Preparation of fibrous collagen product having hemostatic and wound sealing properties

Claim 1

The method of preparing a mass of finely-divided fibrils and fibers having hemostatic properties and when placed on a wound combines with blood to form a mass that is self-adherent to the wound surfaces and seals the wound which comprises the steps of (a) placing water-wet collagen in an ethanol-water mixture, the amount of ethanol being sufficient to constitute from 90% to 50% by weight of the mixture including the water in the water-wet collagen, (b) agitating the mixture for a period sufficient to equalize the ethanol content of the collagen to that of the liquid, (c) separating the excess liquid fo the collagen, (d) placing the recovered collagen in an ethanol-ionizable acid mixture, the amount of acid being sufficient to form a partial salt of collagen containing from about 50% to 90% of the theoretical stoichiometric bound acid content, (e) agitating the mixture for from about 3 to about 20 hours to equalize the ethanol content of the collagen to that of the liquid and to effect the reaction of the collagen with the acid to form a partial salt of collagen, (f) separating the excess liquid from the partial salt, (g) subjecting the recovered partial salt to treatment with ethanol and separating the partial salt from the liquid a sufficient number of cycles until the water content of the partial salt has been reduced to 1%, (h) vacuum drying the recovered partial salt to a volatiles content of about 1%, (i) conditioning the dried partial salt to a volatiles content of about 8% to 15%, and (j) subjecting the conditioned partial salt to a fiberizing and deaggregation or fluffing operation to form a mass of finely-divded fibrils and fibers, the mass of fibrils and fibers consisting of fibrils and fibers at least about 5% by weight of which have an effective length of not more than 1 mm. and not more than about 10% by weight of which have an effective length above 12 mm., the mass of fibrils and fibers having a surface area of at least 1 square meter per gram, having a bulk density of not more tha 8 pounds per cubic foot and exhibiting a HAT test of not more than 1500 when wet with blood.

Claim 2

The method of preparing a mass of finely-divided fibrils and fibers having hemostatic properties and when placed on a wound combines with blood to form a mass that is self-adherent to the wound surfaces and seals the wound which comprises the steps of (a) placing water-wet collagen in an ethanol-water mixture, the amount of ethanol being sufficient to constitute from 90% to 50% by weight of the mixture including the water in the water-wet collagen, (b) agitating the mixture for a period sufficient to equalize the ethanol content of the collagen to that of the liquid, (c) separating the excess liquid fo the collagen, (d) placing the recovered collagen in an ethanol-ionizable acid mixture, the amount of acid being sufficient to form a partial salt of collagen containing from about 50% to 90% of the theoretical stoichiometric bound acid content, (e) agitating the mixture for from about 3 to about 20 hours to equalize the ethanol content of the collagen to that of the liquid and to effect the reaction of the collagen with the acid to form a partial salt of collagen, (f) separating the excess liquid from the partial salt, (g) subjecting the recovered partial salt to treatment with ethanol and separating the partial salt from the liquid a sufficient number of cycles until the water content of the partial salt has been reduced to 1%, (h) vacuum drying the recovered partial salt to a volatiles content of about 1%, (i) conditioning the dried partial salt to a volatiles content of about 8% to 15%, and (j) subjecting the conditioned partial salt to a fiberizing and deaggregation or fluffing operation to form a mass of finely-divded fibrils and fibers, the mass of fibrils and fibers consisting of fibrils and fibers at least about 5% by weight of which have an effective length of not more than 1 mm. and not more than about 10% by weight of which have an effective length above 12 mm., the mass of fibrils and fibers having a surface area of at least 1 square meter per gram, having a bulk density of not more tha 8 pounds per cubic foot and exhibiting a HAT test of not more than 1500 when wet with blood.