US 12,227,622 B2
Centrifugal process for the continuous manufacture of novel, uncrosslinked polysilazanes
Lucas Marin, Central Point, OR (US); Alexander Lukacs, III, Ashland, OR (US); and Michael Leimas, Central Point, OR (US)
Filed by Lucas Marin, Central Point, OR (US); Alexander Lukacs, III, Ashland, OR (US); and Michael Leimas, Central Point, OR (US)
Filed on Aug. 13, 2024, as Appl. No. 18/803,125.
Application 18/803,125 is a continuation of application No. 18/387,800, filed on Nov. 7, 2023.
Claims priority of provisional application 63/432,075, filed on Dec. 13, 2022.
Prior Publication US 2024/0400766 A1, Dec. 5, 2024
Int. Cl. C08G 77/62 (2006.01); B01D 17/02 (2006.01); C01B 21/087 (2006.01)
CPC C08G 77/62 (2013.01) [B01D 17/0217 (2013.01); C01B 21/087 (2013.01)] 3 Claims
 
1. A silazane or polysilazane prepared by a process comprising the steps of:
(a) contacting a flowing stream of halosilane with a flowing stream of anhydrous, liquid ammonia in the chamber of an operating centrifugal device, where said centrifugal device is capable of inertially separating a product stream of aminosilane and silazane ammonolysis intermediates of slightly different densities and polarities from a stream of anhydrous, liquid ammonia-ammonium halide by-product, using a centrifugal force of sufficient magnitude to effect such separation;
(b) allowing a dwell time in the centrifugal device sufficient to fully provide for the reaction of the halosilane reactant with the anhydrous, liquid ammonia to form polar, aminosilanes and silazanes that are soluble in the anhydrous liquid ammonia;
(c) further allowing a sufficient dwell time in the centrifugal device to allow for the separation of these aminosilane and silazane intermediates from the anhydrous, liquid ammonia-ammonium halide by-product in a separate liquid phase;
(d) further allowing a sufficient dwell time in the centrifugal device to provide for at least a partial condensation of the aminosilane and silazane intermediates to a degree of polymerization where the resulting, oligomeric or polymeric silazanes are less polar and more dense than the ammonium halide-anhydrous liquid ammonia by-product solution and remain separated from the by-product ammonium halide-anhydrous, liquid ammonia solution at ambient temperatures and pressures, and;
(e) subsequently collecting the separate phases of (i) oligomeric silazane and polymeric silazane product, and (ii) the by-product solution of ammonium halide in anhydrous, liquid ammonia that exit the centrifugal device through separate exit ports.