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Ionic Liquid Mediated Sol-Gel Synthesis in the Presence of Water or Formic Acid: Which Synthesis for Which Material?

  作者 VIAU LYDIE; NEOUZE MARIEALEXANDRA; BIOLLEY CHRISTINE; VOLLAND SABRINA; BREVET DAVID; GAVEAU PHILIPPE; DIEUDONNE PHILIPPE; GALARNEAU ANNE; VIOUX ANDRE  
  选自 期刊  Chemistry of Materials;  卷期  2012年24-16;  页码  3128-3134  
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[摘要]Sol-gel syntheses involving either neutral water or formic acid as a reactant have been investigated (1) to determine the best conditions to confine a maximum of ionic liquid (IL) inside silica based matrixes and (2) to reach the highest porosity after removing the IL from the ion gels (washed gels). Several sets of ionogels were prepared from various 1-butyl-3-methylimidazolium ILs and various silica or organosilica sources. The study evidenced a critical effect of the anion on the morphology (monolith, powder) and texture of the resulting washed gels. Particularly, tetrafluoroborate anion led to monolith ionogels by a simple hydrolytic method, affording highly condensed mesoporous silicas with some fluorinated surface sites. Such sites have never been reported before and were evidenced by F-19 NMR On the other hand, formic acid solvolysis turned out to be the only method to get non exuding, crack free, and transparent monoliths from ILs containing bis(trifluoromethylsulfonyl)imide [NTf2) anion, with promising applications in photochemistry or photosensing. With bulky imidazolium and pyridinium cations, removal of the IL led to highly porous silicas with pore diameters and pore volumes as high as 10-15 nm and 3 cm(3) g(-1), respectively. These silicas could find applications as supports for immobilizing bulky molecules.

 
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