMR diffusometry, dynamic light scattering, and viscosimetry. The sizes of the micelles were determined for different surfactants and at different surfactant concentrations. The numbers of water molecules bound by a micelle and by one oxyethylene group of the surfactant were estimated

  • 30.
    Arman, S.Y.
    et al.
    Department of Mining and Metallurgical Engineering, Amirkabir University of Technology.
    Omidvar, H.
    Department of Mining and Metallurgical Engineering, Amirkabir University of Technology.
    Tabaian, S.H.
    Department of Mining and Metallurgical Engineering, Amirkabir University of Technology.
    Sajjadnejad, M.
    Department of Mining and Metallurgical Engineering, Amirkabir University of Technology.
    Fouladvand, Shahpar
    Department of Mining and Metallurgical Engineering, Amirkabir University of Technology.
    Afshar, Sh.
    Department of Chemistry, Iran University of Science and Technology.
    Evaluation of nanostructured S-doped TiO2 thin films and their photoelectrochemical application as photoanode for corrosion protection of 304 stainless steel2014In: Surface & Coatings Technology, ISSN 0257-8972, E-ISSN 1879-3347Article in journal (Refereed)
    Abstract [en]

    Undoped and S-doped TiO2 thin films were prepared on titanium substrate through a sol–gel method. The photoelectrochemical behavior of S-doped TiO2 thin film (as photoanode) was studied. The effect of Sulfur doping on structural, optical and morphological properties of TiO2 was studied by X-ray diffraction (XRD), X-ray photoelectron spectroscopy (XPS), FT-IR, UV–ViS and FE-SEM. Superiority of the S-doped TiO2 film was shown through taking advantage of linear sweep voltametry measurement, open-circuit potential of 304 stainless steel as well as potetiodynamic polarization technique. Results showed that S-doped TiO2 thin film is an efficient photoanode with long term stability (several hours).

  • 31.
    Axelsson, Fredrik
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Stabilisering av Aluminiumreducerad AOD-slagg.2019Independent thesis Advanced level (professional degree), 20 credits / 30 HE creditsStudent thesis
    Abstract [en]

    Slag has historically been used as a construction material in different applications. All types of slags are not suitable due to insufficient properties. Production of high alloy stainless steels leads to a slag which is rich in lime, which leads to disintegration due to absorption of water. Certain steel qualities at Sandvik is manufactured with a two slagg procedure where a first reduction slag is use that is replaced with a refining slag. This report looks into changes in the slag-composition to improve the properties in regards to volumetric stability after disposal. Especially it investigates volumetric stability of the reduction slag and if it is possible to combinea production of high quality steel with a stable slag. Further investigations during the project has looked at how the slag works today, with sampling close to the AOD converter but also how different slag compositions affects the slag that is disposed of outside the steelplant with todays disposal routine. Slag that disintegrates due to phase changes during cooling has been observed. A slag composition that seems promising from aproduction and stability perspective has been found. It results in a slag that remain stable even after enduring harsch enviroments. A production with less lime addition during the reduction phase can handle about two thirds of the aluminum reduced steel batches. With this small changein the AOD process roughly 6000tonnes/year of slag could be shifted from disintegration to stable material.

  • 32.
    Bayat, Mohammad
    et al.
    Faculty of Chemical Engineering, Research and Technology Centre for Membrane Processes, Iran University of Science and Technology (IUST), Tehran, Iran.
    Nabavi, Mohammad Sadegh
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Mohammadi, Toraj
    Faculty of Chemical Engineering, Research and Technology Centre for Membrane Processes, Iran University of Science and Technology (IUST), Tehran, Iran.
    An experimental study for finding the best condition for PHI zeolite synthesis using Taguchi method for gas separation2018In: Chemical papers, ISSN 2585-7290, Vol. 72, no 5, p. 1139-1149Article in journal (Refereed)
    Abstract [en]

    Phillipsite zeolite particles and membranes were successfully synthesized at different operational and environmental conditions. Using an L9 orthogonal array of the Taguchi method, effects of experimental condition—synthesis temperature (130–150 °C), synthesis time (2–3 days), number of synthesized layers (1–3), and seeding suspension percentage—for membrane preparation with respect to CO2/CH4 ideal selectivity were investigated. The results showed that the ideal selectivity was improved up to 4.20 from 1.15 by increasing the number of synthesized layers, synthesis temperature, and seed solution concentration and by decreasing synthesis time. Moreover, the best synthesis conditions were defined based on the Taguchi method results and the membrane was synthesized with the highest ideal selectivity which was around 4.40. In addition, it was shown that T zeolite is formed beside PHI zeolite at low temperature even with long synthesis time.

  • 33.
    Bertilsson, Olle
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Study of leaching behavior of tin in Zinc-clinker and Mixed Oxide2018Independent thesis Advanced level (professional degree), 20 credits / 30 HE creditsStudent thesis
    Abstract [en]

    Due to the increasing usage of Sn in different electronics, such as solders and in touchscreens, together with Boliden Rönnskärs increased intake of electronic waste as a secondaryraw material, a Zn-containing product called Zn-clinker has increasing amounts of Sn. TheZn-clinker is shipped to Boliden Zn-smelter in Odda, where the Zn-clinker is mixed in withcalcine (roasted concentrate) and leached in several steps. Since Zn-clinker is a product froma halogen removal in a clinker-furnace, the feed material (Mixed Oxide), for this furnace, wasalso investigated since there are plans to replace clinkering with soda-washing in the future.Most of the Sn ends up in the leaching residue which then is deposited in the mountaincaverns close by the Boliden Odda smelter. Boliden is studying the possibility to recoverPb/Ag and Sn content from the leaching residue and create a valuable by-product. Bystudying how the leaching of Sn behaves, together with a characterization of the materials, thefollowing question should be answered: “During which sulphuric acid leaching conditions, ofZn-clinker and Mixed Oxide, is the leaching of Sn minimized?”

    The leaching results for Zn-clinker showed that 8-10% Sn will leach out, despite changingtemperature, redox potential, time and pH. A characterization of the material with SEM-EDSand XRD-analysis was also conducted to see if Sn could be identified in any phases in thematerials. The studies provided enough evidence that Zn2SnO4 could be concluded to be themain phase in the leaching residue for Zn-clinker, a form that would not leach underconditions presented in this project. However, 8-10% of the Sn will come together with Feand when Fe leach out, so does Sn.

    The leaching results for Mixed Oxide pointed towards that different phases from them foundin Zn-clinker was present. Sn losses varied between 10-20% but raised to 47% whentemperature was changed to 80 °C during leaching. The SEM-EDS analysis showed that theidentified Sn-phases contained more Sn than in Zn-clinker and together with the leachingresults, a conclusion that Sn would mainly be found as SnO2 or SnO in the Mixed Oxide, butthere is still uncertainty about the distributions of these forms.

    Unfortunately half of the As leached out during the soda-washing for Mixed Oxide, creating aleachate with Cl, F and As that need to be taken care of. This could be challenging andpresenting a costly side-project for the route different from the Zn-clinker route used today.Another observation was that PbCO3 formed during the soda-washing, a phase that willconsume more sulphuric acid during leaching.

  • 34.
    Bhuiyan, Iftekhar Uddin
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Characterization of iron ore green pellets by scanning electron microscopy and X-ray microtomography2011Licentiate thesis, comprehensive summary (Other academic)
    Abstract [en]

    Cryogenic scanning electron microscopy (cryo-SEM), image analysis (IA) of SEM micrographs and X-ray microtomography (XMT) were used to obtain new information about the morphology of iron ore green pellets in this work. Cryo-SEM and freeze fracturing was used to observe entrapped air bubbles and arrangement of particles around the bubbles and in the matrix of wet green pellets. The observations of samples prepared by plunge and unidirectional freezing indicate that unidirectional freezing facilitates the observation of entrapped bubbles with minimum formation of artifacts, whereas plunge freezing enables observation of the degree of water filling at the outer surface of wet pellets with minimum amount of artifacts. It was also observed in the wet pellets that the size of the water domains in the matrix is quite small and the finer grains are mixed with coarser grains resulting in a denser matrix, whereas no fine grains were observed in the vicinity of the air bubbles. Two types of pellets prepared with and without addition of extra flotation reagent prior to balling were studied using IA and XMT. IA of scanning electron micrographs of epoxy impregnated pellets was used to separate bubble porosity from packing porosity and to quantify the former. The individual SEM micrographs acquired by a backscattered electron detector were reconstructed to provide the entire two-dimensional (2D) sections of the pellets. The 2D data obtained by IA were unfolded to three-dimensional (3D) by stereology and relatively good agreement with XMT data was observed. The size and amount of air bubbles could be quantified with both techniques. The addition of extra flotation reagent was found to increase the number of entrapped air bubbles and slightly decrease the median bubble diameter. The additional entrapped air bubbles due to the addition of extra flotation reagent was shown to be responsible for the difference in total porosity observed by mercury porosimetry between the two types of pellets. Mercury intrusion porosimetry (MIP) is shown in this work to produce inappropriate results with regard to the porosity due to bubble entrapment, it only provides values for total porosity and the throat size distribution of the porosity. In summary, this work has shown that cryo-SEM, IA of SEM micrographs and XMT are powerful and very useful methods for characterization of the morphology of iron ore green pellets.

  • 35.
    Bhuiyan, Iftekhar Uddin
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Microstructural characterization of iron ore green pellets2013Doctoral thesis, comprehensive summary (Other academic)
    Abstract [en]

    The aim of this thesis work was to develop new methodologies to characterize iron ore green pellets, in wet and dry state. The new characterization methods applied and developed in this work were mainly based on scanning electron microscopy (SEM) to gather both qualitative and quantitative data on different components of the pellets, i.e. mineral particles, water, bentonite and entrapped bubbles.In a first attempt to preserve the structure of wet iron ore green pellets by freezing before investigation by cryogenic SEM, wet pellets were frozen in liquid nitrogen by direct plunging or a new method developed in the present work denoted unidirectional freezing. The former method was found useful to study the degree of water filling at the outer surface of the pellet but led to artifacts in the interior of the pellet. The latter method was developed to confirm that the spherical cavities observed in dry pellets were related to entrapped bubbles in wet pellets. Capillaries were observed at the outer surface of the pellets and fine particles were lacking within a layer of approximately 100 µm from the outer surface and also in the direct vicinity of the air bubbles in the interior of the pellets.More advanced freezing methods were subsequently employed to reveal the artifact free microstructure of bentonite in wet pellets. In order to verify the observations made on a slice of a wet pellet frozen by plunging in liquid ethane, SEM investigations were also carried out on a bentonite suspension and a bentonite-iron ore slurry, which could be cryo-fixed by the most reliable freezing method, i.e. high pressure freezing. All microstructures were comparable and consisted in a voluminous network of well-dispersed clay platelets. This network was found to collapse upon drying. Bentonite was drawn to the contact points between the particles and formed what appeared as bridges, which may impart strength to the dry pellets. A combination of energy dispersive spectroscopy (EDS) and imaging by low-loss backscattered electrons at low voltage evidenced the presence of very finely divided silicate species on the magnetite particles. In order to visualize the three dimensional structure of dispersed bentonite clay with unprecedented resolution, a method based on SEM imaging with a monochromatic and decelerated beam was used for the first time. The recorded images showed very well-dispersed clay platelets forming a fine network of Y shaped contacts, which is quite different from earlier reports of much coarser structures formed as a result of poor sample preparation. Finally, in order to gain quantitative data about the porosity due to bubble entrapment in dry pellets, the entire cross-section of dry epoxy embedded and polished pellets were recorded by SEM. The three-dimensional bubble size distribution was unfolded from 2D SEM data using image processing, image analysis and stereological principles. The same type of pellets was also investigated by X-ray micro-tomography (XMT). The resulting three-dimensional dataset allowed the validation of the unfolding procedure based on stereology. However, the lack of resolution obtained by XMT was shown to lead to slight discrepancies with the SEM data for small bubble sizes. Entrapped air bubbles due to the addition of extra flotation reagent in pellets were shown to be responsible for additional porosity observed by mercury intrusion porosimetry (MIP). In summary, useful characterization methods for iron ore pellets based on SEM have been developed in this work, which opens up new possibilities to for instance study agglomeration processes in more detail.

  • 36.
    Bhuiyan, Iftekhar Uddin
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Mouzon, Johanne
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Forsberg, Fredrik
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Fluid and Experimental Mechanics.
    Forsmo, S.P.E.
    LKAB, Research & Development, 983 81 Malmberget.
    Sjödahl, Mikael
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Fluid and Experimental Mechanics.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Consideration of X-ray microtomography to quantitatively determine the size distribution of bubble cavities in iron ore pellets2013In: Powder Technology, ISSN 0032-5910, E-ISSN 1873-328X, Vol. 233, p. 312-318Article in journal (Refereed)
    Abstract [en]

    X-ray microtomography data of iron ore green pellets of approx. 12 mm in diameter were recorded using a commercial instrument. The reconstructed volume after thresholding represented a unique dataset consisting of a three-dimensional distribution of equiaxed objects corresponding to bubble cavities. This dataset was used to successfully validate a stereological method to determine the size distribution of spherical objects dispersed in a volume. This was achieved by investigating only a few cross-sectional images of this volume and measuring the profiles left by these objects in the cross-sectional images. Excellent agreement was observed between the size distribution of the bubble cavities obtained by directly classifying their size in the reconstructed volume and that estimated by applying the aforementioned stereological method to eight cross-sectional images of the reconstructed volume. Subsequently, we discuss the possibility of calibrating X-ray tomography data quantitatively using the size distribution of the bubble cavities as a figure of merit and the results obtained by applying the stereological method to SEM images as reference data. This was justified by considering the validity of the stereological method demonstrated by tomography, the accurate thresholding made possible by back-scattered electron imaging and the solid reproducibility of the results obtained by SEM. Using different threshold values for binarization of the X-ray microtomography data and comparing the results to those obtained by SEM, we found that X-ray microtomography can be used after proper calibration against SEM data to measure the total porosity of the bubble cavities but can only provide a rough estimate of the median diameter because of the limited resolution achieved in this study.

  • 37.
    Bhuiyan, Iftekhar Uddin
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Mouzon, Johanne
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Forsmo, S.P.E.
    LKAB.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Quantitative image analysis of bubble cavities in iron ore green pellets2011In: Powder Technology, ISSN 0032-5910, E-ISSN 1873-328X, Vol. 214, no 3, p. 306-312Article in journal (Refereed)
    Abstract [en]

    Scanning electron microscopy and image analysis was used for quantitative analysis of bubble cavities in iron ore green pellets. Two types of pellets prepared with and without addition of flotation reagent prior to balling were studied. The bubble cavity porosity amounted to 2.8% in the pellets prepared without addition of flotation reagent prior to balling. When flotation reagent was added prior to balling, the bubble cavity porosity increased by a factor of 2.4 and the median bubble diameter was decreased slightly. It was also shown that mercury intrusion porosimetry is not suitable for determination of the distribution of bubble cavities. Finally, our data suggested that the difference in total porosity determined by mercury intrusion porosimetry and pycnometry between the two types of pellets was due to the bubble cavities.

  • 38.
    Bhuiyan, Iftekhar Uddin
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Mouzon, Johanne
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Forsmo, S.P.E.
    LKAB Research and Development.
    Forsberg, Fredrik
    Air bubbles in iron ore green pellets due to flotation reagent: characterization by scanning electron microscopy and X-ray microtomography2011Conference paper (Other academic)
  • 39.
    Bhuiyan, Iftekhar Uddin
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Mouzon, Johanne
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering.
    Schröppel, Birgit
    Natural and Medical Sciences Institute (NMI), University of Tübingen.
    Kaech, Andres
    Center for Microscopy and Image Analysis, University of Zurich.
    Dobryden, Illia
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Material Science.
    Forsmo, Seija P.E.
    LKAB, Research & Development, 983 81 Malmberget.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering.
    Microstructure of Bentonite in Iron Ore Green Pellets2014In: Microscopy and Microanalysis, ISSN 1431-9276, E-ISSN 1435-8115, Vol. 20, no 1, p. 33-41Article in journal (Refereed)
    Abstract [en]

    Sodium-activated calcium bentonite is used as a binder in iron ore pellets and is known to increase strength of both wet and dry iron ore green pellets. In this article, the microstructure of bentonite in magnetite pellets is revealed for the first time using scanning electron microscopy. The microstructure of bentonite in wet and dry iron ore pellets, as well as in distilled water, was imaged by various imaging techniques (e.g., imaging at low voltage with monochromatic and decelerated beam or low loss backscattered electrons) and cryogenic methods (i.e., high pressure freezing and plunge freezing in liquid ethane). In wet iron ore green pellets, clay tactoids (stacks of parallel primary clay platelets) were very well dispersed and formed a voluminous network occupying the space available between mineral particles. When the pellet was dried, bentonite was drawn to the contact points between the particles and formed solid bridges, which impart strength to the solid compact.

  • 40.
    Bjorklund, Robert B.
    et al.
    Linköping University.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Sterte, Johan
    Arwin, Hans
    Linköping University.
    Vapor adsorption in thin silicalite-1 films studied by spectroscopic ellipsometry1998In: Journal of Physical Chemistry B, ISSN 1520-6106, E-ISSN 1520-5207, Vol. 102, no 12, p. 2245-2250Article in journal (Refereed)
    Abstract [en]

    Thin films of silicalite-1 grown on silicon substrates were studied by spectroscopic ellipsometry. Analysis of spectra using an optical model consisting of a single porous layer on silicon yielded average film thicknesses of 84 and 223 nm for films synthesized for 10 and 30 h. Void fraction for the films was 0.32-0.33. Vapor adsorption from a nitrogen carrier gas at room temperature was monitored by ellipsometry. Isotherms for different adsorbates were obtained by analysis of spectra taken at different vapor concentrations using an optical model where the void volume was filled with both nitrogen and condensed vapors. Quantification of the condensed vapor amount was based on the changes in refractive index when adsorbates replaced nitrogen in the pores. Adsorbate volumes for water, toluene, 1-propanol, and hexane were 0.12, 0.12, 0.15, and 0.17 cm3 liquid g-1 film, respectively.

  • 41.
    Björklund, Robert B.
    et al.
    Linköping University.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Carlsson, Bill
    Vadstena Varmförzinkning AB.
    Ellipsometric study of oxide removal from steel surfaces in hydrochloric acid solutions1999In: Langmuir, ISSN 0743-7463, E-ISSN 1520-5827, Vol. 15, no 2, p. 494-499Article in journal (Refereed)
    Abstract [en]

    Iron oxide films formed on three different steel surfaces by thermal oxidation were removed in hydrochloric acid solutions at 20 C. The oxide removal process in flowing solutions was followed in situ by ellipsometry. Two different removal mechanisms were observed in 0.5-2 M HCl, one where undermining of the film resulted in large intact pieces of the oxide leaving the substrate surface at the end of the removal period, and one where the film scaled off the surface in small pieces during the entire removal process. Oxide films which exhibited the undermining mechanism were found to contain about 10% hematite (Fe2O3) and 90% magnetite (Fe3O4). The scaling off mechanism was observed for films which were nearly pure magnetite. Optical models were constructed using data from scanning electron microscopy (SEM) and X-ray diffraction (XRD) measurements for the thicknesses and compositions of films after different immersion times in HCl solutions. Spectra calculated from the models agreed well with the experimental spectra.

  • 42.
    Björkvall, Maria
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Minerals and Metallurgical Engineering.
    Studie om dynamiken i en pilotrullkrets med rulltrumma2018Independent thesis Advanced level (professional degree), 20 credits / 30 HE creditsStudent thesis
    Abstract [en]

    Luossavaara-Kiirunavaara AB (LKAB) produce pellets from magnetite iron ore. Pellets are formed by balling moist iron ore concentrate to green pellets, which are then burned to pellets. The green pellets are formed in balling circuits consisting of balling drums and roller decks for screening. In 2017 a pilot scale balling circuit with a drum was completed in LKAB's agglomeration laboratory in Malmberget. The purpose of the pilot balling circuit is to predict the dynamics in a full scale balling circuit under different conditions.

    This master degree project is an initial attempt to study the response in LKAB's pilot circuit in terms of green pellet quality and dynamics in the circuit. The goal was to determine an effective way to run experiments and to investigate whether the pilot circuit can predict the dynamics of balling in large-scale circuits. Pelletizing production is within LKAB's core competence, and therefore the origin and character of the reagents, as well as the design of the pilot balling drum circuit, are confidential. Code names are used for both iron ore concentrates and reagents.

    The work began by creating a test procedure with the aim of running as many different mixtures as possible in the pilot balling circuit during a normal working day. Five different mixtures could be run. Four different additives were tested: bentonite, a flotation reagent (FLOT), an organic binder (OB) and a new development product (UTV). The first experiment in the pilot balling circuit was run with varying doses of bentonite because its impact in balling is well known at LKAB. Experiment two and three, with FLOT and OB, could be compared to previous experience from large scale test runs. The fourth and last experiment was a test of how the pilot circuit predicted the behavior of a new development product UTV. Each type of experiment was performed twice.

    The pilot balling circle predicted well both dynamics and green pellet quality in all three experiments where experience from large-scale runs was available. The new, unknown, UTV product showed improved green pellet quality, without affecting adversely on the dynamics of the circuit. UTV can therefore be an interesting option for a future large scale run at LKAB.

    The developed working schedule worked very well. A "basic analysis package" has been created to facilitate planning of future experiments in the pilot balling circuit. The number of persons needed to run the circuit depends on the number of mixtures and analyzes. For smaller experiments, at least five people is required, in addition to the leader of the experiments. More advanced experiments will demand seven people.

  • 43.
    Bleken, Bjørn Tore L.
    et al.
    Department of Chemistry, InGAP Center for Research-based Innovation, University of Oslo Blindern.
    Wragg, David Stephen
    Department of Chemistry, InGAP Center for Research-based Innovation, University of Oslo Blindern.
    Arstad, Bjørnar
    SINTEF Materials and Chemistry, Blindern.
    Gunnæs, Anette Eleonora
    Department of Physics, University of Oslo FERMiO.
    Mouzon, Johanne
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Helveg, Stig
    Haldor Topsøe A/S.
    Lundegaard, Lars Fahl
    Haldor Topsøe A/S.
    Beato, Pablo
    Haldor Topsøe A/S.
    Bordiga, Silvia
    Department of Chemistry, InGAP Center for Research-based Innovation, University of Oslo Blindern.
    Olsbye, Unni
    Department of Chemistry, InGAP Center for Research-based Innovation, University of Oslo Blindern.
    Svelle, Stian
    Department of Chemistry, InGAP Center for Research-based Innovation, University of Oslo Blindern.
    Lillerud, Karl Petter
    Department of Chemistry, InGAP Center for Research-based Innovation, University of Oslo Blindern.
    Unit cell thick nanosheets of zeolite H-ZSM-5: Structure and activity2013In: Topics in catalysis, ISSN 1022-5528, E-ISSN 1572-9028, Vol. 56, no 9-10, p. 558-566Article in journal (Refereed)
    Abstract [en]

    nosheets of zeolite H-ZSM-5 were synthesized and characterized by X-ray diffraction, transmission electron microscopy (TEM), N2- physisorption, FT-IR spectroscopy, 27Al and 29Si MAS NMR spectroscopy in addition to catalytic testing in conversion of methanol to hydrocarbons (MTH). It was found that Rietveld analysis, involving anisotropic broadening parameters, gave average crystallite dimensions in good agreement with TEM images. The selectivities in MTH is intact in the mesoporous nanosheet H-ZSM-5 with the largest difference being a higher C3/C2 ratio compared to regular H-ZSM-5.

  • 44.
    Brånn, Emma
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering.
    Kartläggning av flotationskinetik i Garpenbergs anrikningsverk.2019Independent thesis Advanced level (professional degree), 20 credits / 30 HE creditsStudent thesis
    Abstract [sv]

    Sammanfattning

    Boliden Mineral AB är intresserade av att göra en omfattande kartläggning av flotationskinetiken i alla sina anrikningsverk. Kartläggning av ett anrikningsverk är en viktig pusselbit för att förbättra processen, se eventuella flaskhalsar och utveckla framtida processmodeller. I en flotationsprocess är det önskvärt med höga utbyten, snabb flotation och ett högt tonnage. Syftet var att göra en kartläggning av flotationsprocessen i Garpenbergs anrikningsverk. Den praktiska delen av examensarbetet var att göra flotationsförsök i labbskala. Resultatet från flotationsförsöken anpassades med hjälp av Minitab för att se vilken första ordningens kinetikmodell som passar bäst.

    Genom att använda olika typer av kinetikmodeller så anpassas kinetiken till labbflotationsstudier, det är till för att förfina modellerna vid uppskalningsberäkningar och utvärderingar av nya malmlinser. De tre första ordningens kinetikmodeller som jämförts är den klassiska modellen, Klimpels modell och den fullständigt blandade modellen. Med dessa gjordes en kartläggning av flotationskinetiken i Garpenbergs anrikningsverk. Materialet som flotationsförsöken utfördes på är tagna från anrikningsverket, där värdemineralen är kopparkis, blyglans och zinkblände.

    Kartläggningen av flotationskinetiken i Garpenberg visas i resultatdelen för varje provtagningspunkt med en sammanfattande diskussionsdel om varje del av processen. Koppar- och blyflotationen visar att det är höga utbyten genom hela processen och att ommalningsdelen i kretsen ger en del förbättringar i utbytet. Vad resultatet visar är att verket går optimalt, och att nästan allt koppar och bly tas ut inom 10 minuters flotation. Modellen som passar bäst är den klassiska modellen för alla provpunkter, förutom för ingående malm där Klimpels modell passar bäst. Kartläggningen för zinkflotationen visar att det är höga utbyten genom hela processen. I sista steget i zinkflotationskretsen är provpunkten andra repeteringen, där är det svårt att flotera enbart zink eftersom det är lätt att gångartsmineral också floteras i detta steg. Övriga provtagningspunkter tyder på att verket går optimalt och att det mesta av Zn är uttaget inom 10 minuters flotationstid. Modellen som passar bäst är den klassiska modellen för alla provpunkter, förutom för andra Zn repeteringskoncentrat där Klimpels modell är bäst. Malkretsflotationens resultatdel visar en flotationskrets med bra utbyte, men på grund av den grövre partikelstorleken floterades det långsammare än övriga flotationstester. För bly passar Klimpels modell bäst och för koppar passar den klassiska modellen bäst.

  • 45.
    Cai, Juanjaun
    et al.
    State Key Laboratory of Materials-Oriented Chemical Engineering, College of Chemistry and Chemical Engineering, Nanjing Tech University, Nanjing, China.
    Jiang, Leilei
    State Key Laboratory of Materials-Oriented Chemical Engineering, College of Chemistry and Chemical Engineering, Nanjing Tech University, Nanjing, China.
    Huaming, Wei
    State Key Laboratory of Materials-Oriented Chemical Engineering, College of Chemistry and Chemical Engineering, Nanjing Tech University, Nanjing, China.
    Chongqing, Wang
    State Key Laboratory of Materials-Oriented Chemical Engineering, College of Chemistry and Chemical Engineering, Nanjing Tech University, Nanjing, China.
    Yu, Liang
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Zhang, Lixiong
    State Key Laboratory of Materials-Oriented Chemical Engineering, College of Chemistry and Chemical Engineering, Nanjing Tech University, Nanjing, China.
    Preparation of carbon/cobalt composite from phenolic resin and ZIF-67 for efficient tannic acid adsorption2019In: Microporous and Mesoporous Materials, ISSN 1387-1811, E-ISSN 1873-3093, Vol. 287, p. 9-17Article in journal (Refereed)
    Abstract [en]

    In the present work, a carbon/cobalt composite was prepared and evaluated for adsorption of ecologically harmful tannic acid (TA). The composite was prepared by simply mixing phenolic resin with ZIF-67 and following by carbonization. TEM and SEM images showed that ZIF-67 was etched by phenolic resin and cobalt nanoparticles were formed and evenly distributed in carbon. Macroporous structure was generated between the carbonized phenolic resin and ZIF-67. N2 adsorption-desorption isotherms results exhibited that the composite also had both micro- and meso-pores (average pore size of 5 nm) with a high surface area of 393 m2 g−1. Porous structure and evenly distributed cobalt nanoparticles facilitated the diffusion and adsorption of TA due to the formation of the complex between TA macromolecules and cobalt. The highest observed adsorption amount was as high as 2778 mg g−1, significantly higher than that of the carbon prepared from carbonization of phenolic resin (205 mg g−1) and ZIF-67 (1375 mg g−1). The carbon composite material is easy to recover and reuse due to the magnetic property. The reuse experiment also showed high stability of the composite. All of the results indicated a great potential of the developed carbon composite material in wastewater treatment in the industry.

  • 46.
    Carabante, Ivan
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Arsenic (V) adsorption on iron oxide: implications for soil remedeation and water purification2012Doctoral thesis, comprehensive summary (Other academic)
    Abstract [en]

    Addition of iron oxide based adsorbents to arsenic contaminated soils has been proposed as a mean to reduce the mobility of arsenic in the soil. However, the conditions in the soil such as pH value, the presence of phosphate after addition of fertilizer to the soil or the presence of Zn (II) as a co-contaminant may affect the adsorption of arsenate on the iron oxide and may therefore have implications for the mobility of arsenic in the remediated soil.In the present work, a new flow method was developed to study the adsorption of arsenate on synthetic iron oxide with high surface area (ferrihydrite) in situ by means of Attenuated Total Reflection – Fourier Transform Infrared (ATR – FTIR) spectroscopy and the method was used for studying how the adsorption of arsenate was affected by the pH/pD value, the presence of phosphate and Zn (II) in the system. The highest adsorption of arsenate was found at pD 4 and decreased as the pD value increased. The arsenate complexes formed on ferrihydrite appeared to be very stable at pD 4, while the stability decreased as the pD value increased. Arsenate showed a higher adsorption affinity than phosphate on ferrihydrite under the conditions studied. However, phosphate was able to replace about 10 % of pre-adsorbed arsenate on ferrihydrite at pD 4 and about 20 % of the pre-adsorbed arsenate at pD 8.5 in equimolar concentrations of phosphate and arsenate. Phosphate replaced 30 % of pre-adsorbed arsenate at pD 4 and up to 50 % of pre-adsorbed arsenate at pD 8.5 when the concentration of phosphate in the system was 5 times higher than that of arsenate. Batch adsorption experiments indicated an enhancement in the arsenate removal from a ferrihydrite suspension in the presence of Zn (II) at pH 8 in accordance with previous reports. However, no adsorption of arsenate on ferrihydrite in the presence of high concentrations of Zn (II) in the system was observed by infrared spectroscopy. Instead, precipitation of zinc hydroxide carbonate followed by arsenate adsorption on the zinc precipitate was found to be the most likely explanation of these results.Although iron oxides are selective towards arsenate, high specific surface areas are required to achieve sufficiently high adsorption capacity. A method of increasing the specific surface area of coarse hematite particles to obtain a good adsorbent was also developed in the present work. The method comprises an acid treatment to produce iron ions followed by hydrolysis to precipitate an iron oxy-hydroxide coating on the hematite particles. While the arsenate adsorption capacity of the original coarse hematite particles was found to be negligible, the sintered coarse hematite particles showed good potential as an adsorbent for arsenate with an adsorption capacity of about 0.65 mg[As]/g.The method developed for studying adsorption on iron oxides by in situ ATR - FTIR spectroscopy was further developed for studying the adsorption of flotation collectors on iron oxides. Iron ore is often separated from gangue minerals by means of reverse flotation in which a surfactant should selectively adsorb on the gangue mineral rendering it hydrophobic. However, unwanted adsorption of the surfactants on the iron oxide has been reported to affect the production of iron ore pellets. A method was developed to study the adsorption of the surfactant Atrac 1563 on synthetic hematite in situ by means of ATR - FTIR spectroscopy. The adsorption of Atrac 1563 on hematite at pH 8.5 was found to mostly occur via interactions between the polar ester and ethoxy groups of the surfactant and the hematite surface.

  • 47.
    Carabante, Ivan
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Study of arsenate adsorption on iron oxide by in situ ATR-FTIR spectroscopy2009Licentiate thesis, comprehensive summary (Other academic)
    Abstract [en]

    Stabilization of arsenic contaminated soils by iron oxides has been proposed as a remediation technique to prevent leaching of arsenate into the environment. However, fundamental studies are needed to establish under which conditions the complexes formed are stable. A new method based on ATR-FTIR spectroscopy was adapted to study the adsorption of arsenate species on iron oxides. The measurements required the use of D2O as solvent. The amount of arsenate complexes adsorbed on the iron oxide increased with decreasing pD in the range studied, viz. pD 4-12. Arsenate complexes adsorbed at pD 4 desorbed from the film to some extent as the pD was increased to 8.5 or 12. The stability of arsenate complexes adsorbed on the iron oxide evidently changed with the change in pD, most likely due to the electrostatic repulsion between the negatively charged oxoanion and the more negatively charged iron oxide as the pD increased. From competitive adsorption experiments it was found that arsenate species were more strongly bonded to the iron oxide than phosphate species. Furthermore, it was found that two different phosphate complexes formed on the iron surface at pD 4, one deuterated and the other one de-deuterated. The complexes showed very different stability. The deuterated phosphate complex was desorbed easily from the iron oxide film as arsenate was added to the system whereas the de-deuterated phosphate complex only desorbed slightly from the film upon adding arsenate.This work has increased the fundamental knowledge of the iron oxide/arsenate/phosphate system, which will be of importance for the development of more effective soil remediation techniques.

  • 48. Carabante, Ivan
    et al.
    Grahn, Mattias
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    In situ ATR-FTIR studies on the competitive adsorption of arsenate and phosphate on ferrihydrite2010In: Journal of Colloid and Interface Science, ISSN 0021-9797, E-ISSN 1095-7103, Vol. 351, no 2, p. 523-531Article in journal (Refereed)
    Abstract [en]

    In the present study, in-situ ATR-FTIR spectroscopy was used for the first time to study the competitive adsorption of phosphate and arsenate on ferrihydrite. Deuterium oxide was used as solvent to facilitate the interpretations of recorded infrared spectra.It was found that arsenate and phosphate adsorbed more strongly at lower pD values, showing similarities in the adsorption behavior as a function of pD. However, arsenate complexes were found to be more strongly adsorbed than phosphate complexes in the pD range studied. About five times higher concentration of phosphate in solution was needed to reduce the absorbance due to pre-adsorbed arsenate to the same relative level as for pre-adsorbed phosphate, which was desorbed using a solution containing equal (molar) concentrations in arsenate and phosphate. At pD 4, two phosphate complexes were adsorbed on the iron oxide, one deuterated and one de-deuterated. When phosphate was pre-adsorbed and arsenate subsequently added to the system, the deuterated phosphate complex desorbed rapidly while the de-deuterated phosphate complex was quite stable. At pD 8.5, only the de-deuterated phosphate complex was adsorbed on the iron oxide. Moreover, the arsenate adsorbed was also predominantly de-deuterated as opposite to the arsenate adsorbed at pD 4. During the substitution experiments the configuration of these complexes on the iron oxide surface did not change. To the best of our knowledge, this is the first time this difference in stability of the different phosphate complexes is reported and shows the power of employing in-situ spectroscopy for this kind of studies.

  • 49. Carabante, Ivan
    et al.
    Grahn, Mattias
    Holmgren, Allan
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    The influence of Zn2+ ions on the adsorption of arsenate onto ferrihydrite studied by in situ ATR-FTIR spectroscopy2010Conference paper (Other academic)
  • 50.
    Carabante, Ivan
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Grahn, Mattias
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Holmgren, Allan
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Kumpiene, Jurate
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Geosciences and Environmental Engineering.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Adsorption of As (V) on iron oxide nanoparticle films studied by in situ ATR-FTIR spectroscopy2009In: Colloids and Surfaces A: Physicochemical and Engineering Aspects, ISSN 0927-7757, E-ISSN 1873-4359, Vol. 346, no 1-3, p. 106-113Article in journal (Refereed)
    Abstract [en]

    Stabilization of arsenic contaminated soils by iron oxides has been proposed as a remediation technique to prevent leaching of arsenate into the environment. Fundamental studies are needed to establish under which conditions the complexes formed are stable. In the present work, a powerful technique, viz. ATR-FTIR spectroscopy, is adapted to studies of adsorption of arsenate species on iron oxides. This technique facilitates acquisition of both quantitative and qualitative in situ adsorption data.In the present work, about 800 nm thick films of 6-lineferrihydrite were deposited on ZnSe ATR crystals. Arsenate adsorption on the ferrihydrite film was studied at pD values ranging from 4 to 12 and at an arsenate concentration of 0.03 mM in D2O solution. The amount of adsorbed arsenate decreased with increasing pD as a result of the more negatively charged iron oxide surface at higher pD values. The adsorption and desorption kinetics were also studied. Arsenate showed a higher adsorption rate within the first 70 minutes and a much lower adsorption rate from 70 up to 300 minutes. The low adsorption rate at longer reaction times was partly due to a low desorption rate of already adsorbed carbonate species adsorbed at the surface. The desorption of carbonate species was evidenced by the appearance of negative absorption bands. The desorption of adsorbed arsenate complexes was examined by flushing with D2O at pD 4 and 8.5 and it was found that the complexes were very stable at pD 4 suggesting formation of mostly inner-sphere complexes whereas a fraction of the complexes at pD 8.5 were less stable than at pD 4, possibly due to the formation of outer-sphere complexes.In summary, the ATR technique was shown to provide in situ information about the adsorption rate, desorption rate and the speciation of the complexes formed within a single experiment, which is very difficult to obtain using other techniques.

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