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Research article - Peer-reviewed, 2022

Synthesis and structural characterisation of solid titanium(IV) phosphate materials by means of X-ray absorption and NMR spectroscopy

Rusanova-Naydenova, Daniela; Trublet, Mylene; Klysubun, Wantana; Cholsuk, Chanakan; Iuga, Dinu; Dupree, Ray; Antzutkin, Oleg N.; Persson, Ingmar


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 P-31 and Ti-47/49 NMR spectroscopy. The titanium K edge EXAFS data of alpha-Ti(HPO4)(2)center dot H2O (alpha-TiP) revealed octahedral coordination of oxygens around titanium. Repeated washing of primary beta-/gamma-TiP with hydrochloric acid results in formation of a weakly ordered solid, TiO(OH)(H2PO4)center dot H2O, TiP1-H. The structure of TiP1-H is shown by Ti EXAFS to be a titanyl compound, containing a short Ti=O bond. The analogous data for linked titanium phosphate compounds (LTP) disclosed that inter-linkage occurs between alpha-TiP and titanyl phosphate units, supported by P-31-P-31 NOESY NMR data. Ti-47/49 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.

Published in

Dalton Transactions
2022, volume: 51, number: 21, pages: 8192-8207

Authors' information

Rusanova-Naydenova, Daniela
SunCarbon AB
Trublet, Mylene
Klysubun, Wantana
Synchrotron Light Res Inst
Cholsuk, Chanakan
Synchrotron Light Res Inst
Iuga, Dinu
University of Warwick
Dupree, Ray
University of Warwick
Antzutkin, Oleg N.
University of Warwick
Antzutkin, Oleg N.
Lulea University of Technology
Swedish University of Agricultural Sciences, Department of Molecular Sciences

Sustainable Development Goals

SDG6 Clean water

UKÄ Subject classification

Inorganic Chemistry

Publication Identifiers


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