Characterization and reactivity of zirconia-doped phosphate ion catalyst prepared by sol–gel route and mechanistic study of acetic acid esterification by ethanol
Phosphated zirconia prepared by sol–gel method has been used as catalyst in esterification reaction of acetic acid with ethanol. Optimization of different preparation parameters on the catalyst was studied, such as the effect of molar ratio n P / n Zr , surfactant assisted synthesis, calcination tem...
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| Veröffentlicht in: | Journal of sol-gel science and technology 2017-11, Vol.84 (2), p.349-360 |
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| creator | Ben Nsir, S. Younes, M. K. Rives, A. Ghorbel, A. |
| description | Phosphated zirconia prepared by sol–gel method has been used as catalyst in esterification reaction of acetic acid with ethanol. Optimization of different preparation parameters on the catalyst was studied, such as the effect of molar ratio
n
P
/
n
Zr
, surfactant assisted synthesis, calcination temperature, and the effect of the drying mode. Catalysts were characterized by N
2
physisorption at −196 °C, X-ray diffraction, FTIR spectroscopy, and
31
P MAS NMR spectroscopy. The obtained results show that an increase in phosphate content partially inhibits the development of tetragonal t-ZrP phase and leads to a rise of both specific area and pore size of the catalyst. Besides, the introduction of the surfactant in the preparation step develops this phase and enhances the size of pores, but decreases specific area. However, calcination of the catalyst allows the development of tetragonal ZrO
2
phase and causes the disappearance of ZrP phase. The evacuation of the solvent at its supercritical conditions promotes the development of both tetragonal phase of zirconia and pore size but slows that of the phases related to the ZrP species. Catalytic properties of acid esterification by ethanol were correlated to catalyst characteristic data, suggesting that t-ZrP phase and doping agent-support interaction stabilize active sites of the catalyst. Kinetic and mechanism study shows that catalytic reaction occurs with a first order and takes place through Eley–Rideal mechanism in which adsorbed acetic acid species react with ethanol in fluid phase to form corresponding ester. Application of Eyring theory shows that the adsorption step is characterized by an endothermic character and a rapid associative mechanism occurs between adsorbed species and the second reactant.
Graphical abstract
Eley–Rideal mechanism of acetic acid esterification by ethanol over xerogel catalyst XZrP
0.05 |
| doi_str_mv | 10.1007/s10971-017-4509-6 |
| format | Article |
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n
P
/
n
Zr
, surfactant assisted synthesis, calcination temperature, and the effect of the drying mode. Catalysts were characterized by N
2
physisorption at −196 °C, X-ray diffraction, FTIR spectroscopy, and
31
P MAS NMR spectroscopy. The obtained results show that an increase in phosphate content partially inhibits the development of tetragonal t-ZrP phase and leads to a rise of both specific area and pore size of the catalyst. Besides, the introduction of the surfactant in the preparation step develops this phase and enhances the size of pores, but decreases specific area. However, calcination of the catalyst allows the development of tetragonal ZrO
2
phase and causes the disappearance of ZrP phase. The evacuation of the solvent at its supercritical conditions promotes the development of both tetragonal phase of zirconia and pore size but slows that of the phases related to the ZrP species. Catalytic properties of acid esterification by ethanol were correlated to catalyst characteristic data, suggesting that t-ZrP phase and doping agent-support interaction stabilize active sites of the catalyst. Kinetic and mechanism study shows that catalytic reaction occurs with a first order and takes place through Eley–Rideal mechanism in which adsorbed acetic acid species react with ethanol in fluid phase to form corresponding ester. Application of Eyring theory shows that the adsorption step is characterized by an endothermic character and a rapid associative mechanism occurs between adsorbed species and the second reactant.
Graphical abstract
Eley–Rideal mechanism of acetic acid esterification by ethanol over xerogel catalyst XZrP
0.05</description><identifier>ISSN: 0928-0707</identifier><identifier>EISSN: 1573-4846</identifier><identifier>DOI: 10.1007/s10971-017-4509-6</identifier><language>eng</language><publisher>New York: Springer US</publisher><subject>Acetic acid ; Acids ; Catalysis ; Catalysts ; Ceramics ; Chemical synthesis ; Chemistry and Materials Science ; Composites ; Endothermic reactions ; Esterification ; Ethanol ; Evacuation routing ; Eyring theory ; Fourier transforms ; Glass ; Inorganic Chemistry ; Materials Science ; Nanotechnology ; Natural Materials ; NMR spectroscopy ; Optical and Electronic Materials ; Optimization ; Original Paper: Sol-gel and hybrid materials for catalytic ; photoelectrochemical and sensor applications ; Pore size ; Porosity ; Roasting ; Sol-gel processes ; Spectrum analysis ; Surfactants ; X-ray diffraction ; Zirconium dioxide</subject><ispartof>Journal of sol-gel science and technology, 2017-11, Vol.84 (2), p.349-360</ispartof><rights>Springer Science+Business Media, LLC 2017</rights><rights>Copyright Springer Science & Business Media 2017</rights><rights>Journal of Sol-Gel Science and Technology is a copyright of Springer, (2017). All Rights Reserved.</rights><lds50>peer_reviewed</lds50><woscitedreferencessubscribed>false</woscitedreferencessubscribed><citedby>FETCH-LOGICAL-c381t-6e51eb9558a9fc369653687105afc21ffd288932326b61d30c682a3ea3737ee53</citedby><cites>FETCH-LOGICAL-c381t-6e51eb9558a9fc369653687105afc21ffd288932326b61d30c682a3ea3737ee53</cites></display><links><openurl>$$Topenurl_article</openurl><openurlfulltext>$$Topenurlfull_article</openurlfulltext><thumbnail>$$Tsyndetics_thumb_exl</thumbnail><linktopdf>$$Uhttps://link.springer.com/content/pdf/10.1007/s10971-017-4509-6$$EPDF$$P50$$Gspringer$$H</linktopdf><linktohtml>$$Uhttps://link.springer.com/10.1007/s10971-017-4509-6$$EHTML$$P50$$Gspringer$$H</linktohtml><link.rule.ids>314,780,784,27924,27925,41488,42557,51319</link.rule.ids></links><search><creatorcontrib>Ben Nsir, S.</creatorcontrib><creatorcontrib>Younes, M. K.</creatorcontrib><creatorcontrib>Rives, A.</creatorcontrib><creatorcontrib>Ghorbel, A.</creatorcontrib><title>Characterization and reactivity of zirconia-doped phosphate ion catalyst prepared by sol–gel route and mechanistic study of acetic acid esterification by ethanol</title><title>Journal of sol-gel science and technology</title><addtitle>J Sol-Gel Sci Technol</addtitle><description>Phosphated zirconia prepared by sol–gel method has been used as catalyst in esterification reaction of acetic acid with ethanol. Optimization of different preparation parameters on the catalyst was studied, such as the effect of molar ratio
n
P
/
n
Zr
, surfactant assisted synthesis, calcination temperature, and the effect of the drying mode. Catalysts were characterized by N
2
physisorption at −196 °C, X-ray diffraction, FTIR spectroscopy, and
31
P MAS NMR spectroscopy. The obtained results show that an increase in phosphate content partially inhibits the development of tetragonal t-ZrP phase and leads to a rise of both specific area and pore size of the catalyst. Besides, the introduction of the surfactant in the preparation step develops this phase and enhances the size of pores, but decreases specific area. However, calcination of the catalyst allows the development of tetragonal ZrO
2
phase and causes the disappearance of ZrP phase. The evacuation of the solvent at its supercritical conditions promotes the development of both tetragonal phase of zirconia and pore size but slows that of the phases related to the ZrP species. Catalytic properties of acid esterification by ethanol were correlated to catalyst characteristic data, suggesting that t-ZrP phase and doping agent-support interaction stabilize active sites of the catalyst. Kinetic and mechanism study shows that catalytic reaction occurs with a first order and takes place through Eley–Rideal mechanism in which adsorbed acetic acid species react with ethanol in fluid phase to form corresponding ester. Application of Eyring theory shows that the adsorption step is characterized by an endothermic character and a rapid associative mechanism occurs between adsorbed species and the second reactant.
Graphical abstract
Eley–Rideal mechanism of acetic acid esterification by ethanol over xerogel catalyst XZrP
0.05</description><subject>Acetic acid</subject><subject>Acids</subject><subject>Catalysis</subject><subject>Catalysts</subject><subject>Ceramics</subject><subject>Chemical synthesis</subject><subject>Chemistry and Materials Science</subject><subject>Composites</subject><subject>Endothermic reactions</subject><subject>Esterification</subject><subject>Ethanol</subject><subject>Evacuation routing</subject><subject>Eyring theory</subject><subject>Fourier transforms</subject><subject>Glass</subject><subject>Inorganic Chemistry</subject><subject>Materials Science</subject><subject>Nanotechnology</subject><subject>Natural Materials</subject><subject>NMR spectroscopy</subject><subject>Optical and Electronic Materials</subject><subject>Optimization</subject><subject>Original Paper: Sol-gel and hybrid materials for catalytic</subject><subject>photoelectrochemical and sensor applications</subject><subject>Pore size</subject><subject>Porosity</subject><subject>Roasting</subject><subject>Sol-gel processes</subject><subject>Spectrum analysis</subject><subject>Surfactants</subject><subject>X-ray diffraction</subject><subject>Zirconium dioxide</subject><issn>0928-0707</issn><issn>1573-4846</issn><fulltext>true</fulltext><rsrctype>article</rsrctype><creationdate>2017</creationdate><recordtype>article</recordtype><sourceid>AFKRA</sourceid><sourceid>BENPR</sourceid><sourceid>CCPQU</sourceid><sourceid>DWQXO</sourceid><recordid>eNp9kU1uFDEQhS0EEkPIAbKzxNrgn_ZPL9GIPykSG1hbNe7qjKNOu7E9SJMVd-AI3CwniZtmwQZWJZe_9-pJj5ArwV8Lzu2bInhvBePCsk7znpknZCe0VaxznXlKdryXjnHL7XPyopRbzrnuhN2RX_sjZAgVc7yHGtNMYR5oxraK32M90zTS-5hDmiOwIS040OWYynKEinTFA1SYzqXSJeMCuf0fzrSk6eHHzxucaE6nBq6edxiOMMdSY6Clnobf1hBwfUOIA8Wyphhj2HI0G6xNkaaX5NkIU8HLP_OCfH3_7sv-I7v-_OHT_u01C8qJygxqgYdeawf9GJTpjVbGWcE1jEGKcRykc72SSpqDEYPiwTgJCkFZZRG1uiCvNt8lp2-nFsffplOe20kvpe61FIKr_1Gi153unFSmUWKjQk6lZBz9kuMd5LMX3K-N-a0x3xrza2N-1chNUxo732D-y_mfokdlFpxh</recordid><startdate>20171101</startdate><enddate>20171101</enddate><creator>Ben Nsir, S.</creator><creator>Younes, M. K.</creator><creator>Rives, A.</creator><creator>Ghorbel, A.</creator><general>Springer US</general><general>Springer Nature B.V</general><scope>AAYXX</scope><scope>CITATION</scope><scope>8FE</scope><scope>8FG</scope><scope>ABJCF</scope><scope>AFKRA</scope><scope>BENPR</scope><scope>BGLVJ</scope><scope>CCPQU</scope><scope>D1I</scope><scope>DWQXO</scope><scope>HCIFZ</scope><scope>KB.</scope><scope>L6V</scope><scope>M7S</scope><scope>PDBOC</scope><scope>PQEST</scope><scope>PQQKQ</scope><scope>PQUKI</scope><scope>PRINS</scope><scope>PTHSS</scope></search><sort><creationdate>20171101</creationdate><title>Characterization and reactivity of zirconia-doped phosphate ion catalyst prepared by sol–gel route and mechanistic study of acetic acid esterification by ethanol</title><author>Ben Nsir, S. ; Younes, M. K. ; Rives, A. ; Ghorbel, A.</author></sort><facets><frbrtype>5</frbrtype><frbrgroupid>cdi_FETCH-LOGICAL-c381t-6e51eb9558a9fc369653687105afc21ffd288932326b61d30c682a3ea3737ee53</frbrgroupid><rsrctype>articles</rsrctype><prefilter>articles</prefilter><language>eng</language><creationdate>2017</creationdate><topic>Acetic acid</topic><topic>Acids</topic><topic>Catalysis</topic><topic>Catalysts</topic><topic>Ceramics</topic><topic>Chemical synthesis</topic><topic>Chemistry and Materials Science</topic><topic>Composites</topic><topic>Endothermic reactions</topic><topic>Esterification</topic><topic>Ethanol</topic><topic>Evacuation routing</topic><topic>Eyring theory</topic><topic>Fourier transforms</topic><topic>Glass</topic><topic>Inorganic Chemistry</topic><topic>Materials Science</topic><topic>Nanotechnology</topic><topic>Natural Materials</topic><topic>NMR spectroscopy</topic><topic>Optical and Electronic Materials</topic><topic>Optimization</topic><topic>Original Paper: Sol-gel and hybrid materials for catalytic</topic><topic>photoelectrochemical and sensor applications</topic><topic>Pore size</topic><topic>Porosity</topic><topic>Roasting</topic><topic>Sol-gel processes</topic><topic>Spectrum analysis</topic><topic>Surfactants</topic><topic>X-ray diffraction</topic><topic>Zirconium dioxide</topic><toplevel>peer_reviewed</toplevel><toplevel>online_resources</toplevel><creatorcontrib>Ben Nsir, S.</creatorcontrib><creatorcontrib>Younes, M. K.</creatorcontrib><creatorcontrib>Rives, A.</creatorcontrib><creatorcontrib>Ghorbel, A.</creatorcontrib><collection>CrossRef</collection><collection>ProQuest SciTech Collection</collection><collection>ProQuest Technology Collection</collection><collection>Materials Science & Engineering Collection</collection><collection>ProQuest Central</collection><collection>ProQuest Central</collection><collection>Technology Collection</collection><collection>ProQuest One Community College</collection><collection>ProQuest Materials Science Collection</collection><collection>ProQuest Central</collection><collection>SciTech Premium Collection</collection><collection>https://resources.nclive.org/materials</collection><collection>ProQuest Engineering Collection</collection><collection>Engineering Database</collection><collection>Materials science collection</collection><collection>ProQuest One Academic Eastern Edition (DO NOT USE)</collection><collection>ProQuest One Academic</collection><collection>ProQuest One Academic UKI Edition</collection><collection>ProQuest Central China</collection><collection>Engineering collection</collection><jtitle>Journal of sol-gel science and technology</jtitle></facets><delivery><delcategory>Remote Search Resource</delcategory><fulltext>fulltext</fulltext></delivery><addata><au>Ben Nsir, S.</au><au>Younes, M. K.</au><au>Rives, A.</au><au>Ghorbel, A.</au><format>journal</format><genre>article</genre><ristype>JOUR</ristype><atitle>Characterization and reactivity of zirconia-doped phosphate ion catalyst prepared by sol–gel route and mechanistic study of acetic acid esterification by ethanol</atitle><jtitle>Journal of sol-gel science and technology</jtitle><stitle>J Sol-Gel Sci Technol</stitle><date>2017-11-01</date><risdate>2017</risdate><volume>84</volume><issue>2</issue><spage>349</spage><epage>360</epage><pages>349-360</pages><issn>0928-0707</issn><eissn>1573-4846</eissn><abstract>Phosphated zirconia prepared by sol–gel method has been used as catalyst in esterification reaction of acetic acid with ethanol. Optimization of different preparation parameters on the catalyst was studied, such as the effect of molar ratio
n
P
/
n
Zr
, surfactant assisted synthesis, calcination temperature, and the effect of the drying mode. Catalysts were characterized by N
2
physisorption at −196 °C, X-ray diffraction, FTIR spectroscopy, and
31
P MAS NMR spectroscopy. The obtained results show that an increase in phosphate content partially inhibits the development of tetragonal t-ZrP phase and leads to a rise of both specific area and pore size of the catalyst. Besides, the introduction of the surfactant in the preparation step develops this phase and enhances the size of pores, but decreases specific area. However, calcination of the catalyst allows the development of tetragonal ZrO
2
phase and causes the disappearance of ZrP phase. The evacuation of the solvent at its supercritical conditions promotes the development of both tetragonal phase of zirconia and pore size but slows that of the phases related to the ZrP species. Catalytic properties of acid esterification by ethanol were correlated to catalyst characteristic data, suggesting that t-ZrP phase and doping agent-support interaction stabilize active sites of the catalyst. Kinetic and mechanism study shows that catalytic reaction occurs with a first order and takes place through Eley–Rideal mechanism in which adsorbed acetic acid species react with ethanol in fluid phase to form corresponding ester. Application of Eyring theory shows that the adsorption step is characterized by an endothermic character and a rapid associative mechanism occurs between adsorbed species and the second reactant.
Graphical abstract
Eley–Rideal mechanism of acetic acid esterification by ethanol over xerogel catalyst XZrP
0.05</abstract><cop>New York</cop><pub>Springer US</pub><doi>10.1007/s10971-017-4509-6</doi><tpages>12</tpages></addata></record> |
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| identifier | ISSN: 0928-0707 |
| ispartof | Journal of sol-gel science and technology, 2017-11, Vol.84 (2), p.349-360 |
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| subjects | Acetic acid Acids Catalysis Catalysts Ceramics Chemical synthesis Chemistry and Materials Science Composites Endothermic reactions Esterification Ethanol Evacuation routing Eyring theory Fourier transforms Glass Inorganic Chemistry Materials Science Nanotechnology Natural Materials NMR spectroscopy Optical and Electronic Materials Optimization Original Paper: Sol-gel and hybrid materials for catalytic photoelectrochemical and sensor applications Pore size Porosity Roasting Sol-gel processes Spectrum analysis Surfactants X-ray diffraction Zirconium dioxide |
| title | Characterization and reactivity of zirconia-doped phosphate ion catalyst prepared by sol–gel route and mechanistic study of acetic acid esterification by ethanol |
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