The titanium(I) salt of N,N-(diphosphonomethyl)glycine: synthesis, characterisation, porosity and proton conduction

(Note: The full text of this document is currently only available in the PDF Version )

Enrique Jaimez, Gary B. Hix and Robert C. T. Slade


Abstract

A new diphosphonic acid,N,N -(diphosphonomethyl)glycine, has been prepared. The titanium(iv) salt [Ti(dpmg)] of this acid has been characterised by X-ray powder diffraction, thermogravimetry, 31P MAS NMR spectroscopy, isothermal N2 adsorption–desorption and ac conductivity measurements. Phosphorus is present in a mixture of bonded phosphonate and free phosphonic acid groups. The material is both amorphous and porous (BET specific surface area=119 m2 g-1), and its water content is relative humidity (RH)-dependent. Ti(dpmg) is a protonic conductor (at 90% RH and 90 °C, σ=3×10-2 S cm-1), with conductivity exhibiting Arrhenius-type behaviour at constant RH. Conductivity and Arrhenius parameters are strongly dependent on the water content.


References

  1. S. Drumel, P. Janvier, P. Barboux, M. Bujoli-Doeuff and B. Bujoli, Inorg. Chem., 1995, 34, 148 CrossRef CAS.
  2. D. M. Poojary, Z. Baolong and A. Clearfield, Angew. Chem., 1994, 106, 2422.
  3. S. Bruque, M. A. Aranda, E. R. Losilla, P. Olivera-Pastor and P. Maireles-Torres, Inorg. Chem., 1995, 34, 893 CrossRef CAS.
  4. A. Clearfield and G. D. Smith, Inorg. Chem., 1969, 8, 431 CrossRef CAS.
  5. M. B. Dines, P. Di Giacomo, K. P. Callahan, P. C. Griffith, R. Lane and R. E. Cooksey, in Chemically Modified Surfaces in Catalysis and Electrocatalysis, ed. J. S. Miller, ACS Symp. Ser. 192, American Chemical Society, Washington, DC, 1982 Search PubMed.
  6. G. Alberti, U. Costantino, S. Allulli and N. Tomassini, J. Inorg. Nucl. Chem., 1978, 40, 1113 CrossRef CAS.
  7. K. J. Scott, Y. Zhang, R.-C. Wang and A. Clearfield, Chem. Mater., 1995, 7, 1095 CrossRef CAS.
  8. E. Jaimez, A. Bortun, G. Hix, J. R. García, J. Rodríguez and R. C. T. Slade, J. Chem. Soc., Dalton Trans., 1996, 2285 RSC.
  9. G. L. Rosenthal and J. Caruso, Inorg. Chem., 1992, 31, 3104 CrossRef CAS.
  10. L. Maya and P. O. Danis, J. Chromatogr., 1980, 190, 145 CrossRef CAS.
  11. A. Bortun, A. Clearfield, L. Bortun, E. Jaimez, M. A. Villa-García, J. R. García and J. Rodríguez, J. Mater. Chem., submitted Search PubMed.
  12. G. Cao, M. E. García, M. Alcalá, L. F. Burgess and T. E. Mallouk, J. Am. Chem. Soc., 1992, 114, 7574 CrossRef CAS.
  13. M. Ogawa and K. Kurada, Chem. Rev., 1995, 95, 399 CrossRef CAS.
  14. A. Clearfield, in Surface Organometallic Chemistry: Molecular Approaches to Surface Catalysis, ed. J. M. Basset, Kluwer Academic Publishers: Norwell MA, 1988; pp. 271–298 Search PubMed.
  15. M. Casciola, U. Costantino, A. Peraio and T. Rega, Solid State Ionics, 1995, 77, 229 CrossRef CAS.
  16. D. A. Burwell and M. E. Thompson, Chem. Mater., 1991, 3, 91.
  17. D. A. Burwell and M. E. Thompson, Chem. Mater., 1991, 3, 730 CrossRef CAS.
  18. C. Bhardwaj, H. Hu and A. Clearfield, Inorg. Chem., 1993, 32, 4294 CrossRef.
  19. C. Y. Ortiz-Avila, C. Bhardwaj and A. Clearfield, Inorg. Chem., 1994, 33, 2499 CrossRef CAS.
  20. K. D. Kreuer, Chem. Mater., 1996, 8, 610 CrossRef CAS.
  21. G. Alberti, M. Casciola, U. Costantino, A. Peraio and R. Vivani, Solid State Ionics, 1991, 46, 53 CrossRef CAS.
  22. G. Alberti, M. Casciola, U. Costantino, A. Peraio and E. Monterini, Solid State Ionics, 1992, 50, 315 CrossRef CAS.
  23. A. Bortun, E. Jaimez, R. Llavona, J. R. García and J. Rodríguez, Mater. Res. Bull., 1995, 30, 413 CrossRef CAS.
  24. B. A. Boukamp, Solid State Ionics, 1986, 20, 31 CrossRef CAS.
  25. B. Bujoli, P. Palvadeau and M. Queignec, Eur. J. Solid State Inorg. Chem., 1992, 29, 141 CAS.
  26. K. Segawa, S. Nakata and S. Asaoka, Mater. Chem. Phys., 1987, 17, 181 CrossRef CAS.
  27. S. Brunauer, L. S. Deming, W. S. Deming and E. Teller, J. Am. Chem. Soc., 1940, 62, 1723 CrossRef CAS.
  28. M. A. Villa-García, E. Jaimez, A. Bortun, J. R. García and J. Rodríguez, J. Porous Mater., 1995, 2, 293 Search PubMed.
  29. S. J. Gregg and K. S. W. Sing, Adsorption Surface Area and Porosity, Academic Press, London, 1982 Search PubMed.
  30. K. S. W. Sing, D. H. Everett, R. A. W. Haul, L. Moscou, R. A. Pierotti, J. Rouquerol and T. Simieniewska, Pure Appl. Chem., 1985, 57, 603 CrossRef CAS.
  31. G. Alberti and M. Casciola, in Proton Conductors: Solids, membranes and gels—materials and devices, ed. Ph. Colomban, Cambridge University Press, Cambridge, 1992, p. 238 Search PubMed.
  32. R. C. T. Slade and J. A. Knowles, Solid State Ionics, 1991, 46, 45 CrossRef CAS.
  33. R. C. T. Slade, H. Jinku and J. A. Knowles, Solid State Ionics, 1992, 50, 287 CrossRef.
Click here to see how this site uses Cookies. View our privacy policy here.