Skip to main content
Log in

One-Step Synthesis of Thermoplastic Phenylsilsesquioxane Polymer and Its Copolymers with Diphenylsiloxanes

  • Published:
Journal of Inorganic and Organometallic Polymers Aims and scope Submit manuscript

Abstract

The preparation of reversibly softening polymers and copolymers of phenylsilsesquioxane in a one-step synthesis has been studied. The synthetic methods are based on hydrolytic polycondensation of PhSiCl3 or copolycondensation of PhSiCl3 with Ph2SiCl2 using moistened or hydrated salts: (1) moistened Na2CO3, K2CO3, (2) Na2B4O7·10H2O, (3) Na3PO4·12H2O. Syntheses (1) and (2) gave products as reversibly softening and soluble materials, whereas synthesis (3) produced partially cross-linked resins from which a soluble material might be extracted. Polycondensation using borax gave polymers and copolymers with incorporated boron atoms. The polysilsesquioxanes were characterized by size exclusion chromatography (SEC), 1H and 29Si NMR, IR spectroscopy, and elemental analysis. Thermal properties were studied by DSC and thermogravimetry.

This is a preview of subscription content, log in via an institution to check access.

Access this article

Price excludes VAT (USA)
Tax calculation will be finalised during checkout.

Instant access to the full article PDF.

Similar content being viewed by others

REFERENCES

  1. N. A. Senatova and V. T. Nikolenkov, Dokl. Akad. Nauk 335(1), 689 (1994).

    Google Scholar 

  2. M. Morita, S. Imamura, A. Tanaka, and T. Tamamura, J. Electrochem. Soc. 131, 2402 (1984).

    Google Scholar 

  3. A. Oikawa, S. Fukuyama, Y. Toneda, H. Harada, and T. Takada, J. Electrochem. Soc. 137(10), 3223 (1990).

    Google Scholar 

  4. N. Yoichi and M. Fumio, Japanese Patent 05 55,201 (1993).

  5. U. Shunichrio, European Patent 312 280 (1990).

  6. S. Jassuo, Japanese Patents 07 126,389 (1995); 06 287.303 (1994).

  7. E. Imai and H. Takeno, Japanese Patent 59 129,939 (1984).

  8. M. Yanagisawa, Japanese Patent 62 89.228 (1987).

  9. H. Ban, A. Tanaka, and Y. Kawai, Polymer 31, 564 (1990).

    Google Scholar 

  10. S. Hayashida and S. Imamura, J. Polym. Sci. Part A 33, 55 (1995).

    Google Scholar 

  11. A. Yashimura, S. Imamura, and T. Izowa, Japanese Patent 04 12.333 (1992).

  12. A. Tomaru and S. Hayashida, Japanese Patent 06 109.936 (1994).

  13. H. Makoto and M. Hiroo, Japanese Patent 03 91.704 (1991).

  14. M. Shintaro, A. Etsushi, and A. Hiroshi, Jpn. J. Appl. Phys. Part 2 35(101), L1257 (1996).

    Google Scholar 

  15. Y. Yuka and A. Masaya, Japanese Patent 07 258.604 (1995).

  16. I. I. Therdokhlebova, I. I. Mamaeva, and S. S. A. Pavlova, Vysokomol. Soed. Ser. A 26(9), 1971 (1984).

    Google Scholar 

  17. G. Li, M. Ye, and L. Shi, Chin. J. Polym. Sci. 12(4), 331 (1994); 14(1), 41 (1996).

    Google Scholar 

  18. P. V. Ivanov, Vysokomol. Soed. Ser. A 37(3), 417 (1995).

    Google Scholar 

  19. V. M. Kopylov, L. M. Khananashvili, O. V. Shokol'nik, and P. V. Ivanov, Vysokomol. Soed. Ser. A 37(3), 394 (1995).

    Google Scholar 

  20. R. H. Baney, M. Itoh, A. Sakakibara, and T. Suzuki, Chem. Rev. 95, 1409 (1995).

    Google Scholar 

  21. W. Noll, Chemistry and Technology of Silicone (Academic Press, New York/London, 1968), p. 196.

    Google Scholar 

  22. W. Radziewicz and H. Bentkowska, Roczniki Chem. 36, 285 (1962).

    Google Scholar 

  23. J. Dul, Ph.D. thesis (Technical University of Lodz, Lodz, Poland, 1977).

  24. J. Dul, E. Leśniak, and Z. Lasocki, Polimery 39, 519 (1994).

    Google Scholar 

  25. J. J. Duane, U.S. Patent 2646441 (1949); J. J. Duane, British Patent 683.182 (1952).

    Google Scholar 

  26. J. F. Brown, Jr., J. H. Vogt, Jr., A. Katchman, J. W. Eustance, M. M. Kiser, and K. W. Kranz, J. Am. Chem. Soc. 82, 6194 (1960).

    Google Scholar 

  27. J. F. Brown, Jr., J. Polym. Sci. Part C 1, 83 (1963).

    Google Scholar 

  28. J. F. Brown, Jr. and P. I. Prescott, J. Am. Chem. Soc. 86, 1402 (1964); 86, 1120 (1964).

    Google Scholar 

  29. V. N. Tsvetkov, K. A. Andrianov, N. N. Makarova, M. G. Vitovskaya, E. I. Ryumtsev, and I. N. Shtennikova, Eur. Polym. J. 9, 27 (1973).

    Google Scholar 

  30. K. A. Andrianov, A. A. Zhdanov, and V. Yu. Levin, Annu. Rev. Mater. Sci. 8, 313 (1978).

    Google Scholar 

  31. X. Zhang, S. Chen, and L. Shi, Chinese J. Polym. Sci. 5(2), 162 (1987).

    Google Scholar 

  32. U. N. Emelyanov and Yu. M. Permitina, Xth International Symposium on Organosilicon Chemistry, Poznań, Poland, Aug. 15–20 (1993), Abstract P-33.

  33. K. A. Andrianov, I. M. Barer, M. A. Golubienko, and L. M. Khananashvili, Zh. Obsch. Khim. 43(8), 1754 (1973).

    Google Scholar 

  34. K. A. Andrianov, M. B. Fromberg, and E. N. Arsenova, Zh. Prikl. Khim. 43(8), 2053 (1970).

    Google Scholar 

  35. D. D. Perin and W. L. F. Armarego, Purification of Laboratory Chemicals, 3rd ed. (Pergamon Press, London, 1988), (a) p. 290, (b) p. 164, (c) p. 296, (d) p. 155, (e) p. 194.

    Google Scholar 

  36. A. D. Irwin, J. S. Holmgren, T. W. Zerda, and J. Janas, J. Non-Cryst. Solids 89, 194 (1987).

    Google Scholar 

  37. B. Babrański, Analiza ilościowa zwiazków organicznych (PWN, Warszawa, 1979), p. 142.

    Google Scholar 

  38. E. Leśniak, Z. Michalska, and J. Dul, Polish Patent Application P-324996 (1998).

  39. E. Leśniak, Z. Michalska, and J. Chojnowski, Polish Patent Application P-324956 (1998).

  40. L. A. Mutrofanov, A. V. Karlin, K. D. Suglova, L. Ya. Rushen'tseva, and K. B. Piotrovskij, Zh. Prikl. Khim. 42(5), 1175 (1969).

    Google Scholar 

  41. V. V. Vilyukov, V. V. Kireev, and M. A. Erian, Vysokomol. Soed. Ser. A. 37(4), 576 (1995).

    Google Scholar 

  42. J. Galecki, Preparatyka nieorganiczna (WNT, Warszawa, 1964), p. 701.

    Google Scholar 

  43. L. Vale, J. Chem. Soc. 2253 (1960).

  44. R. Murugavel, A. Voigt, M. G. Walawalkar, and H. W. Roesky, Chem. Rev. 96, 2215 (1996).

    Google Scholar 

  45. V. V. Korshak, V. A. Zamyatina, and N. I. Biekasova, Boroorganitcheskie polimiery (Nauka, Moscow, 1975), pp. 190–192.

    Google Scholar 

  46. V. N. Gruber, A. L. Klebanski, N. V. Kozlova, E. V. Kuz'mina, and G. A. Kruglova, Vysokomol. Soed. T (A) 14, 1638 (1972).

    Google Scholar 

  47. H. Marsmann, in NMR 17 Basic Principles and Progress (Springer-Verlag, New York, 1981), pp. 174–199.

    Google Scholar 

  48. M. Smaihi, T. Jermoumi, and J. Marignan, Chem. Mater. 7, 2293 (1995).

    Google Scholar 

  49. M. K. Lee and D. J. Meier, Polymer 34(23), 4882 (1993).

    Google Scholar 

  50. W. A. Finzel, J. Coat. Technol. 64(809), 47 (1992).

    Google Scholar 

Download references

Author information

Authors and Affiliations

Authors

Rights and permissions

Reprints and permissions

About this article

Cite this article

Leśniak, E., Michalska, Z.M. & Chojnowski, J. One-Step Synthesis of Thermoplastic Phenylsilsesquioxane Polymer and Its Copolymers with Diphenylsiloxanes. Journal of Inorganic and Organometallic Polymers 8, 1–21 (1998). https://doi.org/10.1023/A:1021617902162

Download citation

  • Issue Date:

  • DOI: https://doi.org/10.1023/A:1021617902162

Navigation