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Continuous-flow strategies towards bio-based glycerol carbonate

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Ernotte, Gaëtan ULiège
Promotor(s) : Monbaliu, Jean-Christophe ULiège
Date of defense : 4-Sep-2017 • Permalink : http://hdl.handle.net/2268.2/3119
Details
Title : Continuous-flow strategies towards bio-based glycerol carbonate
Translated title : [fr] Stratégie de synthèse en flux continu du carbonate de glycérol biosourcé
Author : Ernotte, Gaëtan ULiège
Date of defense  : 4-Sep-2017
Advisor(s) : Monbaliu, Jean-Christophe ULiège
Committee's member(s) : Damblon, Christian ULiège
Toye, Dominique ULiège
Estager, Julien 
Language : English
Number of pages : 52
Keywords : [en] dimethylcarbonate
[en] urea
[en] glycerol
[en] glycerol carbonate
[en] microwave reactor
[en] continuous flow reactor
Discipline(s) : Physical, chemical, mathematical & earth Sciences > Chemistry
Research unit : CiTOS
Target public : Researchers
Professionals of domain
Institution(s) : Université de Liège, Liège, Belgique
Degree: Master en sciences chimiques, à finalité spécialisée
Faculty: Master thesis of the Faculté des Sciences

Abstract

[en] This work aims at developing new routes for the production of glycerol carbonate from bio-based glycerol using dimethylcarbonate or urea derivatives as green acyl-donors. The valorization of glycerol into glycerol carbonate offers large opportunities to many application fields. Both micro-wave and continuous flow strategies were investigated using additives such as catalysts to improve glycerol carbonate synthesis. A convenient LC-MS analytic method was set up to determine glycerol carbonate yield for dimethylcarbonate route. Regarding to dimethylcarbonate as acyl donor, experiments using Bu4NBr, K2CO3, and ILs as catalysts candidates were optimized in microwave reactors conducting the reaction at several time reactions, temperature and mol\% catalyst. Only 1 mol\% of Bu4NBr affords glycerol carbonate in quantitative yields after 2 min at 170 °C. Regarding to urea derivatives as acyl donor, catalysis screening was set up for urea and dimethylurea. Promising results were obtained using Cu2O as catalyst for urea reaction, whereas pressure issues were encountered in micro-wave reactors. Cyclocarbonation of glycerol by urea was implemented in micro-fluidic reactors using either ethanol or formic acid as co-solvent and a packed-bed reactor made of dispersion of Cu2O in glass beads. Using EtOH, two main impurities (named X1 and X2) were unfortunately detected in the medium, but promising results were obtained for 10 min residence time at 180 °C under 34 bar. Using HCOOH, glycerol conversion was totally completed but GC formation was negligible. Instead of the formation of GC, a significant amount of X1 was observed. We noticed that the two main impurities encountered in flow were not observed in microwave experiments. In order to prevent any leaching issues in flow experiments, a convenient method was finally tested to prepare Cu2O on glass beads.


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Author

  • Ernotte, Gaëtan ULiège Université de Liège > Master en sc. chimiques, à fin.

Promotor(s)

Committee's member(s)

  • Damblon, Christian ULiège Université de Liège - ULg > Département de chimie (sciences) > Chimie biologique structurale
    ORBi View his publications on ORBi
  • Toye, Dominique ULiège Université de Liège - ULg > Department of Chemical Engineering > Génie de la réaction et des réacteurs chimiques
    ORBi View his publications on ORBi
  • Estager, Julien Certech > Project Manager
  • Total number of views 73
  • Total number of downloads 2










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