Solvent‐Free Synthesis of Nano Zirconium Phenylphosphonates with Molten Phenylphosphonic Acid. Issue 28 (28th April 2020)

• Record Type: Journal Article
• Authors: Contreras‐Ramirez, Aida; Tomlin, Bryan E.; Day, Gregory S.; Clearfield, Abraham; Zhou, Hong‐Cai
• Is Part Of: Chemistry. Volume 26:Issue 28(2020)
• Page Start: 6185
• Page End: 6194
• Publication Date: 2020-04-28
• Subjects: anion exchange -- nanoplates -- phosphates -- topotactic -- zirconium; Chemistry -- Periodicals; 540
• DOI: 10.1002/chem.201905110
• Languages: English
• ISSNs: 0947-6539

Abstract

Abstract: Nanosized α‐zirconium phenylphosphonate particles were successfully prepared by the reaction between different zirconium sources and molten phenylphosphonic acid in the absence of solvent. The resultant nanoplates exhibit particle sizes in the range of 15 to 30 nm. The use of a topotactic anion exchange method starting from α‐zirconium phosphate instead resulted in the generation of 15 to 180 nm plates, while also resulting in nanoparticles with a higher degree of crystallinity. The topotactic anion exchange of the phosphate groups by phenylphosphonate groups could be performed to completion when performed in molten phenylphosphonic acid. Characterization of both the final products as well as the individual steps in the anion exchange were performed by powder XRD, fast neutron activation analysis, TGA, FTIR spectroscopy, TEM, solid‐state NMR and XPS. Abstract : Nanoplates : The synthesis of zirconium phenylphosphonate is performed using different Zr sources and molten phenylphosphonic acid in the absence of solvent. Using zirconium salts, resulted in the formation of nanoparticles that are 15–30 nm in size. Instead, by using a topotactic synthetic procedure starting from αZrP, 15–180 nm particles with higher crystallinity were obtained (see figure).