Synthetic resins or natural rubbers -- part of the class 520 ser – Synthetic resins – From silicon reactant having at least one...
Patent
1997-08-25
1999-05-18
Marquis, Melvyn I.
Synthetic resins or natural rubbers -- part of the class 520 ser
Synthetic resins
From silicon reactant having at least one...
528 15, 528 17, 528 18, 528 19, 528 21, 528 28, 528 38, C08G77/08
Patent
active
059051302
DESCRIPTION:
BRIEF SUMMARY
TECHNICAL FIELD
The present invention relates to a process for the production of a polysilazane which is a high molecular weight polymer serving as a precursor for a heat-resistant ceramic and which has Si--N linkages in the main chain thereof.
BACKGROUND ART
Polysilazanes which provide easiness in molding works can easily give ceramic molded articles having various shapes when used as a raw material for molding.
Since a dense, high purity silicon oxide film (amorphous SiO.sub.2) is obtainable when an organic solvent solution of a polysilazane is used as a coating liquid and is calcined in air for reaction with water and oxygen, the polysilazane with such characteristics is practically used as a high purity silica coating material
Various methods are conventionally known for the synthesis of polysilazanes. For example, the following methods are known: such as SiCl.sub.4 or SiH.sub.2 Cl.sub.2 is reacted with an amine (Japanese Published Unexamined Patent Applications No. Sho-60-226890, No. Sho-62-290730 and No. Sho-63-309526 and Japanese Examined Patent Publications No. Hei-2-15577 and No. Hei-6-62775, etc.); alkali metal hydride catalyst such as KH having dehydrogenation activity (J. of Faint Technology Vol. 42, No. 543, April 1970, Japanese Published Unexamined Patent Applications No. Sho-60-226890, No. Sho-62-290730 and Sho-63-309526 and Japanese Examined Patent Publications No. Hei-2-15577 and No. Hei-6-62775, etc.); and compound with an amine compound using a transition metal complex catalyst such as Ru.sub.3 (CO).sub.12 (organometallics 1986, 5, 2081-2086, etc.).
With method (1) above, however, an ammonium salt of hydrogen halide acid is produced as a by-product in a larger amount than the polysilazane, so that a large amount of the polymer is lost during the removal of the by-product. With method (2) above, it is necessary to take great care of the handling of the metal hydride catalyst which is dangerous, so that the method is ill-suited for a large scale synthesis. With method (3) above, it is very difficult to separate, after the reaction, the synthesized polymer from the transition metal complex catalyst such as Ru.sub.3 (CO).sub.12 which is very expensive and which is a homogeneous catalyst.
To avoid the use of a catalyst which generates a large amount of a by-product, which is dangerous or which is expensive, the following methods have been proposed in which an aminosilane is reacted with ammonia: with ammonia using an acid catalyst such as CF.sub.3 SO.sub.3 H (Japanese Published Unexamined Patent Application No. Sho-62-225534 and Japanese Examined Patent Publication No. Hei-4-60492); and with a large amount of ammonia or an amine (Japanese Examined Patent Publication No. Hei-5-60488).
In the above method (4), however, since the ammonia as well as the amine liberated as a result of the amine inter-exchange are basic, the acid catalyst used reacts with the basic substances, so that the effect of the acid is diminished, resulting in a considerable reduction of the yield of the polymer. With the above method (5) using a large, excess amount of ammonia or an amine, a greater part of the ammonia and amine is discharged from the reaction system without being utilized for the synthesis, so that the method is disadvantageous from the standpoint of costs.
DISCLOSURE OF THE INVENTION
It is an object of the present invention to provide a process for the production of a polysilazane with reduced costs and a high yield in a stable manner.
The present inventors have made an intensive study with a view toward solving the above problem and, as a result, have completed the present invention.
Namely, in accordance with the present invention there is provided a process for the production of a polysilazane having Si--N linkages in the main chain thereof, characterized in that a polyaminosilane compound having at least two amino groups bonded to a silicon atom thereof is subjected to an amine inter-exchange reaction with a polyhydrogenated nitrogen-containing compound having at least two hydrogen atoms bonde
REFERENCES:
patent: 4725660 (1988-02-01), Serita et al.
patent: 5612410 (1997-03-01), Kondo et al.
Funayama Osamu
Isoda Takeshi
Nakahara Hirohiko
Marquis Melvyn I.
Tonen Corporation
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