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Title: | Partial Hydrolysis of Diphosphonate Ester During the Formation of Hybrid TiO2 Nanoparticles: Role of Acid Concentration | Authors: | Mysore Ramesha, Bharadwaj PAWLAK, Bram Arenas Esteban, Daniel REEKMANS, Gunter Bals, Sara MARCHAL, Wouter CARLEER, Robert ADRIAENSENS, Peter Meynen, Vera |
Issue Date: | 2023 | Publisher: | WILEY-V C H VERLAG GMBH | Source: | CHEMPHYSCHEM, 24 (22) (Art.° e202300437) | Abstract: | The hydrolysis of the phosphonate ester linker during the synthesis of hybrid (organic-inorganic) TiO2 nanoparticles is important when forming porous hybrid organic-inorganic metal phosphonates. In the present work, a method was utilized to control the in-situ partial hydrolysis of diphosphonate ester in the presence of a titania precursor as a function of acid content, and its impact on the hybrid nanoparticles was assessed. Organodiphosphonate esters, and more specific, their hydrolysis degree during the formation of hybrid organic-inorganic metal oxide nanoparticles, are relatively under explored as linkers. Here, a detailed analysis on the hydrolysis of tetraethyl propylene diphosphonate ester (TEPD) as diphosphonate linker to produce hybrid TiO2 nanoparticles is discussed as a function of acid content. Quantitative solution NMR spectroscopy revealed that during the synthesis of TiO2 nanoparticles, an increase in acid concentration introduces a higher degree of partial hydrolysis of the TEPD linker into diverse acid/ester derivatives of TEPD. Increasing the HCl/Ti ratio from 1 to 3, resulted in an increase in degree of partial hydrolysis of the TEPD linker in solution from 4 % to 18.8 % under the applied conditions. As a result of the difference in partial hydrolysis, the linker-TiO2 bonding was altered. Upon subsequent drying of the colloidal TiO2 solution, different textures, at nanoscale and macroscopic scale, were obtained dependent on the HCl/Ti ratio and thus the degree of hydrolysis of TEPD. Understanding such linker-TiO2 nanoparticle surface dynamics is crucial for making hybrid organic-inorganic materials (i. e. (porous) metal phosphonates) employed in applications such as electronic/photonic devices, separation technology and heterogeneous catalysis. | Notes: | Meynen, V (corresponding author), Univ Antwerp, Dept Chem, Lab Adsorpt & Catalysis LADCA, Univ Pl 1, B-2610 Antwerp, Belgium.; Meynen, V (corresponding author), Flemish Inst Technol Res, Sustainable Mat Management VITO NV, Boeretang 200, B-2400 Mol, Belgium. vera.meynen@uantwerpen.be |
Keywords: | organodiphosphonate esters;partial hydrolysis;hybrid TiO2 nanoparticles;linker-nanoparticle binding;NMR spectroscopy | Document URI: | http://hdl.handle.net/1942/41580 | ISSN: | 1439-4235 | e-ISSN: | 1439-7641 | DOI: | 10.1002/cphc.202300437 | ISI #: | 001071673900001 | Rights: | 2023 Wiley-VCH GmbH | Category: | A1 | Type: | Journal Contribution |
Appears in Collections: | Research publications |
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Partial Hydrolysis of Diphosphonate Ester During the Formation of Hybrid TiO2 Nanoparticles_ Role of Acid Concentration.pdf Restricted Access | Published version | 1.9 MB | Adobe PDF | View/Open Request a copy |
auteursversie.pdf | Peer-reviewed author version | 2.64 MB | Adobe PDF | View/Open |
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