Synthetic resins or natural rubbers -- part of the class 520 ser – Synthetic resins – From silicon reactant having at least one...
Patent
1993-05-18
1995-05-16
Marquis, Melvyn I.
Synthetic resins or natural rubbers -- part of the class 520 ser
Synthetic resins
From silicon reactant having at least one...
528 38, 528 43, 20415774, C08G 7700
Patent
active
054161827
DESCRIPTION:
BRIEF SUMMARY
TECHNICAL FIELD
This invention relates to a method for producing silicon network polymers.
BACKGROUND ART
Silicone network polymers are attracting attention as optoelectronic materials, ceramic precursors and so on.
Heretofore, a linear polysilane containing Si--Si linkages in the backbone chain has been synthesized from a dichlorosilane as the starting compound by heating the starting compound together with sodium metal at a temperature not below 100.degree. C. A silicon network polymer, however, cannot be synthesized by subjecting a trichlorosilane as such to the same conditions as above. Thus, in order to synthesize a silicon network polymer, it is necessary to modify not only the starting compound but also the reaction conditions. Therefore, a synthetic method employing a sonication technique in combination with a very strong reducing system, e.g. a sodium metal-potassium alloy system (J. Am. Chem. Soc. 110 (1988) 234) and a method using an alkali metal, e.g. sodium metal, and an appropriate auxiliary agent such as 12-crown-4 (Macromolecules 1990, 23, 3423-3426) have been proposed. However, these methods are disadvantageous in that they do not provide for molecular weight control and that the use of alkali in a large amount presents a major safety problem in commercial production runs. Thus, neither of the methods can be utilized for production on a commercial scale.
As a technology for synthesizing linear polysilanes, several processes involving electrode reactions which permit molecular weight control and are safe have been reported (J. Chem. Soc. Chem. Commun., 1990, 1160, Electrochem. Acta, 35, 1867 (1990), Denki Kagaku Oyobi Kogyo Butsuri Kagaku 59, 5, 421 (1991), JP Kokai H-3-104893, etc.). However, none of the above-cited literature consider production of a silicon network polymer and, for that matter, none provide information on how such a silicon network polymer could ever be obtained.
Therefore, the development of an electrode reaction technology for producing silicone network polymers has been awaited.
DISCLOSURE OF INVENTION
In view of the above state of the art, the inventor of this invention did much research and discovered that the serious drawbacks of the known synthetic methods employing an alkali metal are substantially eliminated or alleviated when a trihalosilane is subjected to electrode reaction employing a defined metal as a positive electrode with the polarity of two electrodes switched at predetermined intervals.
It was also found that when the reaction vessel or the reaction mixture is exposed to ultrasonic waves in conducting the electrode reaction, the reaction time is drastically decreased, the molecular weight of the reaction product increased and the production yield also increased in a remarkable degree.
The present invention therefore provides the following methods for producing silicon network polymers.
1. A method for producing a silicon network polymer characterized by subjecting a trihalosilane of general formula halogen) to an electrode reaction using a perchloric acid salt as the supporting electrolyte, an aprotic solvent as the reaction solvent, an Mg, Cu or Al electrode as one electrode and an electrode made of an electronically conductive material, which may be the same as or different from said one electrode as the counter electrode, with the polarity of said electrodes being switched from time to time to thereby provide a silicon network polymer of general formula compound; n is equal to 10 to 10000).
2. A method for producing a silicon network polymer characterized by subjecting a trihalosilane of general formula halogen) to electrode reaction using a perchloric acid salt as the supporting electrolyte, an aprotic solvent as the reaction solvent, Mg, Cu or Al as one electrode material and an electronically conductive material which is either the same as or different from said one electrode material as the counter electrode material with the polarity of the electrodes being switched from time to time under application of ultrasonic waves to thereby prov
Kashimura Shigenori
Kawasaki Shinichi
Nishida Ryoichi
Shono Tatsuya
Marquis Melvyn I.
Osaka Gas Company Ltd.
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