Use of metal salts in the synthesis of oligomeric hydrogensilses

Details Use of metal salts in the synthesis of oligomeric hydrogensilses Use of metal salts in the synthesis of oligomeric hydrogensilses

1991-03-12

1992-04-21

Shaver, Paul F.

Chemistry of inorganic compounds

Silicon or compound thereof

Oxygen containing

C01B 3300, C01B 3304

Patent

active

051066041

ABSTRACT:
Hydridospherosiloxanes and soluble hydrogensilsesquioxane resin are produced having the formula (HSiO.sub.3/2).sub.n, where n is an even integer greater than 8. A biphasic reaction medium is prepared, having a first solvent phase and a second solvent phase. The first solvent phase can contain a hydrocarbon solvent, such as an alcohol. The first solvent phase can be methanol or ethanol. The second solvent phase is a concentrated solution of a metal salt, such as Fe(III) in a polar organic solvent and water. A silicon compound represented by the formula: HSiX.sub.3, where X is a group which is hydrolyzable in the solvent of said first solvent phase, is added to the biphasic reaction medium. X can be Cl or OCH.sub.3. The first solvent phase is separated from the second solvent phase and then the separated first solvent phase is treated with a metal salt, such as sodium or potassium carbonate. Slow evaporation of the first solvent phase solvent is employed to isolate a mixture of crystals of (HSiO.sub.3/2).sub.8, and (HSiO.sub.3/2).sub.10. The crystal mixture is washed with a hydrocarbon solvent and crystals of (HSiO.sub.3/2).sub.8 are isolated.

REFERENCES:
patent: 3615272 (1971-10-01), Collins et al.
patent: 4808653 (1989-02-01), Haluska et al.
patent: 4895914 (1990-01-01), Saitoh et al.

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