In-zeolites prepared by oxidative solid state ion exchange (OSSIE): Surface species and structural characterization
Identifieur interne : 003F45 ( Main/Repository ); précédent : 003F44; suivant : 003F46In-zeolites prepared by oxidative solid state ion exchange (OSSIE): Surface species and structural characterization
Auteurs : RBID : Pascal:10-0159264Descripteurs français
- Pascal (Inist)
- Zéolite, Oxydation, Etat solide, Echange ion, Caractérisation, Indium, Mordénite, Matériau poreux, Catalyseur, Incorporation, Désalumination, Spectrométrie RMN, Aluminium, Oxyde d'indium, Oxyde d'azote, Cristal, Diffraction RX, Dispersion, Spectrométrie photoélectron, Rayon X, Haute température, Imprégnation, Modification, Spectrométrie IR, Déplétion.
- Wicri :
- concept : Aluminium.
English descriptors
- KwdEn :
- Aluminium, Catalyst, Characterization, Crystals, Dealumination, Depletion, Dispersion, High temperature, Impregnation, Incorporation, Indium, Indium oxide, Infrared spectrometry, Ion exchange, Modification, Mordenite, NMR spectrometry, Nitrogen oxide, Oxidation, Photoelectron spectrometry, Porous material, Solid state, X ray, X ray diffraction, Zeolite.
Abstract
The characteristics of surface indium species and the transformations suffered by In-zeolite catalysts during the indium incorporation process by oxidative solid state ion exchange (OSSIE) are studied. This method causes a progressive dealumination of mordenite during the exchange process evidenced by 29Si MAS NMR and 27Al MAS NMR, producing a high proportion of octahedral aluminum that is further distorted at higher temperatures. However, ZSM5 is a much more stable framework for this exchange process. Exchanged indium (InO)+ and highly-dispersed indium oxide species (InxOy) have the ability of adsorbing NO and further oxidizing it towards NO2. Together with these dispersed species, a certain proportion of In2O3 crystals can be observed by XRD, which is higher for In-ZSM5. This zeolite presents a lower threshold dispersion capacity. Wider and asymmetric XPS In 3d5/2 signals indicate the presence of two surface indium species, one of them with a similar behavior to that of bulk oxide albeit not equal, and the other strongly interacting with the zeolite. The high temperature treatment does not modify the amount of surface indium species but changes their relative proportions. The quantity of highly dispersed species is increased on In-mordenite while the opposite occurs as regards on In-ZSM5. This latter zeolite is constituted by small, packed crystals with lower superficial acidic OH groups, which could originate a higher amount of voluminous polynuclear indium cations remaining on the zeolite crystal surface during impregnation, thus provoking the higher proportion of In2O3 outside channels after OSSIE. Structural modifications are also observed by FTIR being higher for mordenite, such as OH depletion by solid-state exchange, dehydroxilation and creation of extra-framework Al-OH species.
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<record><TEI><teiHeader><fileDesc><titleStmt><title xml:lang="en" level="a">In-zeolites prepared by oxidative solid state ion exchange (OSSIE): Surface species and structural characterization</title><author><name sortKey="Zamaro, Juan M" uniqKey="Zamaro J">Juan M. Zamaro</name><affiliation wicri:level="1"><inist:fA14 i1="01"><s1>Instituto de Investigaciones en Católisis y Petroquimica, INCAPE (FIQ, UNL, CONICET) Santiago del Estero 2829</s1><s2>3000, Santa Fe</s2><s3>ARG</s3><sZ>1 aut.</sZ><sZ>2 aut.</sZ><sZ>3 aut.</sZ></inist:fA14><country>Argentine</country><wicri:noRegion>3000, Santa Fe</wicri:noRegion></affiliation></author><author><name sortKey="Miro, Eduardo E" uniqKey="Miro E">Eduardo E. Miro</name><affiliation wicri:level="1"><inist:fA14 i1="01"><s1>Instituto de Investigaciones en Católisis y Petroquimica, INCAPE (FIQ, UNL, CONICET) Santiago del Estero 2829</s1><s2>3000, Santa Fe</s2><s3>ARG</s3><sZ>1 aut.</sZ><sZ>2 aut.</sZ><sZ>3 aut.</sZ></inist:fA14><country>Argentine</country><wicri:noRegion>3000, Santa Fe</wicri:noRegion></affiliation></author><author><name sortKey="Boix, Alicia V" uniqKey="Boix A">Alicia V. Boix</name><affiliation wicri:level="1"><inist:fA14 i1="01"><s1>Instituto de Investigaciones en Católisis y Petroquimica, INCAPE (FIQ, UNL, CONICET) Santiago del Estero 2829</s1><s2>3000, Santa Fe</s2><s3>ARG</s3><sZ>1 aut.</sZ><sZ>2 aut.</sZ><sZ>3 aut.</sZ></inist:fA14><country>Argentine</country><wicri:noRegion>3000, Santa Fe</wicri:noRegion></affiliation></author><author><name sortKey="Martinez Hernandez, Angel" uniqKey="Martinez Hernandez A">Angel Martinez-Hernandez</name><affiliation wicri:level="1"><inist:fA14 i1="02"><s1>Facultad de Ciencias Químicas, Universidad Aut6noma de Nuevo Le6n</s1><s2>CP. 66400, N.L.</s2><s3>MEX</s3><sZ>4 aut.</sZ></inist:fA14><country>Mexique</country><wicri:noRegion>CP. 66400, N.L.</wicri:noRegion></affiliation></author><author><name sortKey="Fuentes, Gustavo A" uniqKey="Fuentes G">Gustavo A. Fuentes</name><affiliation wicri:level="1"><inist:fA14 i1="03"><s1>Area de Ingeniería Quimica, Universidad A. Metropolitana - Iztapalapa, A.P. 55-534</s1><s2>09340 D.F.</s2><s3>MEX</s3><sZ>5 aut.</sZ></inist:fA14><country>Mexique</country><wicri:noRegion>09340 D.F.</wicri:noRegion></affiliation></author></titleStmt><publicationStmt><idno type="inist">10-0159264</idno><date when="2010">2010</date><idno type="stanalyst">PASCAL 10-0159264 INIST</idno><idno type="RBID">Pascal:10-0159264</idno><idno type="wicri:Area/Main/Corpus">004790</idno><idno type="wicri:Area/Main/Repository">003F45</idno></publicationStmt><seriesStmt><idno type="ISSN">1387-1811</idno><title level="j" type="abbreviated">Microporous mesoporous mater.</title><title level="j" type="main">Microporous and mesoporous materials</title></seriesStmt></fileDesc><profileDesc><textClass><keywords scheme="KwdEn" xml:lang="en"><term>Aluminium</term><term>Catalyst</term><term>Characterization</term><term>Crystals</term><term>Dealumination</term><term>Depletion</term><term>Dispersion</term><term>High temperature</term><term>Impregnation</term><term>Incorporation</term><term>Indium</term><term>Indium oxide</term><term>Infrared spectrometry</term><term>Ion exchange</term><term>Modification</term><term>Mordenite</term><term>NMR spectrometry</term><term>Nitrogen oxide</term><term>Oxidation</term><term>Photoelectron spectrometry</term><term>Porous material</term><term>Solid state</term><term>X ray</term><term>X ray diffraction</term><term>Zeolite</term></keywords><keywords scheme="Pascal" xml:lang="fr"><term>Zéolite</term><term>Oxydation</term><term>Etat solide</term><term>Echange ion</term><term>Caractérisation</term><term>Indium</term><term>Mordénite</term><term>Matériau poreux</term><term>Catalyseur</term><term>Incorporation</term><term>Désalumination</term><term>Spectrométrie RMN</term><term>Aluminium</term><term>Oxyde d'indium</term><term>Oxyde d'azote</term><term>Cristal</term><term>Diffraction RX</term><term>Dispersion</term><term>Spectrométrie photoélectron</term><term>Rayon X</term><term>Haute température</term><term>Imprégnation</term><term>Modification</term><term>Spectrométrie IR</term><term>Déplétion</term></keywords><keywords scheme="Wicri" type="concept" xml:lang="fr"><term>Aluminium</term></keywords></textClass></profileDesc></teiHeader><front><div type="abstract" xml:lang="en">The characteristics of surface indium species and the transformations suffered by In-zeolite catalysts during the indium incorporation process by oxidative solid state ion exchange (OSSIE) are studied. This method causes a progressive dealumination of mordenite during the exchange process evidenced by <sup>29</sup>Si MAS NMR and <sup>27</sup>Al MAS NMR, producing a high proportion of octahedral aluminum that is further distorted at higher temperatures. However, ZSM5 is a much more stable framework for this exchange process. Exchanged indium (InO)<sup>+</sup> and highly-dispersed indium oxide species (In<sub>x</sub>O<sub>y</sub>) have the ability of adsorbing NO and further oxidizing it towards NO<sub>2</sub>. Together with these dispersed species, a certain proportion of In<sub>2</sub>O<sub>3</sub> crystals can be observed by XRD, which is higher for In-ZSM5. This zeolite presents a lower threshold dispersion capacity. Wider and asymmetric XPS In 3d<sub>5/2</sub> signals indicate the presence of two surface indium species, one of them with a similar behavior to that of bulk oxide albeit not equal, and the other strongly interacting with the zeolite. The high temperature treatment does not modify the amount of surface indium species but changes their relative proportions. The quantity of highly dispersed species is increased on In-mordenite while the opposite occurs as regards on In-ZSM5. This latter zeolite is constituted by small, packed crystals with lower superficial acidic OH groups, which could originate a higher amount of voluminous polynuclear indium cations remaining on the zeolite crystal surface during impregnation, thus provoking the higher proportion of In<sub>2</sub>O<sub>3</sub> outside channels after OSSIE. Structural modifications are also observed by FTIR being higher for mordenite, such as OH depletion by solid-state exchange, dehydroxilation and creation of extra-framework Al-OH species.</div></front></TEI><inist><standard h6="B"><pA><fA01 i1="01" i2="1"><s0>1387-1811</s0></fA01><fA03 i2="1"><s0>Microporous mesoporous mater.</s0></fA03><fA05><s2>129</s2></fA05><fA06><s2>1-2</s2></fA06><fA08 i1="01" i2="1" l="ENG"><s1>In-zeolites prepared by oxidative solid state ion exchange (OSSIE): Surface species and structural characterization</s1></fA08><fA11 i1="01" i2="1"><s1>ZAMARO (Juan M.)</s1></fA11><fA11 i1="02" i2="1"><s1>MIRO (Eduardo E.)</s1></fA11><fA11 i1="03" i2="1"><s1>BOIX (Alicia V.)</s1></fA11><fA11 i1="04" i2="1"><s1>MARTINEZ-HERNANDEZ (Angel)</s1></fA11><fA11 i1="05" i2="1"><s1>FUENTES (Gustavo A.)</s1></fA11><fA14 i1="01"><s1>Instituto de Investigaciones en Católisis y Petroquimica, INCAPE (FIQ, UNL, CONICET) Santiago del Estero 2829</s1><s2>3000, Santa Fe</s2><s3>ARG</s3><sZ>1 aut.</sZ><sZ>2 aut.</sZ><sZ>3 aut.</sZ></fA14><fA14 i1="02"><s1>Facultad de Ciencias Químicas, Universidad Aut6noma de Nuevo Le6n</s1><s2>CP. 66400, N.L.</s2><s3>MEX</s3><sZ>4 aut.</sZ></fA14><fA14 i1="03"><s1>Area de Ingeniería Quimica, Universidad A. Metropolitana - Iztapalapa, A.P. 55-534</s1><s2>09340 D.F.</s2><s3>MEX</s3><sZ>5 aut.</sZ></fA14><fA20><s1>74-81</s1></fA20><fA21><s1>2010</s1></fA21><fA23 i1="01"><s0>ENG</s0></fA23><fA43 i1="01"><s1>INIST</s1><s2>19627</s2><s5>354000190103970100</s5></fA43><fA44><s0>0000</s0><s1>© 2010 INIST-CNRS. All rights reserved.</s1></fA44><fA45><s0>20 ref.</s0></fA45><fA47 i1="01" i2="1"><s0>10-0159264</s0></fA47><fA60><s1>P</s1></fA60><fA61><s0>A</s0></fA61><fA64 i1="01" i2="1"><s0>Microporous and mesoporous materials</s0></fA64><fA66 i1="01"><s0>NLD</s0></fA66><fC01 i1="01" l="ENG"><s0>The characteristics of surface indium species and the transformations suffered by In-zeolite catalysts during the indium incorporation process by oxidative solid state ion exchange (OSSIE) are studied. This method causes a progressive dealumination of mordenite during the exchange process evidenced by <sup>29</sup>Si MAS NMR and <sup>27</sup>Al MAS NMR, producing a high proportion of octahedral aluminum that is further distorted at higher temperatures. However, ZSM5 is a much more stable framework for this exchange process. Exchanged indium (InO)<sup>+</sup> and highly-dispersed indium oxide species (In<sub>x</sub>O<sub>y</sub>) have the ability of adsorbing NO and further oxidizing it towards NO<sub>2</sub>. Together with these dispersed species, a certain proportion of In<sub>2</sub>O<sub>3</sub> crystals can be observed by XRD, which is higher for In-ZSM5. This zeolite presents a lower threshold dispersion capacity. Wider and asymmetric XPS In 3d<sub>5/2</sub> signals indicate the presence of two surface indium species, one of them with a similar behavior to that of bulk oxide albeit not equal, and the other strongly interacting with the zeolite. The high temperature treatment does not modify the amount of surface indium species but changes their relative proportions. The quantity of highly dispersed species is increased on In-mordenite while the opposite occurs as regards on In-ZSM5. This latter zeolite is constituted by small, packed crystals with lower superficial acidic OH groups, which could originate a higher amount of voluminous polynuclear indium cations remaining on the zeolite crystal surface during impregnation, thus provoking the higher proportion of In<sub>2</sub>O<sub>3</sub> outside channels after OSSIE. Structural modifications are also observed by FTIR being higher for mordenite, such as OH depletion by solid-state exchange, dehydroxilation and creation of extra-framework Al-OH species.</s0></fC01><fC02 i1="01" i2="X"><s0>001C01J08</s0></fC02><fC02 i1="02" i2="X"><s0>001C01I05A</s0></fC02><fC02 i1="03" i2="X"><s0>001C01A03</s0></fC02><fC03 i1="01" i2="X" l="FRE"><s0>Zéolite</s0><s5>01</s5></fC03><fC03 i1="01" i2="X" l="ENG"><s0>Zeolite</s0><s5>01</s5></fC03><fC03 i1="01" i2="X" l="SPA"><s0>Zeolita</s0><s5>01</s5></fC03><fC03 i1="02" i2="X" l="FRE"><s0>Oxydation</s0><s5>02</s5></fC03><fC03 i1="02" i2="X" l="ENG"><s0>Oxidation</s0><s5>02</s5></fC03><fC03 i1="02" i2="X" l="SPA"><s0>Oxidación</s0><s5>02</s5></fC03><fC03 i1="03" i2="X" l="FRE"><s0>Etat solide</s0><s5>03</s5></fC03><fC03 i1="03" i2="X" l="ENG"><s0>Solid state</s0><s5>03</s5></fC03><fC03 i1="03" i2="X" l="SPA"><s0>Estado sólido</s0><s5>03</s5></fC03><fC03 i1="04" i2="X" l="FRE"><s0>Echange ion</s0><s5>04</s5></fC03><fC03 i1="04" i2="X" l="ENG"><s0>Ion exchange</s0><s5>04</s5></fC03><fC03 i1="04" i2="X" l="SPA"><s0>Cambio iónico</s0><s5>04</s5></fC03><fC03 i1="05" i2="X" l="FRE"><s0>Caractérisation</s0><s5>05</s5></fC03><fC03 i1="05" i2="X" l="ENG"><s0>Characterization</s0><s5>05</s5></fC03><fC03 i1="05" i2="X" l="SPA"><s0>Caracterización</s0><s5>05</s5></fC03><fC03 i1="06" i2="X" l="FRE"><s0>Indium</s0><s2>NC</s2><s5>06</s5></fC03><fC03 i1="06" i2="X" l="ENG"><s0>Indium</s0><s2>NC</s2><s5>06</s5></fC03><fC03 i1="06" i2="X" l="SPA"><s0>Indio</s0><s2>NC</s2><s5>06</s5></fC03><fC03 i1="07" i2="X" l="FRE"><s0>Mordénite</s0><s5>07</s5></fC03><fC03 i1="07" i2="X" l="ENG"><s0>Mordenite</s0><s5>07</s5></fC03><fC03 i1="07" i2="X" l="SPA"><s0>Mordenita</s0><s5>07</s5></fC03><fC03 i1="08" i2="X" l="FRE"><s0>Matériau poreux</s0><s5>08</s5></fC03><fC03 i1="08" i2="X" l="ENG"><s0>Porous material</s0><s5>08</s5></fC03><fC03 i1="08" i2="X" l="SPA"><s0>Material poroso</s0><s5>08</s5></fC03><fC03 i1="09" i2="X" l="FRE"><s0>Catalyseur</s0><s5>10</s5></fC03><fC03 i1="09" i2="X" l="ENG"><s0>Catalyst</s0><s5>10</s5></fC03><fC03 i1="09" i2="X" l="SPA"><s0>Catalizador</s0><s5>10</s5></fC03><fC03 i1="10" i2="X" l="FRE"><s0>Incorporation</s0><s5>11</s5></fC03><fC03 i1="10" i2="X" l="ENG"><s0>Incorporation</s0><s5>11</s5></fC03><fC03 i1="10" i2="X" l="SPA"><s0>Incorporación</s0><s5>11</s5></fC03><fC03 i1="11" i2="X" l="FRE"><s0>Désalumination</s0><s5>12</s5></fC03><fC03 i1="11" i2="X" l="ENG"><s0>Dealumination</s0><s5>12</s5></fC03><fC03 i1="11" i2="X" l="SPA"><s0>Desaluminación</s0><s5>12</s5></fC03><fC03 i1="12" i2="X" l="FRE"><s0>Spectrométrie RMN</s0><s5>13</s5></fC03><fC03 i1="12" i2="X" l="ENG"><s0>NMR spectrometry</s0><s5>13</s5></fC03><fC03 i1="12" i2="X" l="SPA"><s0>Espectrometría RMN</s0><s5>13</s5></fC03><fC03 i1="13" i2="X" l="FRE"><s0>Aluminium</s0><s2>NC</s2><s2>FR</s2><s2>FX</s2><s5>14</s5></fC03><fC03 i1="13" i2="X" l="ENG"><s0>Aluminium</s0><s2>NC</s2><s2>FR</s2><s2>FX</s2><s5>14</s5></fC03><fC03 i1="13" i2="X" l="SPA"><s0>Aluminio</s0><s2>NC</s2><s2>FR</s2><s2>FX</s2><s5>14</s5></fC03><fC03 i1="14" i2="X" l="FRE"><s0>Oxyde d'indium</s0><s5>15</s5></fC03><fC03 i1="14" i2="X" l="ENG"><s0>Indium oxide</s0><s5>15</s5></fC03><fC03 i1="14" i2="X" l="SPA"><s0>Indio óxido</s0><s5>15</s5></fC03><fC03 i1="15" i2="X" l="FRE"><s0>Oxyde d'azote</s0><s5>16</s5></fC03><fC03 i1="15" i2="X" l="ENG"><s0>Nitrogen oxide</s0><s5>16</s5></fC03><fC03 i1="15" i2="X" l="SPA"><s0>Nitrógeno óxido</s0><s5>16</s5></fC03><fC03 i1="16" i2="X" l="FRE"><s0>Cristal</s0><s5>17</s5></fC03><fC03 i1="16" i2="X" l="ENG"><s0>Crystals</s0><s5>17</s5></fC03><fC03 i1="16" i2="X" l="SPA"><s0>Cristal</s0><s5>17</s5></fC03><fC03 i1="17" i2="X" l="FRE"><s0>Diffraction RX</s0><s5>18</s5></fC03><fC03 i1="17" i2="X" l="ENG"><s0>X ray diffraction</s0><s5>18</s5></fC03><fC03 i1="17" i2="X" l="SPA"><s0>Difracción RX</s0><s5>18</s5></fC03><fC03 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l="SPA"><s0>Impregnación</s0><s5>23</s5></fC03><fC03 i1="23" i2="X" l="FRE"><s0>Modification</s0><s5>24</s5></fC03><fC03 i1="23" i2="X" l="ENG"><s0>Modification</s0><s5>24</s5></fC03><fC03 i1="23" i2="X" l="SPA"><s0>Modificación</s0><s5>24</s5></fC03><fC03 i1="24" i2="X" l="FRE"><s0>Spectrométrie IR</s0><s5>25</s5></fC03><fC03 i1="24" i2="X" l="ENG"><s0>Infrared spectrometry</s0><s5>25</s5></fC03><fC03 i1="24" i2="X" l="SPA"><s0>Espectrometría IR</s0><s5>25</s5></fC03><fC03 i1="25" i2="X" l="FRE"><s0>Déplétion</s0><s5>26</s5></fC03><fC03 i1="25" i2="X" l="ENG"><s0>Depletion</s0><s5>26</s5></fC03><fC03 i1="25" i2="X" l="SPA"><s0>Depleción</s0><s5>26</s5></fC03><fC07 i1="01" i2="X" l="FRE"><s0>Tamis moléculaire</s0><s5>09</s5></fC07><fC07 i1="01" i2="X" l="ENG"><s0>Molecular sieve</s0><s5>09</s5></fC07><fC07 i1="01" i2="X" l="SPA"><s0>Tamiz molecular</s0><s5>09</s5></fC07><fN21><s1>102</s1></fN21><fN44 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