High purity silane and silicone production

C - Chemistry – Metallurgy – 01 – B

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23/196, 23/327

C01B 33/04 (2006.01) C01B 33/02 (2006.01)

Patent

CA 1151395

ABSTRACT A mini-plant for producing silane from dichlorosilane via a redistribution reaction has produced 97% pure SiH4 at 93% efficiency The residual impurities were monochlorosilane (2.5%) and dichlorosilane (.5%). The silane purity of 97% achieved by operating the silane still partial condenser at 40 psig and -32°C outlet temperature was significantly higher than predicted by ideal vapor-liquid equilibrium considerations. Laboratory equilibrium concentrations and order of magnitude reaction rates were confirmed in mini-plant operations. Kinetic isotope studies on the mechanism of the amine catalyzed redistribution of chloro- silanes indicated the amine hydrochloride may not be the active species as originally proposed. The hydrogenation of silicon tetrachloride to trichlorosilane appears to be a true equilibrium, approachable from either HSiCl3 or SiC14. Virtually no H2SiC12 was formed by hydrogenation of HSiCl3.

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