Direct precipitation method for producing extrusion-grade cellulose acetate powder and resulting product
AssigneeEastman Kodak Company
InventorsChung-Ming Kuo, Richard T. Bogan
Life of this patent
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Abstract
Improved method for preparing cellulose acetate powder, particularly extrusion-grade powder, by direct precipitation, with the precipitation step occurring at a temperature of about 65.degree. C. to about 95.degree. C. and with the coagulating agent subsequently being removed from the resulting liquid powder slurry also at a temperature of about 65.degree. C. to about 95.degree. C.; and the cellulose acetate powder product resulting from the improved method, the powder being particularly adapted to take up plasticizer up to about 50 percent by weight and still flow uniformly without caking or becoming tacky.
Claims16
Method for preparing cellulose acetate powder from an acid dope containing from about 6% to about 15% by weight cellulose acetate ester, the acid dope comprising about 60 to about 100 percent aqueous acetic acid solution and a cellulose acetate ester dissolved in the solution and having an acetyl content of about 38 to about 41 weight percent;
- the method comprising:
- (a) mixing in the dope about 0.25 to about 5.0 parts per part of cellulose acetate ester of a water immiscible coagulating agent having a boiling point less than 150.degree. C. (302.degree. F.) to form a mixture;
- (b) precipitating from the mixture the cellulose acetate ester in about 25% to about 35% aqueous acid at a temperature of about 65.degree. C. (149.degree. F.) to about 95.degree. C. (203.degree. F.) by adding at a rate slow enough to prevent localized precipitation about 5% to about 12% aqueous acetic acid solution that is preheated to the same temperature as the acid dope while vigorously agitating the mixture sufficiently to keep large coagulate particles apart into smaller coagulate particles of a size that will pass through a 45 mesh screen so as to form a liquid powder slurry;
- (c) aging the liquid powder slurry for about 15 minutes in about 25% to about 35% aqueous acetic acid;
- (d) removing the coagulating agent from the liquid powder slurry down to about 1% or less by weight of the liquid powder slurry and at a temperature of about 65.degree. C. to about 95.degree. C.;
- (e) removing liquid from the liquid powder slurry remaining after step (d) to obtain a wet powder of coagulate particles;
- (f) washing the wet powder with water to remove the residual acetic acid;
- and drying the powder at a temperature of about 65.degree. C. to about 95.degree. C. to remove the water.
An improved cellulose acetate powder having an intrinsic viscosity in accordance with ASTM D-871 testing method of about 0.75 to about 2.0 and an acetyl range of about 38 to about 41 weight percent and comprising coagulate particles that will pass through about a 45 mesh screen and have free-flowing characteristics suitable for use in an extruder, each of said coagulate particles having exterior and interior surfaces that are substantially porous and essentially free of fused surfaces, said cellulose acetate powder having a tapped bulk density of about 17 to about 26 pounds per cubic foot and being capable of taking up plasticizer up to about 50% by weight of the coagulate particles without said coagulate particles becoming tacky and caking.
Dependencies are inferred from the claim text.