in neat (no solvent) chlorination of crude Si at 300-310 °C; best yield of SiCl4;;
参考文献
Gattermann, L.; Ellery, E.
Ber., 1899 , vol. 32, p. 1114 - 1116
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Gattermann, L.; Weinlig, K.
Ber., 1894 , vol. 27, p. 1943 - 1948
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Gmelin Handbook: Si: MVol.B, 242, page 657 - 659
in gas Kinetics; metals were vaporized in a high temperature beam and the vapor were collimated upon entering a separatly pumped chamber filled with halogen; chemiluminescence spectroscopy;
参考文献
Journal of Chemical Physics, , vol. 91, # 5 p. 2834 - 2839
in diethylene glycol dimethyl ether byproducts: H2; further intermediate: KSiH3; under N2, dispersion of potassium reacts with SiH4 at 100°C, concd. in vacuo at 30°C, C4F9SO3SiH3 added at -60°C, stored at this temp. for 10 min, warmed to 40°C; volatiles removed over 3 h in vacuo, SiH4 removed; GC;
in diethylene glycol dimethyl ether byproducts: H2; further intermediate: NaSiH3; under N2, dispersion of sodium reacts with SiH4 at 100°C, concd. in vacuo at 30°C, C4F9SO3SiH3 added at -60°C, stored at this temp. for 10 min, warmed to 40°C; volatiles removed over 3 h in vacuo, SiH4 removed; GC;
in diethylene glycol dimethyl ether byproducts: H2; further intermediate: KSiH3; under N2, dispersion of potassium reacts with SiH4 at 100°C, soln. of PhSO3H added dropwise at -40°C; volatiles removed at room temp. in vacuo, SiH4 removed; GC;
in diethylene glycol dimethyl ether byproducts: H2; further intermediate: NaSiH3; under N2, dispersion of sodium reacts with SiH4 at 100°C, soln. of PhSO3H added dropwise at -40°C; volatiles removed at room temp. in vacuo, SiH4 removed; GC;
in neat (no solvent) distillation of ICl to crystalline Si near red heat;; fractional distillation over Cu filings;;
参考文献
Besson, A.
Comptes Rendus Hebdomadaires des Seances de l'Academie des Sciences, 1891 , vol. 112, p. 1314 - 1316
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Gmelin Handbook: Si: MVol.B, 275, page 742 - 743
