Porous spherical cellulose acetate particles

Claim 2

Porous, spherical particles of cellulose acetate, which consist essentially of cellulose acetate having an acetylation degree of 49 to 60%, a degree of esterification of from 2.0 to 2.8, a particle diameter of 0.05 to 10 mm, a sphericity of 0.8 or larger, a pore volume of 0.65 cc/g or larger and a collapsing strength of 9 kg or higher.

Claim 3

Porous, spherical particles as claimed in claim 1, the surface of which has been saponified.

Claim 4

A process for producing porous spherical cellulose acetate particles, which comprises feeding a dope comprising a solution formed by dissolving a cellulose acetate of a degree of esterification of 2.0 to 2.8 in an acetic acid/water (80/20 to 90/10, by weight) solvent so that the concentration of the cellulose acetate may be 25±7 wt. %; feeding said dope through a supply pipe to a coagulation bath comprising an acetic acid/water (30/70 to 42/58, by weight) solvent and having a temperature of 40°±5° C.; operating an agitator having a rotor passing near a discharge port on the end of said supply pipe; effecting precipitation and granulation while adding water so that the acetic acid to water ratio of the coagulation bath may be maintained at a substantially constant value during said operation; centrifugally separating precipitated particles from the solution; washing these particles with water of 40° to 90° C.; and drying the particles.

Claim 5

A process for producing porous spherical cellulose acetate particles, which comprises feeding a dope comprising a solution formed by dissolving a cellulose acetate of a degree of esterification of 2.0 to 2.8 in an acetic acid/water (80/20 to 90/10, by weight) solvent so that the concentration of the cellulose acetate may be 25±7 wt. %; feeding said dope through a supply pipe to a coagulation bath comprising an acetic acid/water (30/70 to 42/58, by weight) solvent and having a temperature of 40°±5° C.; operating an agitator having a rotor passing near a discharge port on the end of said supply pipe; effecting precipitation and granulation while adding water so that the acetic acid to water ratio of the coagulation bath may be maintained at a substantially constant value during said operation; centrifugally separating precipitated particles from the solution; washing these particles with water of 40° to 90° C.; and drying the particles.

Claim 6

A process for producing porous spherical cellulose acetate particles, which comprises: providing a dope comprising a solution formed by dissolving (1) cellulose acetate having a degree of esterification of from 2.0 to 2.8, in (2) a solvent comprising a first mixture of acetic acid and water in which the weight ratio of acetic acid/water is from 80/20 to 90/10, said dope containing from 18 to 32 wt. % of said cellulose acetate; providing a coagulation bath comprising a second mixture of acetic acid and water in which the weight ratio of acetic acid/water is in the range of from 30/70 to 42/58; feeding a stream of said dope through a supply pipe into said coagulation bath having a temperature of 35° to 45° C., simultaneously operating an agitator having a rotor that passes near the discharge end of said supply pipe to break up said stream into droplets, said droplets precipitating in the form of spherical cellulose acetate particles in said coagulation bath, and adding water to said coagulation bath to maintain the weight ratio of acetic acid/water in said coagulation bath in said range of from 30/70 to 42/58 while said dope is being fed into said coagulation bath; then separating said precipitated spherical particles from said coagulation bath; washing said particles with water having a temperature of 40° to 90° C.; and then drying said particles.

Claim 7

A process for producing porous spherical cellulose acetate particles, which comprises: providing a dope comprising a solution formed by dissolving (1) cellulose acetate having a degree of esterification of from 2.0 to 2.8, in (2) a solvent comprising a first mixture of acetic acid and water in which the weight ratio of acetic acid/water is from 80/20 to 90/10, said dope containing from 18 to 32 wt. % of said cellulose acetate; providing a coagulation bath comprising a second mixture of acetic acid and water in which the weight ratio of acetic acid/water is in the range of from 30/70 to 42/58; feeding a stream of said dope through a supply pipe into said coagulation bath having a temperature of 35° to 45° C., simultaneously operating an agitator having a rotor that passes near the discharge end of said supply pipe to break up said stream into droplets, said droplets precipitating in the form of spherical cellulose acetate particles in said coagulation bath, and adding water to said coagulation bath to maintain the weight ratio of acetic acid/water in said coagulation bath in said range of from 30/70 to 42/58 while said dope is being fed into said coagulation bath; then separating said precipitated spherical particles from said coagulation bath; washing said particles with water having a temperature of 40° to 90° C.; and then drying said particles.

Claim 8

A process as claimed in claim 4 in which said dope contains about 25 wt. % of said cellulose acetate.

Claim 9

A process as claimed in claim 4 in which said stream of dope is extruded through a nozzle in the form of a rod-like continuous body into said coagulation bath so as to begin coagulating therein and said rotor comprises blade means for cutting said rod-like continuous body into fine pieces which form into spherical particles as they continue precipitating in said coagulation bath.

Claim 10

A process as claimed in claim 4 including the additional step of saponifying the surfaces of said particles after the step of drying said particles.

Claim 11

A process as claimed in claim 4 in which, after the step of drying said particles, said particles are immersed in an aqueous solution of sodium hydroxide having a concentration of 0.2 to 2 wt. %, for 1 to 6 minutes, wherein the ratio of said aqueous solution to said particles is between 3 and 10, whereby to saponify the surfaces of said particles, and then recovering the saponified particles.

Claim 12

Saponifield porous spherical particles having a cellulose acetate core and a cellulose shell, said particles having been prepared by the process of claim 8 and having an acetylation degree of 48 to 59%, a particle diameter of 0.05 to 10 mm, a sphericity of 0.7 or larger, a pore volume of 0.4 cc/g or larger and a collapsing strength of 10 kg or higher.

Claim 13

A process as claimed in claim 4 in which said dope is an aged dope prepared by acetylating cellulose to form cellulose triacetate and then saponifying and aging said cellulose triacetate with a mixture of acetic acid and water until there is obtained a dope containing cellulose acetate having a degree of esterification of 2.0 to 2.8, said aged dope containing 1.5 wt. % or less of an inorganic salt.

Claim 14

Porous spherical cellulose acetate particles prepared by the process of claim 4 and having an acetylation degree of 49 to 60%, a degree of esterification of from 2.0 to 2.8, a particle diameter of 0.05 to 10 mm, a sphericity of 0.8 or larger, a pore volume of 0.65 cc/g or larger and a collapsing strength of 9 kg or higher.