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The Effect of H2 S on Oxidation Properties of Zro2 -Based Biomass

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The Effect of H2 S on Oxidation Properties of Zro2 -Based Biomass Department of Biotechnology and Chemical Technology Aalto- Inkeri Kauppi DD The effect of H S on 214 2 / 2015 2015 oxidation properties of T h e e ZrO -based biomass f f 2 e c t o f H gasification gas clean-up 2 S o n o x catalysts i d a t i o n p r o p e r Inkeri Kauppi t i e s o f Z r O 2 - b a s e d b i o m a s s g a s i fi c a t i o n g a s c l e a n - u p c a t a l y s t s 9HSTFMG*agfida+ ISBN 978-952-60-6583-0 (printed) BUSINESS + ISBN 978-952-60-6584-7 (pdf) ECONOMY ISSN-L 1799-4934 ISSN 1799-4934 (printed) ART + ISSN 1799-4942 (pdf) DESIGN + ARCHITECTURE UniversityAalto Aalto University School of Chemical Technology SCIENCE + Department of Biotechnology and Chemical Technology TECHNOLOGY www.aalto.fi CROSSOVER DOCTORAL DOCTORAL DISSERTATIONS DISSERTATIONS 2015 Aalto University publication series DOCTORAL DISSERTATIONS 214/2015 The effect of H2S on oxidation properties of ZrO2-based biomass gasification gas clean-up catalysts Inkeri Kauppi A doctoral dissertation completed for the degree of Doctor of Science (Technology) to be defended, with the permission of the Aalto University School of Chemical Technology, at a public examination held at the lecture hall Ke2 of the school on 15th of January 2016. Aalto University School of Chemical Technology Department of Biotechnology and Chemical Technology Industrial Chemistry Supervising professor Prof. Juha Lehtonen Thesis advisor Dr. Sc. Jaana Kanervo Preliminary examiners Prof. Dr. Hab. Maria Ziolek Adam Mickiewicz University, Poland Prof. Dr. JH (Harry) Bitter Wageningen University, The Netherlands Opponents Prof. Lars J. Pettersson Kungliga tekniska högskolan (KTH, Royal Institute of Technology), Sweden Aalto University publication series DOCTORAL DISSERTATIONS 214/2015 © Eeva Inkeri Kauppi ISBN 978-952-60-6583-0 (printed) ISBN 978-952-60-6584-7 (pdf) ISSN-L 1799-4934 ISSN 1799-4934 (printed) ISSN 1799-4942 (pdf) http://urn.fi/URN:ISBN:978-952-60-6584-7 Unigrafia Oy Helsinki 2015 Finland Abstract Aalto University, P.O. Box 11000, FI-00076 Aalto www.aalto.fi Author Eeva Inkeri Kauppi Name of the doctoral dissertation The effect of H2S on oxidation properties of ZrO2-based biomass gasification gas clean-up catalysts Publisher School of Chemical Technology Unit Department of Biotechnology and Chemical Technology Series Aalto University publication series DOCTORAL DISSERTATIONS 214/2015 Field of research Industrial Chemistry Manuscript submitted 14 August 2015 Date of the defence 15 January 2016 Permission to publish granted (date) 28 October 2015 Language English Monograph Article dissertation (summary + original articles) Abstract Biomass gasification gas contains impurities which have to be removed before the gas can be utilized in e.g. energy or liquid fuels production. ZrO2-based catalysts can be used to oxidize tar impurities when oxygen is added to the gas. These catalysts have proven activity even when H2S is present. Moreover, an improving effect of H2S on ZrO2 oxidation activity has been observed at temperatures of 600 and 700 °C. Therefore, the reactivities of unsulfided and sulfided ZrO2-based catalysts were studied in order to understand the enhancing effect of sulfur on oxidation activity during gasification gas clean-up. Different adsorption modes of H2S on the ZrO2-based catalysts were established. Molecular adsorption occurred on all the studied catalysts at room temperature. The molecularly adsorbed H2S species are weakly bound and thus are not likely to be present on the surface at the high temperatures of gasification gas clean-up. Therefore, they cannot be the source of the enhanced reactivity, either. Dissociative adsorption of H2S was suggested on cation-anion pairs or by titration of terminal hydroxyl groups on ZrO2 and doped ZrO2. However, the terminal SH groups formed in these surface processes cannot contribute to the observed oxidation activity improvement on ZrO2, as revealed by density functional theory (DFT) calculations. Stable sulfur species formed on the surface of ZrO2 during adsorption of H2S at elevated temperatures (at 100 °C and above). H2S reacts with the surface probably via replacement of surface lattice oxygen at specific defect sites. The amount of sulfur deposited on the surface in these high temperature processes was found to correlate with enhanced oxidation activity compared to unsulfided ZrO2. This indicates that H2S at elevated temperatures produces surface sulfur which improves the redox properties of ZrO2. Based on DFT calculations, sulfur species in the lattice (multicoordinated SH or S) at specific sites can cause enhanced reactivity of lattice oxygen, but so far the exact structure of this site remains unknown. The interaction of H2S with ZrO2 is limited to specific surface sites, comprising not more than approximately 11 % of the surface. Studies on toluene oxidation (a model compound for tar) also indicated that tar oxidation occurs on specific sites where the intermediate species form. Based on observations, it is proposed that the oxidation improvement by sulfur occurs on these specific sites where sulfur improves the reactivity of surface lattice oxygen. The sulfur- tolerance of ZrO2 is thus originated by the limited number of sites capable of binding sulfur. Keywords zirconia, hydrogen sulfide, tar oxidation, gasification gas clean-up ISBN (printed) 978-952-60-6583-0 ISBN (pdf) 978-952-60-6584-7 ISSN-L 1799-4934 ISSN (printed) 1799-4934 ISSN (pdf) 1799-4942 Location of publisher Helsinki Location of printing Helsinki Year 2015 Pages 57 urn http://urn.fi/URN:ISBN:978-952-60-6584-7 Tiivistelmä Aalto-yliopisto, PL 11000, 00076 Aalto www.aalto.fi Tekijä Eeva Inkeri Kauppi Väitöskirjan nimi Rikkivedyn vaikutus biomassan kaasutuskaasun puhdistuksessa käytettävien ZrO2 - katalyyttien hapetusominaisuuksiin Julkaisija Kemian tekniikan korkeakoulu Yksikkö Biotekniikan ja kemian tekniikan laitos Sarja Aalto University publication series DOCTORAL DISSERTATIONS 214/2015 Tutkimusala Teknillinen kemia Käsikirjoituksen pvm 14.08.2015 Väitöspäivä 15.01.2016 Julkaisuluvan myöntämispäivä 28.10.2015 Kieli Englanti Monografia Yhdistelmäväitöskirja (yhteenveto-osa + erillisartikkelit) Tiivistelmä Biomassan kaasutuksessa syntyvän tuotekaasun sisältämät epäpuhtaudet täytyy poistaa ennen kuin kaasua voidaan käyttää esimerkiksi energiantuotannossa tai nestemäisten polttoaineiden valmistukseen. Epäpuhtautena olevat tervat voidaan hapettaa ZrO2- katalyyteillä hapen läsnä ollessa, jopa kaasun sisältäessä rikkivetyä (H2S). Aikaisemmin on todettu, että H2S:llä on ZrO2:n hapetusaktiivisuutta parantava vaikutus lämpötiloissa 600 ja 700 °C. Tämän vuoksi tässä työssä tutkittiin rikittämättömien ja rikitettyjen ZrO2-katalyyttien reaktiivisuutta. Tavoitteena oli löytää syyt H2S:n hapetusaktiivisuutta parantavaan vaikutukseen biomassan kaasutuskaasun puhdistuksessa. H2S adsorboitui molekuläärisesti kaikille katalyyteille huoneen lämpötilassa. Molekuläärisesti adsorboituneet muodot ovat sitoutuneet heikosti eivätkä ole läsnä katalyytillä edellä mainituissa korkeissa lämpötiloissa. Siksi molekuläärisesti adsorboitunut H2S ei ole syy havaittuun hapetusaktiivisuuden paranemiseen. Dissosiatiivinen H2S:n adsorptio tapahtui joko ZrO2:n kationi-anioni pareille tai titraten terminaalisia OH-ryhmiä muodostaen terminaalisia SH-ryhmiä. Terminaaliset SH-ryhmätkään eivät vaikuttaneet ZrO2-pinnan hapen reaktiivisuuteen, mikä havaittiin laskennallisesti. Yli 100 °C:ssa muodostui H2S:n adsorboituessa ZrO2:n pinnalle vahvasti sitoutuneita rikin muotoja, jotka ovat luultavimmin sitoutuneet hilaan syrjäyttäen pinnan happea erityispaikoilla. Tällä tavalla adsorboituneen rikin määrä korreloi lisääntyneen reaktiivisen pintahapen määrään verrattuna puhtaan ZrO2:n pinnan hapen reaktiivisuuteen viitaten siihen, että pinnan hapetus-pelkistys ominaisuudet paranivat. Laskennallisten tulosten perusteella ZrO2:n hilaan liittyneet rikin muodot (multikoordinoitunut SH tai S) voivat parantaa hilahapen reaktiivisuutta erityispaikoilla, kuitenkin näiden paikkojen tarkka luonne on vielä epäselvä. H2S:n vuorovaikutus ZrO2:n kanssa on rajoittunut tietyille erityispaikoille, jotka peittävät enintään 11 % pinnasta. Tutkimukset tervan malliaineena käytetyn tolueenin adsorptiosta ja hapetuksesta osoittivat myös, että tervojen hapetus tapahtuu erityispaikoilla, joille muodostuu reaktiivisia hapetuksen välituotteita. Oletettavasti rikin vaikutuksesta tapahtuva hapetusaktiivisuuden paraneminen tapahtuu näillä erityispaikoilla, joilla rikin läsnäolo parantaa hapetusreaktioon osallistuvan pintahapen reaktiivisuutta. ZrO2-katalyyttien hyvä rikin sietokyky perustuu osin rikkiyhdisteiden rajalliseen reaktiivisuuteen pinnan kanssa. Avainsanat zirkonia, rikkivety, tervojen hapetus, kaasutuskaasun puhdistus ISBN (painettu) 978-952-60-6583-0 ISBN (pdf) 978-952-60-6584-7 ISSN-L 1799-4934 ISSN (painettu) 1799-4934 ISSN (pdf) 1799-4942 Julkaisupaikka Helsinki Painopaikka Helsinki Vuosi 2015 Sivumäärä 57 urn http://urn.fi/URN:ISBN:978-952-60-6584-7 Acknowledgements The work for this thesis was conducted at Aalto University School of Chemical Technology, former Helsinki University of Technology, within the Research Group Industrial Chemistry. The work was made possible financially by Gradu- ate School of Chemical Engineering (GSCE) funded by Academy of Finland. I would also like to thank Finnish Foundation for Technology Promotion and Al- fred Kordelin foundation for financial support. I am indebted to my supervisors, Professors Outi Krause and Juha Lehtonen, for their support and for giving me the possibility to carry out
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