A simple and novel synthetic route to prepare anatase TiO2 nanopowders from natural ilmenite via the H3PO4/NH3 process

Lalinda Palliyaguru; Ushan S. Kulathunga; Lakruwani I. Jayarathna; Champa D. Jayaweera; Pradeep M. Jayaweera

doi:10.1007/s12613-020-2030-3

Volume 27 Issue 6

Jun. 2020

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Article Navigation > International Journal of Minerals, Metallurgy and Materials > 2020 > 27(6): 846-855

Lalinda Palliyaguru, Ushan S. Kulathunga, Lakruwani I. Jayarathna, Champa D. Jayaweera, and Pradeep M. Jayaweera, A simple and novel synthetic route to prepare anatase TiO₂ nanopowders from natural ilmenite via the H₃PO₄/NH₃ process, Int. J. Miner. Metall. Mater., 27(2020), No. 6, pp. 846-855. https://doi.org/10.1007/s12613-020-2030-3

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Lalinda Palliyaguru, Ushan S. Kulathunga, Lakruwani I. Jayarathna, Champa D. Jayaweera, and Pradeep M. Jayaweera, A simple and novel synthetic route to prepare anatase TiO2 nanopowders from natural ilmenite via the H3PO4/NH3 process, Int. J. Miner. Metall. Mater., 27(2020), No. 6, pp. 846-855. https://doi.org/10.1007/s12613-020-2030-3

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Research Article

A simple and novel synthetic route to prepare anatase TiO₂ nanopowders from natural ilmenite via the H₃PO₄/NH₃ process

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Corresponding author:
Pradeep M. Jayaweera E-mail: pradeep@sjp.ac.lk
Received: 3 October 2019; Revised: 24 February 2020; Accepted: 25 February 2020; Available online: 26 February 2020

Abstract

Abstract

A simple and novel technique for the preparation of anatase TiO₂ nanopowders using natural ilmenite (FeTiO₃) as the starting material is reported. Digesting ilmenite with concentrated H₃PO₄ under refluxing conditions yields a white α-titanium bismonohydrogen orthophosphate monohydrate (TOP), Ti(HPO₄)₂·H₂O, which can be easily isolated via gravity separation from unreacted ilmenite. The addition of ammonia to the separated TOP followed by calcination at 500°C completes the preparation of anatase TiO₂. Calcination at temperatures above 800°C converts the anatase form of TiO₂ to the stable rutile phase. The removal of iron from ilmenite during the commercial production of synthetic TiO₂ is problematic and environmentally unfriendly. In the present study, the removal of iron was found to be markedly simple due to the high solubility of iron phosphate species in concentrated H₃PO₄ with the precipitation of TOP. The titanium content of the prepared samples on metal basis with silica and phosphorous as major impurities was over 90%. Prepared TiO₂ samples were characterized using X-ray fluorescence, Fourier-transform infrared spectroscopy, Raman spectroscopy, ultraviolet–visible diffuse reflectance spectroscopy, high-resolution transmission electron microscopy, and X-ray diffraction analyses. The photocatalytic potentials of the commercial and as-prepared TiO₂ samples were assessed by the photodegradation of rhodamine B dye.
- ilmenite;
- phosphoric acid;
- titanium phosphates;
- titanium dioxide;
- anatase;
- rutile

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