Effect of the support on the basic and catalytic properties of KF
KF supported by various supports was characterized by DTG-DTA coupled with mass spectral analysis of the gases evolved by the solid, in situ XRD, calorimetry, 19F NMR spectroscopy, and tested in the Michael addition of cyclohexene-2-one with nitroalkanes. After dehydration at low temperatures, from...
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| Veröffentlicht in: | Journal of catalysis 2004-01, Vol.221 (2), p.483-490 |
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| creator | Clacens, Jean-Marc Genuit, Daisy Delmotte, Luc Garcia-Ruiz, Amado Bergeret, Gérard Montiel, Ramon Lopez, Joseph Figueras, François |
| description | KF supported by various supports was characterized by DTG-DTA coupled with mass spectral analysis of the gases evolved by the solid, in situ XRD, calorimetry,
19F NMR spectroscopy, and tested in the Michael addition of cyclohexene-2-one with nitroalkanes. After dehydration at low temperatures, from
19F NMR spectroscopy F is in part as KF when the support is
α-alumina but only as K
3AlF
6 when the support is
γ-alumina. During activation no fluorine is lost. On
α-alumina KF is detected by XRD only after calcination at about 723 K and results in part of the decomposition of K
3AlF
6; it disappears with formation of K
2AlF
5 and KAlO
2 at higher temperatures. A comparison of the results obtained by XRD and NMR suggests that KF is well dispersed on
α-alumina. KF/
α-alumina is a strong base, stronger than KF on
γ-alumina, and more active for Michael reactions. On KF/
α-alumina the Michael condensation of 2-cyclohexen-1-one with nitroalkanes can be achieved in 5 min with an equimolar mixture of reactants. Solvent-free reactions can also be achieved reaching 75% yield in adduct after 8 h, and KF/
α-alumina is also active after simple drying at 393 K, avoiding the usual activation at higher temperatures. |
| doi_str_mv | 10.1016/j.jcat.2003.09.009 |
| format | Article |
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19F NMR spectroscopy, and tested in the Michael addition of cyclohexene-2-one with nitroalkanes. After dehydration at low temperatures, from
19F NMR spectroscopy F is in part as KF when the support is
α-alumina but only as K
3AlF
6 when the support is
γ-alumina. During activation no fluorine is lost. On
α-alumina KF is detected by XRD only after calcination at about 723 K and results in part of the decomposition of K
3AlF
6; it disappears with formation of K
2AlF
5 and KAlO
2 at higher temperatures. A comparison of the results obtained by XRD and NMR suggests that KF is well dispersed on
α-alumina. KF/
α-alumina is a strong base, stronger than KF on
γ-alumina, and more active for Michael reactions. On KF/
α-alumina the Michael condensation of 2-cyclohexen-1-one with nitroalkanes can be achieved in 5 min with an equimolar mixture of reactants. Solvent-free reactions can also be achieved reaching 75% yield in adduct after 8 h, and KF/
α-alumina is also active after simple drying at 393 K, avoiding the usual activation at higher temperatures.</description><identifier>ISSN: 0021-9517</identifier><identifier>EISSN: 1090-2694</identifier><identifier>DOI: 10.1016/j.jcat.2003.09.009</identifier><identifier>CODEN: JCTLA5</identifier><language>eng</language><publisher>Amsterdam: Elsevier Inc</publisher><subject>Activation of supported KF ; Basic strength ; Catalysis ; Chemical Sciences ; Chemistry ; Exact sciences and technology ; General and physical chemistry ; Michael addition ; Solid base ; Solvent-free reactions ; Theory of reactions, general kinetics. Catalysis. Nomenclature, chemical documentation, computer chemistry ; Thermal analysis ; XRD</subject><ispartof>Journal of catalysis, 2004-01, Vol.221 (2), p.483-490</ispartof><rights>2003 Elsevier Inc.</rights><rights>2004 INIST-CNRS</rights><rights>Distributed under a Creative Commons Attribution 4.0 International License</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c428t-bdc181dc537491bf592906a8841264bef2f1ec159036d731400b4f8f3eed3c7b3</citedby><orcidid>0000-0002-0579-217X</orcidid></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktohtml>$$Uhttps://dx.doi.org/10.1016/j.jcat.2003.09.009$$EHTML$$P50$$Gelsevier$$H</linktohtml><link.rule.ids>230,314,780,784,885,3549,27923,27924,45994</link.rule.ids><backlink>$$Uhttp://pascal-francis.inist.fr/vibad/index.php?action=getRecordDetail&idt=15608011$$DView record in Pascal Francis$$Hfree_for_read</backlink><backlink>$$Uhttps://hal.science/hal-00007386$$DView record in HAL$$Hfree_for_read</backlink></links><search><creatorcontrib>Clacens, Jean-Marc</creatorcontrib><creatorcontrib>Genuit, Daisy</creatorcontrib><creatorcontrib>Delmotte, Luc</creatorcontrib><creatorcontrib>Garcia-Ruiz, Amado</creatorcontrib><creatorcontrib>Bergeret, Gérard</creatorcontrib><creatorcontrib>Montiel, Ramon</creatorcontrib><creatorcontrib>Lopez, Joseph</creatorcontrib><creatorcontrib>Figueras, François</creatorcontrib><title>Effect of the support on the basic and catalytic properties of KF</title><title>Journal of catalysis</title><description>KF supported by various supports was characterized by DTG-DTA coupled with mass spectral analysis of the gases evolved by the solid, in situ XRD, calorimetry,
19F NMR spectroscopy, and tested in the Michael addition of cyclohexene-2-one with nitroalkanes. After dehydration at low temperatures, from
19F NMR spectroscopy F is in part as KF when the support is
α-alumina but only as K
3AlF
6 when the support is
γ-alumina. During activation no fluorine is lost. On
α-alumina KF is detected by XRD only after calcination at about 723 K and results in part of the decomposition of K
3AlF
6; it disappears with formation of K
2AlF
5 and KAlO
2 at higher temperatures. A comparison of the results obtained by XRD and NMR suggests that KF is well dispersed on
α-alumina. KF/
α-alumina is a strong base, stronger than KF on
γ-alumina, and more active for Michael reactions. On KF/
α-alumina the Michael condensation of 2-cyclohexen-1-one with nitroalkanes can be achieved in 5 min with an equimolar mixture of reactants. Solvent-free reactions can also be achieved reaching 75% yield in adduct after 8 h, and KF/
α-alumina is also active after simple drying at 393 K, avoiding the usual activation at higher temperatures.</description><subject>Activation of supported KF</subject><subject>Basic strength</subject><subject>Catalysis</subject><subject>Chemical Sciences</subject><subject>Chemistry</subject><subject>Exact sciences and technology</subject><subject>General and physical chemistry</subject><subject>Michael addition</subject><subject>Solid base</subject><subject>Solvent-free reactions</subject><subject>Theory of reactions, general kinetics. Catalysis. Nomenclature, chemical documentation, computer chemistry</subject><subject>Thermal analysis</subject><subject>XRD</subject><issn>0021-9517</issn><issn>1090-2694</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2004</creationdate><recordtype>article</recordtype><recordid>eNp9kM1KxDAURoMoOI6-gKtuXLhovTfpX8DNMMw44oAbXYc0TZiU2pakDszbm1rRndmEL3znXnIIuUVIEDB_aJJGyTGhACwBngDwM7JA4BDTnKfnZAFAMeYZFpfkyvsGADHLygVZbYzRaox6E40HHfnPYehdiN13rKS3KpJdHYXpsj2NIQ2uH7QbrfYT9LK9JhdGtl7f_NxL8r7dvK138f716Xm92scqpeUYV7XCEmuVsSLlWJmMUw65LMsUaZ5W2lCDWmHGgeV1wTAFqFJTGqZ1zVRRsSW5n-ceZCsGZz-kO4leWrFb7cX0BuEUrMyPGLp07irXe--0-QUQxCRMNGISJiZhAnhgeYDuZmiQXsnWONkp6__ILIcyaAu9x7mnw2-PVjvhldWd0rV1QaWoe_vfmi8cOH8E</recordid><startdate>20040125</startdate><enddate>20040125</enddate><creator>Clacens, Jean-Marc</creator><creator>Genuit, Daisy</creator><creator>Delmotte, Luc</creator><creator>Garcia-Ruiz, Amado</creator><creator>Bergeret, Gérard</creator><creator>Montiel, Ramon</creator><creator>Lopez, Joseph</creator><creator>Figueras, François</creator><general>Elsevier Inc</general><general>Elsevier</general><scope>IQODW</scope><scope>AAYXX</scope><scope>CITATION</scope><scope>1XC</scope><orcidid>https://orcid.org/0000-0002-0579-217X</orcidid></search><sort><creationdate>20040125</creationdate><title>Effect of the support on the basic and catalytic properties of KF</title><author>Clacens, Jean-Marc ; Genuit, Daisy ; Delmotte, Luc ; Garcia-Ruiz, Amado ; Bergeret, Gérard ; Montiel, Ramon ; Lopez, Joseph ; Figueras, François</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c428t-bdc181dc537491bf592906a8841264bef2f1ec159036d731400b4f8f3eed3c7b3</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2004</creationdate><topic>Activation of supported KF</topic><topic>Basic strength</topic><topic>Catalysis</topic><topic>Chemical Sciences</topic><topic>Chemistry</topic><topic>Exact sciences and technology</topic><topic>General and physical chemistry</topic><topic>Michael addition</topic><topic>Solid base</topic><topic>Solvent-free reactions</topic><topic>Theory of reactions, general kinetics. Catalysis. Nomenclature, chemical documentation, computer chemistry</topic><topic>Thermal analysis</topic><topic>XRD</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Clacens, Jean-Marc</creatorcontrib><creatorcontrib>Genuit, Daisy</creatorcontrib><creatorcontrib>Delmotte, Luc</creatorcontrib><creatorcontrib>Garcia-Ruiz, Amado</creatorcontrib><creatorcontrib>Bergeret, Gérard</creatorcontrib><creatorcontrib>Montiel, Ramon</creatorcontrib><creatorcontrib>Lopez, Joseph</creatorcontrib><creatorcontrib>Figueras, François</creatorcontrib><collection>Pascal-Francis</collection><collection>CrossRef</collection><collection>Hyper Article en Ligne (HAL)</collection><jtitle>Journal of catalysis</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Clacens, Jean-Marc</au><au>Genuit, Daisy</au><au>Delmotte, Luc</au><au>Garcia-Ruiz, Amado</au><au>Bergeret, Gérard</au><au>Montiel, Ramon</au><au>Lopez, Joseph</au><au>Figueras, François</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Effect of the support on the basic and catalytic properties of KF</atitle><jtitle>Journal of catalysis</jtitle><date>2004-01-25</date><risdate>2004</risdate><volume>221</volume><issue>2</issue><spage>483</spage><epage>490</epage><pages>483-490</pages><issn>0021-9517</issn><eissn>1090-2694</eissn><coden>JCTLA5</coden><abstract>KF supported by various supports was characterized by DTG-DTA coupled with mass spectral analysis of the gases evolved by the solid, in situ XRD, calorimetry,
19F NMR spectroscopy, and tested in the Michael addition of cyclohexene-2-one with nitroalkanes. After dehydration at low temperatures, from
19F NMR spectroscopy F is in part as KF when the support is
α-alumina but only as K
3AlF
6 when the support is
γ-alumina. During activation no fluorine is lost. On
α-alumina KF is detected by XRD only after calcination at about 723 K and results in part of the decomposition of K
3AlF
6; it disappears with formation of K
2AlF
5 and KAlO
2 at higher temperatures. A comparison of the results obtained by XRD and NMR suggests that KF is well dispersed on
α-alumina. KF/
α-alumina is a strong base, stronger than KF on
γ-alumina, and more active for Michael reactions. On KF/
α-alumina the Michael condensation of 2-cyclohexen-1-one with nitroalkanes can be achieved in 5 min with an equimolar mixture of reactants. Solvent-free reactions can also be achieved reaching 75% yield in adduct after 8 h, and KF/
α-alumina is also active after simple drying at 393 K, avoiding the usual activation at higher temperatures.</abstract><cop>Amsterdam</cop><pub>Elsevier Inc</pub><doi>10.1016/j.jcat.2003.09.009</doi><tpages>8</tpages><orcidid>https://orcid.org/0000-0002-0579-217X</orcidid></addata></record> |
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| source | ScienceDirect Journals (5 years ago - present) |
| subjects | Activation of supported KF Basic strength Catalysis Chemical Sciences Chemistry Exact sciences and technology General and physical chemistry Michael addition Solid base Solvent-free reactions Theory of reactions, general kinetics. Catalysis. Nomenclature, chemical documentation, computer chemistry Thermal analysis XRD |
| title | Effect of the support on the basic and catalytic properties of KF |
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