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  • 1.
    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.

  • 2.
    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.

  • 3.
    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.

  • 4.
    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)
  • 5.
    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

  • 6.
    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)
  • 7.
    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.

  • 8. 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.

  • 9. 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.

  • 10. 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.

  • 11.
    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)
  • 12.
    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)
  • 13.
    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.

  • 14.
    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.

  • 15.
    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)
  • 16.
    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.

  • 17.
    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.

  • 18.
    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.

  • 19. 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.

  • 20. 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)
  • 21.
    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.

  • 22.
    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.
    Influence of Zn(II) on the adsorption of arsenate onto ferrihydrite2012In: Environmental Science and Technology, ISSN 0013-936X, E-ISSN 1520-5851, Vol. 46, no 24, p. 13152-13159Article in journal (Refereed)
    Abstract [en]

    Addition of iron oxide to arsenic-contaminated soil has been proposed as a means of reducing the mobility of arsenic in the soil. Arsenic and zinc are common coexisting contaminants in soils. The presence of zinc therefore may affect the adsorption properties of arsenic on iron oxide, and may thus affect its mobility in the soil. The influence of Zn(II) on the adsorption of arsenate ions on iron oxide was studied. Batch adsorption experiments indicated that Zn(II) increased the arsenate removal from a solution by ferrihydrite at pH 8. However, ATR-FTIR spectroscopy showed that no adsorption of arsenate on a ferrihydrite film occurred at pD 8 in the presence of Zn(II). Precipitation of zinc hydroxide carbonate followed by arsenate adorption onto the precipitate was found to be a plausible mechanism explaining the arsenate removal from a solution in the presence of Zn(II) at pH/pD 8. The previously suggested mechanisms attributing the enhanced removal of arsenate from solution in the presence of Zn(II) to additional adsorption on iron oxides could not be verified under the experimental conditions studied. It was also shown that at pH/pD 4, the presence of Zn(II) in the system did not significantly affect the adsorption of arsenate on ferrihydrite.

  • 23.
    Carabante, Ivan
    et al.
    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.
    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.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    A powerful method for studying the adsorption of As(V) on iron oxides in situ2008In: Arsenic in the environment - Arsenic from nature to humans: Book of Abstracts, 2008Conference paper (Other academic)
  • 24.
    Carabante, Ivan
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Geosciences and Environmental Engineering.
    Mouzon, Johanne
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Kumpiene, Jurate
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Geosciences and Environmental Engineering.
    Grahn, Mattias
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Fredriksson, Andreas
    Mining Technology R and D, LKAB Kiruna Mine.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Reutilization of porous sintered hematite bodies as effective adsorbents for arsenic(V) removal from water2014In: Industrial & Engineering Chemistry Research, ISSN 0888-5885, E-ISSN 1520-5045, Vol. 53, no 32, p. 12689-12696Article in journal (Refereed)
    Abstract [en]

    A method was developed to enhance the arsenic adsorption capacity of porous bodies of sintered hematite. The method comprised the formation of a coating of 1 wt % iron oxide nanoparticles on the raw material. The nanoparticles showed two distinct habits: spherical habit, likely ferrihydrite, and acicular habit, likely goethite and/or akaganéite. The specific surface area of the hematite raw material increased from 0.5 to 3.75 m2/g, and the adsorption capacity increased from negligible to 0.65 mg of [As]/g as calculated from equilibrium and breakthrough adsorption data. Equilibrium adsorption data of arsenate on the adsorbent from a solution at pH 5 followed the Langmuir model, while breakthrough adsorption data for a 500 μg/L arsenate solution at pH 5 followed the Thomas model. The adsorbed arsenic could be desorbed using distilled water at pH 12. These results show the potential for the reutilization of waste products comprising coarse hematite bodies as adsorbents.

  • 25.
    Carvalho, Lara
    et al.
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Energy Science.
    Furusjö, Erik
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Energy Science. IVL – Swedish Environmental Institute, Stockholm, Sweden.
    Ma, Chunyan
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Energy Science.
    Ji, Xiaoyan
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Energy Science.
    Lundgren, Joakim
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Energy Science. International Institute for Applied Systems Analysis (IIASA), Laxenburg, Austria.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Grahn, Mattias
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Öhrman, Olov G. W.
    IVL – Swedish Environmental Institute, Stockholm, Sweden;RISE Energy Technology Center AB, Piteå, Sweden.
    Wetterlund, Elisabeth
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Energy Science. International Institute for Applied Systems Analysis (IIASA), Laxenburg, Austria.
    Alkali enhanced biomass gasification with in situ S capture and a novel syngas cleaning: Part 2: Techno-economic analysis2018In: Energy, ISSN 0360-5442, E-ISSN 1873-6785, Vol. 165, no Part B, p. 471-482Article in journal (Refereed)
    Abstract [en]

    Previous research has shown that alkali addition has operational advantages in entrained flow biomass gasification and allows for capture of up to 90% of the biomass sulfur in the slag phase. The resultant low-sulfur content syngas can create new possibilities for syngas cleaning processes. The aim was to assess the techno-economic performance of biofuel production via gasification of alkali impregnated biomass using a novel gas cleaning systemcomprised of (i) entrained flow catalytic gasification with in situ sulfur removal, (ii) further sulfur removal using a zinc bed, (iii) tar removal using a carbon filter, and (iv) CO2 reductionwith zeolite membranes, in comparison to the expensive acid gas removal system (Rectisol technology). The results show that alkali impregnation increases methanol productionallowing for selling prices similar to biofuel production from non-impregnated biomass. It was concluded that the methanol production using the novel cleaning system is comparable to the Rectisol technology in terms of energy efficiency, while showing an economic advantagederived from a methanol selling price reduction of 2–6 €/MWh. The results showed a high level of robustness to changes related to prices and operation. Methanol selling prices could be further reduced by choosing low sulfur content feedstocks.

  • 26.
    Dobryden, Illia
    et al.
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Material Science.
    Potapova, Elisaveta
    Holmgren, Allan
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Weber, Hans
    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.
    Almqvist, Nils
    Luleå University of Technology, Department of Engineering Sciences and Mathematics, Material Science.
    Force interactions between magnetite, silica, and bentonite studied with atomic force microscopy2015In: Physics and chemistry of minerals, ISSN 0342-1791, E-ISSN 1432-2021, Vol. 42, no 4, p. 319-326Article in journal (Refereed)
    Abstract [en]

    Iron ore pellets consist of variety of mineral particles and are an important refined product used in steel manufacturing. Production of high-quality pellets requires good understanding of interactions between different constituents, such as magnetite, gangue residues, bentonite, and additives. Much research has been reported on magnetite, silica, and bentonite surface properties and their effect on pellet strength but more scant with a focus on a fundamental particle–particle interaction. To probe such particle interaction, atomic force microscopy (AFM) using colloidal probe technique has proven to be a suitable tool. In this work, the measurements were performed between magnetite–magnetite, bentonite–magnetite, silica–bentonite, and silica–magnetite particles in 1 mM CaCl2 solution at various pH values. The interaction character, i.e., repulsion or attraction, was determined by measuring and analyzing AFM force curves. The observed quantitative changes in interaction forces were in good agreement with the measured zeta-potentials for the particles at the same experimental conditions. Particle aggregation was studied by measuring the adhesion force. Absolute values of adhesion forces for different systems could not be compared due to the difference in particle size and contact geometry. Therefore, the relative change of adhesion force between pH 6 and 10 was used for comparison. The adhesion force decreased for the magnetite–magnetite and bentonite–silica systems and slightly increased for the magnetite–bentonite system at pH 10 as compared to pH 6, whereas a pronounced decrease in adhesion force was observed in the magnetite–silica system. Thus, the presence of silica particles on the magnetite surface could have a negative impact on the interaction between magnetite and bentonite in balling due to the reduction of the adhesion force.

  • 27.
    Engström, V.
    et al.
    Luleå tekniska universitet.
    Mihailova, Boriana
    Bulgarian Academy of Sciences.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Holmgren, Allan
    Sterte, Johan
    The effect of seed size on the growth of silicalite-1 films on gold surfaces2000In: Microporous and Mesoporous Materials, ISSN 1387-1811, E-ISSN 1873-3093, Vol. 38, no 1, p. 51-60Article in journal (Refereed)
    Abstract [en]

    Silicalite-1 films grown on gold surfaces seeded with colloidal crystals with a size of 60, 165 and 320 nm were investigated by reflection–absorption infrared spectroscopy, scanning electron microscopy and X-ray diffraction in order to follow up the formation of nano-scale defects and to determine the optimal synthesis conditions for preparation of silicalite-1 films with a low concentration of defects. Using 60-nm-sized colloidal crystals, the seeding method was capable of producing silicalite-1 films with low concentrations of defects and with thicknesses ranging from 100 to 300 nm, which are predominantly oriented with the a-axis perpendicular to the surface. Hydrothermal treatment times of the 60-nm-seeded surfaces longer than 36 h as well as the seeding with 165 or 320 nm colloidal crystals substantially enhanced the formation of defects in the films.

  • 28.
    Faisal, Abrar
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Holmlund, Mattias
    Swedish University of Agriculture Sciences.
    Ginesy, Mireille
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Holmgren, Allan
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Enman, Josefine
    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.
    Grahn, Mattias
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Recovery of l-Arginine from Model Solutions and Fermentation Broth Using Zeolite-Y Adsorbent2019In: ACS Sustainable Chemistry & Engineering, ISSN 2168-0485, Vol. 7, no 9, p. 8900-8907Article in journal (Refereed)
    Abstract [en]

    Arginine was produced via fermentation of sugars using the engineered microorganism Escherichia coli. Zeolite-Y adsorbents in the form of powder and extrudates were used to recover arginine from both a real fermentation broth and aqueous model solutions. An adsorption isotherm was determined using model solutions and zeolite-Y powder. The saturation loading was determined to be 0.2 g/g using the Sips model. Arginine adsorbed from a real fermentation broth using either zeolite-Y powder or extrudates both showed a maximum loading of 0.15 g/g at pH 11. This adsorbed loading is very close to the corresponding value obtained from the model solution showing that under the experimental conditions the presence of additional components in the broth did not have a significant effect on the adsorption of arginine. Furthermore, a breakthrough curve was determined for extrudates using a 1 wt % arginine model solution. The selectivity for arginine over ammonia and alanine from the real fermentation broth at pH 11 was 1.9 and 8.3, respectively, for powder, and 1.0, and 4.1, respectively, for extrudates. To the best of our knowledge, this is the first time recovery of arginine from real fermentation broths using any type of adsorbent has been reported.

  • 29.
    Faisal, Abrar
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Zarebska, Agata
    Saremi, Pardis
    Korelskiy, Danil
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering.
    Ohlin, Lindsay
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering.
    Rova, Ulrika
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering.
    Grahn, Mattias
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering.
    MFI zeolite as adsorbent for selective recovery of hydrocarbons from ABE fermentation broths2014In: Adsorption, ISSN 0929-5607, E-ISSN 1572-8757, Vol. 20, no 2-3, p. 465-470Article in journal (Refereed)
    Abstract [en]

    1-Butanol and butyric acid are two interesting compounds that may be produced by acetone, butanol, and ethanol fermentation using e.g. Clostridium acetobutylicum. The main drawback, restricting the commercialization potential of this process, is the toxicity of butanol for the cell culture resulting in low concentrations of this compound in the broth. To make this process economically viable, an efficient recovery process has to be developed. In this work, a hydrophobic MFI type zeolite with high silica to alumina ratio was evaluated as adsorbent for the recovery of butanol and butyric acid from model solutions. Dual component adsorption experiments revealed that both butanol and butyric acid showed a high affinity for the hydrophobic MFI zeolite when adsorbed from aqueous model solutions. Multicomponent adsorption experiments using model solutions, mimicking real fermentation broths, revealed that the adsorbent was very selective to the target compounds. Further, the adsorption of butyric and acetic acid was found to be pH dependent with high adsorption below, and low adsorption above, the respective pKa values of the acids. Thermal desorption of butanol from MFI type zeolite was also studied and a suitable desorption temperature was identified.

  • 30.
    Faisal, Abrar
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Zhou, Ming
    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.
    Grahn, Mattias
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Erratum to: Recovery of butanol from model ABE fermentation broths Using MFI adsorbent: A comparison between traditional beads and a structured adsorbent in the form of a film2016In: Adsorption, ISSN 0929-5607, E-ISSN 1572-8757, Vol. 22, no 3, p. 409-Article in journal (Refereed)
  • 31.
    Faisal, Abrar
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Zhou, Ming
    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.
    Grahn, Mattias
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Recovery of butanol from model ABE fermentation broths Using MFI adsorbent: A comparison between traditional beads and a structured adsorbent in the form of a film2016In: Adsorption, ISSN 0929-5607, E-ISSN 1572-8757, Vol. 22, no 2, p. 205-214Article in journal (Refereed)
    Abstract [en]

    Butanol, a promising biofuel, can be produced by ABE (acetone, butanol and ethanol) fermentation using e.g. Clostridium acetobutylicum. However, the butanol concentration in the resulting broth is limited to only ca. 20 g/L due to the toxicity for the microorganisms. This low product concentration demands an efficient recovery process for successful commercialization of this process. In this study, a structured adsorbent in the form of steel monolith coated with a silicalite-1 film was prepared using the in situ growth method. The adsorbent was carefully characterized by SEM and XRD. The performance of the adsorbent was evaluated by performing breakthrough experiments at room temperature using model ABE fermentation broths and the performance was compared with that of traditional adsorbents in the form of beads. The structured silicalite-1 adsorbent showed less saturation loading time as compared to commercial binder free silicalite-1 beads, reflecting the different dimensions of the columns used, set by experimental constraints. Studies of the desorption process showed that by operating at appropriate conditions, butanol with high concentration i.e. up to 95.2 wt% for butanol–water model system and 88.5 wt% for ABE fermentation broth can be obtained using the structured silicalite-1 adsorbent. Commercial silicalite-1 beads also showed good selectivity but the concentration of butanol in the desorbed product was limited to 70 % for the butanol–water model system and 69 % for ABE fermentation broth, probably as a result of entrained liquid between the beads.

  • 32.
    Faisal, Abrar
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering. Department of Chemical Engineering COMSATS Institute of Information Technology Lahore.
    Zhou, Ming
    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.
    Grahn, Mattias
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Zeolite MFI adsorbent for recovery of butanol from ABE fermentation broths produced from an inexpensive black liquor-derived hydrolyzate2018In: Biomass Conversion and Biorefinery, ISSN 2190-6815, E-ISSN 2190-6823, Vol. 8, no 3, p. 679-687Article in journal (Refereed)
    Abstract [en]

    In this work, high-silica MFI zeolite adsorbent was evaluated for selective recovery of butanol from a real ABE (acetone, butanol, and ethanol) fermentation broth by batch adsorption measurements. The fermentation broth was produced using a hydrolyzate originating from Kraft black liquor, an internal stream in pulp mills, i.e., a low-cost substrate. The adsorbent was very selective towards butanol and butyric acid and became nearly saturated with a mixture of butanol and butyric acid with relative amounts of butanol and butyric acid depending on the pH. The presence of phenolic compounds in significant amounts in the fermentation broths, originating from the black liquor hydrolyzate, did not affect the adsorption of butanol and butyric acid.

  • 33.
    Farzaneh, Amirfarrokh
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Zhou, Ming
    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.
    Bacsik, Zoltan
    Department of Materials and Environmental Chemistry, Stockholm University.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Holmgren, Allan
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Grahn, Mattias
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Adsorption of Butanol and Water Vapors in Silicalite‑1 Films with a Low Defect Density2016In: Langmuir, ISSN 0743-7463, E-ISSN 1520-5827, Vol. 32, p. 11789-11798Article in journal (Refereed)
    Abstract [en]

    Pure silica zeolites are potentially hydrophobic and have therefore been considered to be interesting candidates for separating alcohols, e.g., 1-butanol, from water. Zeolites are traditionally synthesized at high pH, leading to the formation of intracrystalline defects in the form of silanol defects in the framework. These silanol groups introduce polar adsorption sites into the framework, potentially reducing the adsorption selectivity toward alcohols in alcohol/water mixtures. In contrast, zeolites prepared at neutral pH using the fluoride route contain significantly fewer defects. Such crystals should show a much higher butanol/water selectivity than crystals prepared in traditional hydroxide (OH−) media. Moreover, silanol groups are present at the external surface of the zeolite crystals; therefore, minimizing the external surface of the studied adsorbent is important. In this work, we determine adsorption isotherms of 1-butanol and water in silicalite-1 films prepared in a fluoride (F−) medium using in situ attenuated total reflectance−Fourier transform infrared (ATR−FTIR) spectroscopy. This film was composed of well intergrown, plate-shaped b-oriented crystals, resulting in a low external area. Single-component adsorption isotherms of 1-butanol and water were determined in the temperature range of 35− 80 °C. The 1-butanol isotherms were typical for an adsorbate showing a high affinity for a microporous material and a large increase in the amount adsorbed at low partial pressures of 1-butanol. The Langmuir−Freundlich model was successfully fitted to the 1-butanol isotherms, and the heat of adsorption was determined. Water showed a very low affinity for the adsorbent, and the amounts adsorbed were very similar to previous reports for large silicalite-1 crystals prepared in a fluoride medium. The sample also adsorbed much less water than did a reference silicalite-1(OH−) film containing a high density of internal defects.The results show that silicalite-1 films prepared in a F− medium with a low density of defects and external area are very promising for the selective recovery of 1-butanol from aqueous solutions.

  • 34.
    Farzaneh, Amirfarrokh
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Zhou, Ming
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Potapova, Elisaveta
    Bacsik, Zoltan
    Department of Materials and Environmental Chemistry, Stockholm University.
    Ohlin, Lindsay
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Holmgren, Allan
    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.
    Grahn, Mattias
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Adsorption of Water and Butanol in Silicalite-1 Film Studied with in-situ ATR-FTIR Spectroscopy2015In: Langmuir, ISSN 0743-7463, E-ISSN 1520-5827, Vol. 31, no 17, p. 4887-4894Article in journal (Refereed)
    Abstract [en]

    Biobutanol produced by, e.g., acetone–butanol–ethanol (ABE) fermentation is a promising alternative to petroleum-based chemicals as, e.g., solvent and fuel. Recovery of butanol from dilute fermentation broths by hydrophobic membranes and adsorbents has been identified as a promising route. In this work, the adsorption of water and butanol vapor in a silicalite-1 film was studied using in situ attenuated total reflectance–Fourier transform infrared (ATR–FTIR) spectroscopy to better understand the adsorption properties of silicalite-1 membranes and adsorbents. Single-component adsorption isotherms were determined in the temperature range of 35–120 °C, and the Langmuir model was successfully fitted to the experimental data. The adsorption of butanol is very favorable compared to that of water. When the silicalite-1 film was exposed to a butanol/water vapor mixture with 15 mol % butanol (which is the vapor composition of an aqueous solution containing 2 wt % butanol, a typical concentration in an ABE fermentation broth, i.e., the composition of the gas obtained from gas stripping of an ABE broth) at 35 °C, the adsorption selectivity toward butanol was as high as 107. These results confirm that silicalite-1 quite selectively adsorbs hydrocarbons from vapor mixtures. To the best of our knowledge, this is the first comprehensive study on the adsorption of water and butanol in silicalite-1 from vapor phase.

  • 35.
    Filippov, Andrei
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Dvinskikh, Sergey V.
    Royal Institute of Technology.
    Khakimov, Aidar
    Kazan (Volga Region) Federal University, Kazan.
    Grahn, Mattias
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Zhou, Han
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Furo, Istvan
    Royal Institute of Technology.
    Antzutkin, Oleg
    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.
    Dynamic properties of water in silicalite-1 powder2012In: Magnetic Resonance Imaging, ISSN 0730-725X, E-ISSN 1873-5894, Vol. 30, no 7, p. 1022-1031Article in journal (Refereed)
    Abstract [en]

    Self-diffusion of D 2O in partially filled silicalite-1 crystals was studied at 25°C by 2H nuclear magnetic resonance (NMR) with bipolar field gradient pulses and longitudinal Eddy-current-delay. For the first time, reliable experimental diffusion data for this system were obtained. Analysis of NMR diffusion decays revealed the presence of a continuous distribution of apparent self-diffusion coefficients (SDCs) of water, ranging from 10 -7 to ~10 -10 m 2/s, which include values much higher and lower than that of bulk water (~10 -9 m 2/s) in liquid phase. The observed distribution of SDC changes with variation of the diffusion time in the range of 10-200 ms. A two-site Kärger exchange model was successfully fitted to the data. Finally, the water distribution and exchange in silicalite-1 pores were described by taking into account (a) a gas-like phase in the zeolite pores, a gas-like phase in mesopores and an intercrystalline gas-like phase and (b) intercrystalline liquid droplets with intermediate exchange rate with the other phases. The other phases experience fast exchange on the NMR diffusion time scale. Diffusion coefficients and mean residence times of water in some of these states were estimated

  • 36.
    Garcia, Gustavo
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Aguilar, Wilson
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Carabante, Ivan
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Geosciences and Environmental Engineering.
    Cabrera, Saúl
    Chemistry Research Institute IIQ, San Andres Mayor University UMSA, La Paz.
    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.
    Preparation of zeolite A with excellent optical properties from clay2015In: Journal of Alloys and Compounds, ISSN 0925-8388, E-ISSN 1873-4669, Vol. 619, p. 771-777Article in journal (Refereed)
    Abstract [en]

    Discoloration of zeolite A powder is a common problem when natural raw materials such as kaolin clay are used because of the formation of colored iron compounds. In this study, we report on a novel method to produce zeolite A with excellent optical properties, from clays. The brightness is as high as 94.5 and the yellowness is as low as 3.0. The product is comprised of intergrown zeolite A crystals with cubic habit and a length ranging between 0.5 and 2 μm. Good optical properties are obtained when the raw material contains magnesium, as some natural raw materials do, or alternatively, when a magnesium compound is added to the raw material. Magnesium probably forces iron inside colorless extraneous magnesium aluminosilicate compounds. This simple process appears very promising for the preparation of zeolite A with good optical properties from inexpensive natural raw materials.

  • 37.
    Garcia, Gustavo
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering. Solid State and Theoretical Chemistry, Chemistry Research Institute, San Andres Mayor University.
    Cabrera, Saúl
    Solid State and Theoretical Chemistry, Chemistry Research Institute, San Andres Mayor University, University Campus.
    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.
    Selective synthesis of FAU-type zeolites2018In: Journal of Crystal Growth, ISSN 0022-0248, E-ISSN 1873-5002, Vol. 489, p. 36-41Article in journal (Refereed)
    Abstract [en]

    In the present work, parameters influencing the selectivity of the synthesis of FAU-zeolites from diatomite were studied. The final products after varying synthesis time were characterized by scanning electron microscopy, energy dispersive spectroscopy, X-ray diffraction and gas adsorption. It was found that high concentrations of NaCl could completely inhibit the formation of zeolite P, which otherwise usually forms as soon as maximum FAU crystallinity is reached. In the presence of NaCl, the FAU crystals were stable for extended time after completed crystallization of FAU before formation of sodalite. It was also found that addition of NaCl barely changed the crystallization kinetics of FAU zeolite and only reduced the final FAU particle size and SiO2/Al2O3 ratio slightly. Other salts containing either Na or Cl were also investigated. Our results suggest that there is a synergistic effect between Na+ and Cl-. This is attributed to the formation of (Na4Cl)3+ clusters that stabilize the sodalite cages. This new finding may be used to increase the selectivity of syntheses leading to FAU-zeolites and avoid the formation of undesirable by-products, especially if impure natural sources of aluminosilica are used.

  • 38.
    Garcia, Gustavo
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Cardenas, Edgar
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Cabrera, Saúl
    Chemistry Research Institute IIQ, San Andres Mayor University UMSA, La Paz.
    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.
    Synthesis of zeolite Y from diatomite as silica source2016In: Microporous and Mesoporous Materials, ISSN 1387-1811, E-ISSN 1873-3093, Vol. 219, p. 29-37Article in journal (Refereed)
    Abstract [en]

    Bolivian diatomite was successfully used as a silica source for the synthesis of zeolite Y. Prior to synthesis, the diatomite was leached with sulfuric acid to remove impurities and aluminum sulfate was used as an aluminum source. The raw materials were reacted hydrothermally at 100 °C in water with sodium hydroxide and different Na2O/SiO2 ratios were investigated. The final products were characterized by scanning electron microscopy, X-ray diffraction, gas adsorption and inductively coupled plasma-atomic emission spectroscopy. Diatomites originating from different locations and therefore containing different types and amounts of minerals and clays as impurities were investigated. After optimization of synthesis time, zeolite Y with low SiO2/Al2O3 ratio (3.0–3.9) was obtained at a high yield for high alkalinity conditions (Na2O/SiO2 = 0.85–2.0). Lower Na2O/SiO2 ratios resulted in incomplete dissolution of diatomite and lower yield. Nevertheless, decreasing alkalinity resulted in a steady increase of the SiO2/Al2O3 ratio in zeolite Y. Consequently, it was possible to synthesize almost pure zeolite Y with a SiO2/Al2O3 ratio of 5.3 for a Na2O/SiO2 ratio of 0.6, albeit at a low yield. In this respect, diatomite enables the synthesis of high silica zeolite Y and behaves similarly to colloidal silica in traditional syntheses, with both sources of silica having in common a high degree of polymerization. Interestingly, the presence of minerals and clays in the starting diatomite had marginal effects on the outcome of the synthesis. However, their dissolution resulted in presence of calcium and magnesium in the zeolite Y crystals. Finally, overrun of all investigated compositions resulted in the formation of zeolite P nucleating and growing onto dissolving zeolite Y crystals, which was shown to be triggered when aluminum was completely depleted at high alkalinity

  • 39. Grahn, Mattias
    et al.
    Agarwal, Shilpa
    Luleå tekniska universitet.
    Holmgren, Allan
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    In-situ ATR-FTIR spectroscopy of structured zeolite H-ZSM-5 catalysts2010Conference paper (Other academic)
  • 40.
    Grahn, Mattias
    et al.
    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.
    Maxwell-Stefan modelling of High flux tubular silicalite-1 membranes for CO2 removal from CO2/H2 gas mixtures2014In: Journal of Membrane Science, ISSN 0376-7388, E-ISSN 1873-3123, Vol. 471, p. 328-337Article in journal (Refereed)
    Abstract [en]

    In this work, a Maxwell-Stefan model for high flux tubular silicalite-1 membranes for separation of CO2 from a CO2/H2 mixture was developed. The model concerns tubular membranes operating in a counter flow module and includes transport through flow-through defects in the silicalite-1 film and pressure drop over the graded alumina support. Adsorption and diffusion parameters for perfect silicalite-1 crystals were taken from literature. The flux and selectivity predicted by the model were in reasonably good agreement with experimentally observed data for a ZSM-5 membrane without any fitting of the model. However, the CO2 flux and selectivity measured experimentally for the ZSM-5 membrane were higher than that predicted by the model for a silicalite-1 membrane.The model was used to investigate a case with a 20 000 Nm3/d feed comprised of a 50/50 mixture of CO2/H2 at pressure of 25 bar and a membrane temperature of 296 K. The permeate pressure was 1 bar and 90% of the CO2 permeated the membrane. In this case, the membrane permselectivity and CO2 flux varied along the length of the tubes between 20–26 and 950–396 kg/(m2 h), respectively. Further, both defects and pressure drop over the support were shown to have an adverse effect on the selectivity, which indicates that membrane selectivity can be improved by reducing the flow-through defects and/or by preparing supports with less flow resistance. For a one-stage process, the required membrane area is as small as ca 0.85 m2 and the hydrogen loss through the membrane was 12.4%. For a two-stage process the required membrane area almost doubled to 1.6 m2, however the hydrogen loss through the second membrane is reduced to as little as 2.5%. In summary, this work shows that high flux zeolite membranes may be an interesting option for CO2 removal from synthesis gas.

  • 41.
    Grahn, Mattias
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering.
    Higman, Christopher
    HigmanConsulting GmbH.
    Holmgren, Allan
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering. ZeoMemSweden AB.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Chemical Engineering. ZeoMemSweden AB.
    Efficient syngas upgrading with high flux zeolite membranes2017In: 34th Annual International Pittsburgh Coal Conference: Coal - Energy, Environment and Sustainable Development, PCC 2017, International Pittsburgh Coal Conference , 2017Conference paper (Refereed)
  • 42.
    Grahn, Mattias
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Holmgren, Allan
    Hedlund, Jonas
    Adsorption of n-hexane and p-xylene in thin silicalite-1 films studied by FTIR/ATR spectroscopy2008In: The Journal of Physical Chemistry C, ISSN 1932-7447, E-ISSN 1932-7455, Vol. 112, no 20, p. 7717-7724Article in journal (Refereed)
    Abstract [en]

    Adsorption isotherms for p-xylene and n-hexane in silicalite-1 films with a thickness of 200 nm were determined at 323, 343, 368, 393, and 423 K using Fourier transform infrared/attenuated total reflection (FTIR/ATR) spectroscopy. For both adsorbates, the low-pressure data agreed with literature data for MFI powder and the estimated Henry's constant and adsorption enthalpy were close to previously reported results. The upper region of the n-hexane isotherm (p > 2 kPa at 323 K) was likely influenced by micropores in open grain boundaries, as expected for a polycrystalline film of small (<200 nm) crystals. As for n-hexane, the first part (0 ≤ p ≤ 65 Pa at 323 K) of the p-xylene isotherm agreed with data for powder. However, the saturation capacity was only about half of that previously reported for powders, which indicates that p-xylene molecules do not adsorb in the sinusoidal channels in the film. We speculate that the small crystals used in the present work may behave differently from the larger crystals in previous works. Another explanation for the lower saturation capacity may be the bonding of crystals to the supports, which are known to induce strain in the attached crystals.

  • 43.
    Grahn, Mattias
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Lobanova, Antonia
    Luleå tekniska universitet.
    Holmgren, Allan
    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.
    A novel experimental technique for estimation of molecular orientation in zeolite2007In: Studies in Surface Science and Catalysis, ISSN 0167-2991, Vol. 170, p. 724-731Article in journal (Refereed)
    Abstract [en]

    FTIR spectroscopy in combination with polarized light and an ATR probe coated with a b-oriented ZSM-5 film was for the first time used to determine the orientation of adsorbed molecules in the ZSM-5 structure. Two adsorbates were studied, n-hexane and p-xylene and the results agreed with previously reported results obtained by other experimental techniques.

  • 44.
    Grahn, Mattias
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Lobanova, Antonina
    Luleå tekniska universitet.
    Holmgren, Allan
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Hedlund, Jonas
    Orientational analysis of adsorbates in molecular sieves by FTIR/ATR spectroscopy2008In: Chemistry of Materials, ISSN 0897-4756, E-ISSN 1520-5002, Vol. 20, no 19, p. 6270-6276Article in journal (Refereed)
    Abstract [en]

    ZnS ATR elements were coated with well-defined b-oriented ZSM-5 films by in situ growth. Both adsorption isotherms, as well as molecular orientation of p-xylene adsorbed in the films, were measured at 323 and 373 K by FTIR/ATR spectroscopy. The observed isotherms for the b-oriented ZSM-5 films in the present work were very similar to previously reported isotherms of supported MFI films, albeit the crystals in the latter films were aluminum free (silicalite-1) and orientated differently relative to the support surface than the crystals in the films studied in the present work. The novel technique facilitated, for the first time, the examination of how the tilt angle varies with loading and temperature. The data obtained in the present work showed that the p-xylene molecules were mainly oriented with their long axis parallel to the b-direction of the MFI crystals in concert with previously reported results based on FTIR microscopy, Monte Carlo simulations, NMR, and XRD data. At high concentrations, the tilt angle was in good agreement with observations by FTIR microscopy. It was also found that the orientation of the molecules changed with loading, this might be due to different adsorption geometries in the channel intersection as reported previously. The observed tilt angles may also be influenced from competitive adsorption on silanol groups, as was also indicated in the spectra. The results also indicate that the adsorption properties of zeolite films and powders may differ. Hence, adsorption parameters determined for zeolite powders may not necessarily be applicable to films.

  • 45.
    Grahn, Mattias
    et al.
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Wang, Zheng
    Luleå tekniska universitet.
    Lidström-Larsson, Margareta
    Holmgren, Allan
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Hedlund, Jonas
    Sterte, Johan
    Silicalite-1 coated ATR elements as sensitive chemical sensor probes2005In: Microporous and Mesoporous Materials, ISSN 1387-1811, E-ISSN 1873-3093, Vol. 81, no 1-3, p. 357-363Article in journal (Refereed)
    Abstract [en]

    A novel sensitive chemical sensor probe has been fabricated. The sensor principle is based on silicalite-1 coated ATR (attenuated total reflection) elements and FTIR spectroscopy. The microporous silicalite-1 film enriches the analyte to the probe surface, thus increasing the sensitivity. At a relative pressure of n-hexane in helium of 6 × 10−5 the sensitivity of the probe is approximately 85 times higher for the silicalite-1 coated element compared to a 10 cm transmission gas cell and ca. 180 times higher compared to an uncoated element. The performance of the probe is illustrated by determination of an adsorption isotherm for n-hexane in silicalite-1.

  • 46.
    Gualtieri, Magdalena Lassinantti
    et al.
    Luleå tekniska universitet.
    Andersson, Charlotte
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering.
    Jareman, Fredrik
    Luleå tekniska universitet.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Gualtieri, Alessandro F.
    Dipartimento di Scienze della Terra, Universita di Modena e Reggio Emilia.
    Leoni, Matteo
    Dipartimento di Ingegneria dei Materiali, Università di Trento, I-38050 Mesiano.
    Meneghini, Carlo
    Dipartimento di Fisica ‘E. Amaldi’ Università di Roma Tre, Via della Vasca Navale 84, I-00146 Roma.
    Crack formation in α-alumina supported MFI zeolite membranes studied by in situ high temperature synchrotron powder diffraction2007In: Journal of Membrane Science, ISSN 0376-7388, E-ISSN 1873-3123, Vol. 290, no 1-2, p. 95-104Article in journal (Refereed)
    Abstract [en]

    Cracks are frequently formed in α-alumina supported MFI membranes during calcination. To better understand crack formation, in situ powder diffraction data were collected during calcination of a type of MFI membrane (ca. 1800 nm thick) which is known to crack reproducibly. In addition, data for MFI powder and a blank support were also collected. Both a synchrotron radiation facility and an in-house instrument were used. The unit cell parameters were determined with the Rietveld method, and the strain in the direction perpendicular to the film surface was calculated for the film as well as for the support. The microstrain in the support was also estimated. Based on the results obtained here, a model for crack formation in this type of MFI membrane was proposed. The lack of cracks in other types of MFI membranes (ca. 500 nm) prepared in our laboratory is also explained by the model. In thicker MFI films, the crystals are well intergrown. During heating, the MFI crystals contract and the α-alumina support expands. Consequently, a thermal stress develops in the composite which eventually leads to formation of cracks in the film and structural defects in the support. In thinner films, the crystals are less well intergrown and the thermal expansion mismatch leads to opening of grain boundaries rather than cracks.

  • 47.
    Gualtieri, Magdalena Lassinantti
    et al.
    Luleå tekniska universitet.
    Gualtieri, Alessandro
    Università di Modena e Reggio Emilia.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    The influence of heating rate on template removal in silicalite-1: an in situ HT-XRPD study2006In: Microporous and Mesoporous Materials, ISSN 1387-1811, E-ISSN 1873-3093, Vol. 89, no 1-3, p. 1-8Article in journal (Refereed)
    Abstract [en]

    The effect of heating rate on thermal behavior of TPA-silicalite-1 during calcination and the reaction kinetics for TPA decomposition were investigated. The cell parameters of the TPA-silicalite-1 during the heating cycles were determined with the aid of high temperature X-ray diffraction data and the Rietveld method. The template decomposition is accompanied by a large contraction of the unit cell. The unit cell dimensions during template removal are not affected significantly by the heating rate. Consequently, the rate of contraction is approximately proportional to the heating rate. The intensity of some diffraction peaks changes during heating, especially the 101/011 and the 200/020 peaks. The intensity change of those peaks shows the same dependence with temperature as the TPA occupancy, indicating that these parameters are related. An analysis of the kinetics for TPA decomposition based on the intensity change of the 101/011 and the 200/020 peaks was performed. The apparent activation energy (Ea) of the template decomposition in silicalite-1 determined with the Kissinger and the Flynn–Wall–Ozawa methods was 138 (±25) and 138 (±29) kJ mol−1, respectively. The reaction order, determined with the method of Kennedy and Clark, was close to 0.5 indicating that the rate-limiting step is mono-dimensional diffusion. Ea was 140 (±30) kJ mol−1, in good agreement with the results obtained with the other methods. With the results presented here, it is possible to discuss possible effects of the heating rate on the crack formation frequently observed in zeolite membranes during calcination

  • 48.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Control of the preferred orientation in MFI films synthesized by seeding2000In: Journal of porous materials, ISSN 1380-2224, E-ISSN 1573-4854, Vol. 7, no 4, p. 455-464Article in journal (Refereed)
    Abstract [en]

    Single crystal silicon and quartz wafers were seeded with colloidal TPA-silicate-1 crystals. Hydrothermal treatment of the seeded substrates was used to grow dense MFI films. The preferred orientation of the crystals constituting the films as a function of the amount and size of seeds, film thickness and hydrothermal treatment conditions was investigated. In thin films, most of the crystalline material was found to be oriented with the b-axes close to perpendicular to the substrate surface. In thick films, the a- or c-axes were close to perpendicular to the substrate surface depending on the conditions used for hydrothermal treatment. The seed size and amount was found to affect the rate of change in preferred orientation as a function of film thickness. A film growth mechanism which is able to explain the experimental results is proposed

  • 49.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Thin films of molecular sieves: synthesis and applications1998Doctoral thesis, comprehensive summary (Other academic)
    Abstract [en]

    The seed film method for synthesis of ultra thin and thin molecular sieve films was developed. The versatility of the method was demonstrated by successful preparation of films of a number of molecular sieves (silicate-1, ZSM-5, NA) on various supports (silicon, alumina, gold, etc.). The preferred orientation of the crystalline material could be controlled. Silicate-1 films on silicon wafers were evaluated as optical gas sensors. Sorption isotherms of water, toluene, 1-propanol and n-hexane were recorded. ZSM-5 films with a thickness of 1.5 um were crystallized on a porous support and the membranes were evaluated in permeation experiments. The flux in single gas experiments decreased in the series H2O, H2, CO2, O2, N2 and CH4. The difference in flux between each molecule was about 1 order of magnitude which indicated the high quality of the membranes. The measured separation factors for binary mixtures of N2/SF6 and H2/i-C4 were 99 and 66.

  • 50.
    Hedlund, Jonas
    Luleå University of Technology, Department of Civil, Environmental and Natural Resources Engineering, Sustainable Process Engineering.
    Ultra thin films of molecular sieves1997Licentiate thesis, comprehensive summary (Other academic)
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