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Slurry Phase Reaction of Elemental Silicon with Methanol in the Presence of Copper: Direct Synthesis of Trimethoxysilane

  • Han, Joon-Soo (Organosilicon Chemistry Laboratory, Korea Institute of Science and Technology) ;
  • Cho, Joo-Hyun (Organosilicon Chemistry Laboratory, Korea Institute of Science and Technology,Organosilicon Chemistry Laboratory, Korea Institute of Science and Technology) ;
  • Lee, Myong-Euy (Department of Chemistry, Graduate School, Yonsei University) ;
  • Yoo, Bok-Ryul (Department of Chemistry, Graduate School, Yonsei University)
  • Published : 2009.03.20

Abstract

Slurry phase reaction of elemental silicon with methanol has been studied in the presence of copper using a small amount of cuprous chloride as an activator in DBT (dibenzyltoluene) at various temperatures from 200 ${^{\circ}C}$ to 320 ${^{\circ}C}$. Trimethoxysilane (1a) with a Si-H unit was obtained as the major product and tetramethoxysilane (1b) as the minor product. The reaction worked well using a 0.5 wt % CuCl as an activator. The optimum temperature for this direct synthesis of 1a was 240 ${^{\circ}C}$. Methoxysilanes were obtained in 95% yield with 81% selectivity to 1a from 85% conversion of elemental silicon.

Keywords

References

  1. Marciniec, B. Comprehensive Handbook on Hydrosilylation Pergamon Press: Oxford, 1992
  2. Speier, J. L.; Webster, J. A.; Barnes, G. H. J. Am. Chem. Soc. 1957, 79, 974 https://doi.org/10.1021/ja01561a054
  3. Speier, J. L. Homogeneous Catalysis of Hydrosilation by Transition Metals in Advances Organometallic Chemistry; Stone, F. G. A., West, R., Eds.; Academic Press: 1979; Vol. 17, p 407
  4. Benkeser, R. A. Kang, J. J. Organomet. Chem. 1980, 185, C9 https://doi.org/10.1016/S0022-328X(00)94412-7
  5. Combes, C. Compt. Rendus Acad. Sci. 1896, 122, 531
  6. Ruff, O.; Albert, K. Chem. Ber. 1905, 38, 2222 https://doi.org/10.1002/cber.190503802179
  7. Oye, H. A.; Rong, H. M.; Nygaard, L.; Schussler, G.; Tuset, J. K. Silicon for the Chemical Industry IV; Geiranger, Ed.; Norwegian University of Science and Technology: Norway, 1998
  8. Lee, S.-I.; Kim, D.-B.; Sin, J.-H.; Lee, Y.-S.; Nah, C. J. Ind. Eng. Chem. 2007, 13, 786 https://doi.org/10.1021/ie50141a018
  9. Hong, C. K.; Hwang, I.; Kim, N.; Park, D. H.; Hwang, B. S.; Nah, C. J. Ind. Eng. Chem. 2008, 14, 71 https://doi.org/10.1016/j.jiec.2007.07.002
  10. Kim, D.; Lee, H. G.; Jung, H.; Kang, S. H. Bull. Korean Chem. Soc. 2007, 26, 241
  11. Crivello, J. V.; Bi, D. J. Polym. Sci., Part A 1993, 31, 3121 https://doi.org/10.1002/pola.1993.080311228
  12. Peng, Z.-y.; Lan, Z.-l.; Yin, D.-l. Jingxi Shiyou Huagong 2006, 23, 54.
  13. Peng, Z.-y.; Lan, Z.-l.; Yin, D.-l. Chem. Abstr. 2004, 142, 76503. https://doi.org/10.1016/0021-9517(90)90312-8
  14. Suzuki, E.; Kamata, T.; Ono, Y. J. Catalysis 1990, 125, 390 https://doi.org/10.1016/0021-9517(90)90312-8
  15. Suzuki, E.; Ono, Y. Shokubai 1989, 31(2), 104 https://doi.org/10.1016/j.jallcom.2006.04.046
  16. Suzuki, E.; Ono, Y. Chem. Abstr.1989, 111, 115314. https://doi.org/10.5012/bkcs.2007.28.10.1661
  17. Mattern, N.; Seyrich, R.; Wilde, L.; Baehtz, C.; Knapp, M.; Acker, J. J. Alloys Compd. 2007, 429, 211 https://doi.org/10.1016/0022-328X(96)06129-3
  18. Lim, W. C.; Cho, J. H.; Han, J. S.; Yoo, B. R. Bull. Korean Chem. Soc. 2007, 28(10), 1661 https://doi.org/10.1021/om9605342
  19. Yeon, S. H.; Han, J. S.; Yoo, B. R.; Jung, I. N. J. Organomet. Chem. 1996, 516, 91 https://doi.org/10.1016/S0065-3055(03)50003-X
  20. Han, J. S.; Yeon, S. H.; Yoo, B. R.; Jung, I. N. Organometallics 1997, 16, 93 https://doi.org/10.1021/om9605342
  21. Yoo, B. R.; Jung, I. N. Adv. Organomet. Chem. 2004, 50, 145 https://doi.org/10.1016/S0065-3055(03)50003-X

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