Blog

Access to fluorochemicals directly from fluorspar | Communications Chemistry

Thank you for visiting nature.com. You are using a browser version with limited support for CSS. To obtain the best experience, we recommend you use a more up to date browser (or turn off compatibility mode in Internet Explorer). In the meantime, to ensure continued support, we are displaying the site without styles and JavaScript.

Communications Chemistry volume  6, Article number: 178 (2023 ) Cite this article sodium fluoride for sale

Fluorochemicals have a wide range of applications in industry, but accessing these relies on the energy intensive conversion of acid-grade fluorspar (CaF2) to toxic hydrogen fluoride (HF) gas, which is in turn used for the downstream production of fluorochemicals via multistep processes. Now, directly treating acid-grade fluorspar with dipotassium hydrogen phosphate (K2HPO4) under mechanochemical conditions affords a fluorinating reagent for direct S–F and C(sp3/sp2)–F bond construction, bypassing the need for HF production.

Simple inorganic fluoride salts are often insoluble in the solvents that dissolve their reaction partners. While bio-inspired urea organocatalysts have been developed to make potassium fluoride (KF) and cesium fluoride (CsF) soluble through hydrogen bonding, enabling enantioselective fluorinations with these alkali-metal fluorides1, using calcium difluoride (fluorspar; CaF2) as a fluorinating reagent remains very challenging owing to its high insolubility. So far, only limited fluorochemicals such as LiPF6, PF5, POF3 and Ca(SO3F)2 are produced using inorganic CaF2, and under extremely harsh conditions2,3,4.

Now, a team led by Véronique Gouverneur from Oxford University in the UK shows that potassium phosphate salts can be used to activate CaF2 in the solid-state by mechanochemistry, providing direct access to fluorinated products while bypassing the need for toxic HF production (https://doi.org/10.1126/science.adi1557)5. “The vision in my laboratory is to rejuvenate fluorine chemistry with global challenges in mind. The technology we have invented is a first step in this direction and sets the stage to create a new circular fluorochemicals economy”, says Gouverneur.

Mechanochemistry is able to initiate reactions independently of solubility, and aid solid-state diffusion kinetics. Here, the team took inspiration from calcium phosphate (bio)mineralization, such as in the formation of bones and teeth, with a view to using the formation of a calcium phosphate by-product as a driving force for fluorination. Pleasingly, treating industry standard acid-grade fluorspar with K2HPO4 was found to be an effective protocol for CaF2 activation. The resultant powdered product, Fluoromix, was found to be suitable for forging S−F and C(sp3/sp2)–F bonds in solution, generating over 50 fluorochemicals in high yield (Fig. 1).

Mechanochemical generation of Fluoromix from acid-grade fluorspar, and application to produce various fluorochemicals. Adapted with permission from Science https://www.science.org/doi/10.1126/science.adi1557. Copyright (2023) AAAS.

“One of the biggest challenges was deciphering the underlying processes in the mechanochemical activation of CaF2”, comments first author Calum Patel. “We initially hypothesized that the species formed could be potassium fluoride (KF) and a calcium phosphate by-product (or derivative thereof), but this was more complex than anticipated.” Powder X-ray diffraction was used to monitor the consumption of CaF2 by the potassium phosphate salt, and the reaction between KF and K2HPO4 was key to determining the composition of Fluoromix. Indeed, the product of this reaction, K3HPO4F, was observed in Fluoromix, and when ball milled with calcium hydrogen phosphate (CaHPO4), a new product (K2-xCay(PO3F)a(PO4)b) formed, which was also found to be present in Fluoromix. “Prof. Michael Hayward was instrumental in determining the structures of these new salts, both of which possess fluorinating abilities”, says Patel.

“We hope that this technology will enable us to access a wider fluorochemical space, specifically critically needed and non-persistent fluorochemicals. Ultimately, we hope this work will inspire scientists across the globe to provide disruptive solutions to chemical challenges.” concludes Patel.

Pupo, G. et al. Asymmetric nucleophilic fluorination under hydrogen bonding phase-transfer catalysis. Science 360, 638–642 (2018).

Article  CAS  PubMed  Google Scholar 

Tarbutton, G., Egan, E. P. Jr. & Frary, S. G. Phosphorus-halogen compounds from phosphorus pentoxide and halides. Properties of phosphorus trifluoride and phosphorus oxyfluoride. J. Am. Chem. Soc. 63, 1782–1789 (1941).

Jordan, R. K. “Carbonyl fluorination process,” US Patent US4087475 (1975).

Liu, J. et al. Synthesis of LiPF6 Using CaF2 as the fluorinating agent directly: an advanced industrial production process fully harmonious to the environments. Ind. Eng. Chem. Res. 58, 20491–20494 (2019).

Patel, C. et al. Fluorochemicals from fluorspar via a phosphate-enabled mechanochemical process that bypasses HF. Science 381, 302–306 (2023).

Article  CAS  PubMed  Google Scholar 

Communications Chemistry https://www.nature.com/commschem

You can also search for this author in PubMed  Google Scholar

Publisher’s note Springer Nature remains neutral with regard to jurisdictional claims in published maps and institutional affiliations.

Open Access This article is licensed under a Creative Commons Attribution 4.0 International License, which permits use, sharing, adaptation, distribution and reproduction in any medium or format, as long as you give appropriate credit to the original author(s) and the source, provide a link to the Creative Commons license, and indicate if changes were made. The images or other third party material in this article are included in the article’s Creative Commons license, unless indicated otherwise in a credit line to the material. If material is not included in the article’s Creative Commons license and your intended use is not permitted by statutory regulation or exceeds the permitted use, you will need to obtain permission directly from the copyright holder. To view a copy of this license, visit http://creativecommons.org/licenses/by/4.0/.

Guo, H. Access to fluorochemicals directly from fluorspar. Commun Chem 6, 178 (2023). https://doi.org/10.1038/s42004-023-00987-2

DOI: https://doi.org/10.1038/s42004-023-00987-2

Anyone you share the following link with will be able to read this content:

Sorry, a shareable link is not currently available for this article.

Provided by the Springer Nature SharedIt content-sharing initiative

Communications Chemistry (Commun Chem) ISSN 2399-3669 (online)

neon used in semiconductor industry Sign up for the Nature Briefing newsletter — what matters in science, free to your inbox daily.