Solventless synthesis of solketal with commercially available sulfonic acid based ion exchange resins and their catalytic performance

As a means to valorize glycerol, the synthesis of solketal through a ketalization reaction with acetone was performed. Mild solventless conditions were applied to test the activity of different commercially available sulfonic ion exchange resins that had already been used for other applications, nam...

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Main Authors: Esteban Jesús, García-Ochoa Félix, Ladero Miguel
Format: Article
Language:English
Published: De Gruyter 2017-02-01
Series:Green Processing and Synthesis
Subjects:
Online Access:https://doi.org/10.1515/gps-2016-0105
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author Esteban Jesús
García-Ochoa Félix
Ladero Miguel
author_facet Esteban Jesús
García-Ochoa Félix
Ladero Miguel
author_sort Esteban Jesús
collection DOAJ
description As a means to valorize glycerol, the synthesis of solketal through a ketalization reaction with acetone was performed. Mild solventless conditions were applied to test the activity of different commercially available sulfonic ion exchange resins that had already been used for other applications, namely: Amberlyst 35dry, Amberlyst 36dry, Purolite CT275DR, Purolite CT276 and Lewatit GF101. Thorough characterization of the resins is herein provided and discussed, including acidity, elemental analysis, thermogravimetric, 13C-NMR, surface area and pore size distribution measurements. Lewatit GF101 showed the best performance reaching a yield to solketal of 47% after 6 h of operation at 313 K using a molar excess of acetone to glycerol of 4.5 to 1, owing to a greater availability of active centers as well as the ease of access to them than in the rest of the resins. Additionally, reutilization with and without regeneration was performed in up to five cycles, showing that Purolite CT276 had the lowest relative drop of its maximum activity, despite being the least active in each of the cycles.
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spelling doaj.art-da5bd3131a7e454abb095f6ccab03b172022-12-21T20:15:13ZengDe GruyterGreen Processing and Synthesis2191-95422191-95502017-02-0161798910.1515/gps-2016-0105Solventless synthesis of solketal with commercially available sulfonic acid based ion exchange resins and their catalytic performanceEsteban Jesús0García-Ochoa Félix1Ladero Miguel2School of Chemical Engineering, University of Birmingham, Edgbaston, Birmingham B15 2TT, UKDepartment of Chemical Engineering, College of Chemical Sciences, Complutense University of Madrid, 28040 Madrid, SpainDepartment of Chemical Engineering, College of Chemical Sciences, Complutense University of Madrid, 28040 Madrid, SpainAs a means to valorize glycerol, the synthesis of solketal through a ketalization reaction with acetone was performed. Mild solventless conditions were applied to test the activity of different commercially available sulfonic ion exchange resins that had already been used for other applications, namely: Amberlyst 35dry, Amberlyst 36dry, Purolite CT275DR, Purolite CT276 and Lewatit GF101. Thorough characterization of the resins is herein provided and discussed, including acidity, elemental analysis, thermogravimetric, 13C-NMR, surface area and pore size distribution measurements. Lewatit GF101 showed the best performance reaching a yield to solketal of 47% after 6 h of operation at 313 K using a molar excess of acetone to glycerol of 4.5 to 1, owing to a greater availability of active centers as well as the ease of access to them than in the rest of the resins. Additionally, reutilization with and without regeneration was performed in up to five cycles, showing that Purolite CT276 had the lowest relative drop of its maximum activity, despite being the least active in each of the cycles.https://doi.org/10.1515/gps-2016-0105catalyst deactivationglycerolion exchange resinsolketalsolventless synthesis
spellingShingle Esteban Jesús
García-Ochoa Félix
Ladero Miguel
Solventless synthesis of solketal with commercially available sulfonic acid based ion exchange resins and their catalytic performance
Green Processing and Synthesis
catalyst deactivation
glycerol
ion exchange resin
solketal
solventless synthesis
title Solventless synthesis of solketal with commercially available sulfonic acid based ion exchange resins and their catalytic performance
title_full Solventless synthesis of solketal with commercially available sulfonic acid based ion exchange resins and their catalytic performance
title_fullStr Solventless synthesis of solketal with commercially available sulfonic acid based ion exchange resins and their catalytic performance
title_full_unstemmed Solventless synthesis of solketal with commercially available sulfonic acid based ion exchange resins and their catalytic performance
title_short Solventless synthesis of solketal with commercially available sulfonic acid based ion exchange resins and their catalytic performance
title_sort solventless synthesis of solketal with commercially available sulfonic acid based ion exchange resins and their catalytic performance
topic catalyst deactivation
glycerol
ion exchange resin
solketal
solventless synthesis
url https://doi.org/10.1515/gps-2016-0105
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AT laderomiguel solventlesssynthesisofsolketalwithcommerciallyavailablesulfonicacidbasedionexchangeresinsandtheircatalyticperformance