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Synthesis and structural characterisation of solid titanium(iv) phosphate materials by means of X-ray absorption and NMR spectroscopy
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Rusanova-Naydenova, Daniela, Trublet, Mylène, Klysubun, Wantana, Cholsuk, Chanakan, Iuga, Dinu, Dupree, Ray, Antzutkin, Oleg N. and Persson, Ingmar (2022) Synthesis and structural characterisation of solid titanium(iv) phosphate materials by means of X-ray absorption and NMR spectroscopy. Dalton Transactions, 51 (21). pp. 8192-8207. doi:10.1039/d2dt00902a ISSN 1477-9226.
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WRAP-synthesis-structural-characterisation-solid-titanium(iv)-phosphate-materials-means-X-ray-absorption-NMR-spectroscopy-Dupree-2022.pdf - Published Version - Requires a PDF viewer. Available under License Creative Commons Attribution. Download (2302Kb) | Preview |
Official URL: http://dx.doi.org/10.1039/d2dt00902a
Abstract
Solid titanium phosphate, TiP, materials hold great promise for wastewater treatment for removal of metal ions and complexes. A series of TiP materials, synthesised at mild conditions and short reaction times, have been structurally characterised using solid-state X-ray absorption spectroscopy, phosphorus and titanium K edge XANES and EXAFS, and 31P and 47/49Ti NMR spectroscopy. The titanium K edge EXAFS data of α-Ti(HPO4)2·H2O (α-TiP) revealed octahedral coordination of oxygens around titanium. Repeated washing of primary β-/γ-TiP with hydrochloric acid results in formation of a weakly ordered solid, TiO(OH)(H2PO4)·H2O, TiP1-H. The structure of TiP1-H is shown by Ti EXAFS to be a titanyl compound, containing a short Ti[double bond, length as m-dash]O bond. The analogous data for linked titanium phosphate compounds (LTP) disclosed that inter-linkage occurs between α-TiP and titanyl phosphate units, supported by 31P–31P NOESY NMR data. 47/49Ti NMR and Ti pre-edge XANES show evidence of two different titanium environments in LTP, one very similar to that observed in TiP1-H and a second more symmetric octahedral environment. Data are discussed in terms of induced acidic hydrolyses of titanium(IV) and phosphate counterpart during washings with hydrochloric acid and water. A straightforward relation between synthesis parameters/post synthetic treatment and structural re-arrangement in the materials is established.
Item Type: | Journal Article | |||||||||||||||
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Subjects: | Q Science > QD Chemistry T Technology > TP Chemical technology |
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Divisions: | Faculty of Science, Engineering and Medicine > Science > Physics | |||||||||||||||
Library of Congress Subject Headings (LCSH): | Titanium, Phosphates, Chemical engineering, Nuclear magnetic resonance spectroscopy, Chemistry, Inorganic | |||||||||||||||
Journal or Publication Title: | Dalton Transactions | |||||||||||||||
Publisher: | Royal Society of Chemistry | |||||||||||||||
ISSN: | 1477-9226 | |||||||||||||||
Official Date: | 9 May 2022 | |||||||||||||||
Dates: |
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Volume: | 51 | |||||||||||||||
Number: | 21 | |||||||||||||||
Page Range: | pp. 8192-8207 | |||||||||||||||
DOI: | 10.1039/d2dt00902a | |||||||||||||||
Status: | Peer Reviewed | |||||||||||||||
Publication Status: | Published | |||||||||||||||
Access rights to Published version: | Open Access (Creative Commons) | |||||||||||||||
Date of first compliant deposit: | 8 June 2022 | |||||||||||||||
Date of first compliant Open Access: | 9 June 2022 | |||||||||||||||
RIOXX Funder/Project Grant: |
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