Process for preparation of cellulose acetate

Claim 2

A process for preparing cellulose acetate, which comprises (A) forming a reaction mixture of activated cellulose, acetic anhydride in an amount of from 1.5 to 6 times the amount of said cellulose and an effective catalytic amount of an acidic catalyst in an amount less than 1/20 of the amount of said cellulose, at about ambient temperature or up to 50° C., elevating the temperature of said reaction mixture to 50° to 85° C. over a period of 20 to 60 minutes at a substantially uniform temperature elevating rate and then maintaining said reaction mixture at said temperature of 50° to 85° C. for from 3 to 20 minutes, and (B) then neutralizing said acidic catalyst in the reaction mixture containing primary cellulose acetate obtained in step (A) and hydrolyzing the reaction mixture at a temperature of from 110° to 120° C. in a bath in which water is incorporated.

Claim 3

A process for preparing cellulose acetate according to claim 1, wherein the activated cellulose is obtained by adding to a starting cellulose material, an acid material selected from the group consisting of acetic acid or a mixture of acetic acid and sulfuric acid, in an amount not more than about 1/4 of the weight of the starting cellulose material and treating the starting cellulose material with said acid material for 20 to 60 minutes.

Claim 4

A process for preparing cellulose acetate which consists essentially of: mixing α-cellulose starting material with a first acid material selected from the group consisting of glacial acetic acid and a mixture of glacial acetic acid and sulfuric acid, the amount of said first acid material being not more than about 25% by weight, based on the weight of said α-cellulose starting material, and maintaining said mixture at an elevated temperature for from 20 to 60 minutes to transform said α-cellulose to an activated cellulose; then adding to said mixture a second acid material selected from the group consisting of a mixture of acetic anhydride and glacial acetic acid and a mixture of acetic anhydride, glacial acetic acid and sulfuric acid, to form an acetylation reaction mixture containing from 200 to 400% by weight of acetic anhydride, based on the weight of said activated cellulose, and containing an effective catalytic amount of sulfuric acid but less than about 5% by weight, based on the weight of said activated cellulose, and cooling said acetylation reaction mixture so as to permit the temperature of said acetylation reaction mixture to rise, due to the exothermic heat of reaction, at a uniform rate of temperature increase, from about room temperature or below up to a final reaction temperature of from 50° to 85° C. over a period of from 20 to 60 minutes and then maintaining the acetylation reaction mixture at said final reaction temperature for from 3 to 20 minutes to complete the acetylation reaction; then adding a neutralizing agent to completely neutralize said sulfuric acid in the acetylation reaction mixture, then placing the acetylation reaction mixture in a closed vessel and blowing steam thereinto to raise the temperature of the contents of said vessel to an ripening reaction temperature of from 110° to 120° C. and maintaining said contents of said vessel at said ripening reaction temperature for from 2 to 10 hours to effect hydrolysis; and then treating said contents to recover said cellulose acetate.

Claim 5

A process for preparing cellulose acetate which consists essentially of: mixing α-cellulose starting material with a first acid material selected from the group consisting of glacial acetic acid and a mixture of glacial acetic acid and sulfuric acid, the amount of said first acid material being not more than about 25% by weight, based on the weight of said α-cellulose starting material, and maintaining said mixture at an elevated temperature for from 20 to 60 minutes to transform said α-cellulose to an activated cellulose; then adding to said mixture a second acid material selected from the group consisting of a mixture of acetic anhydride and glacial acetic acid and a mixture of acetic anhydride, glacial acetic acid and sulfuric acid, to form an acetylation reaction mixture containing from 200 to 400% by weight of acetic anhydride, based on the weight of said activated cellulose, and containing an effective catalytic amount of sulfuric acid but less than about 5% by weight, based on the weight of said activated cellulose, and cooling said acetylation reaction mixture so as to permit the temperature of said acetylation reaction mixture to rise, due to the exothermic heat of reaction, at a uniform rate of temperature increase, from about room temperature or below up to a final reaction temperature of from 50° to 85° C. over a period of from 20 to 60 minutes and then maintaining the acetylation reaction mixture at said final reaction temperature for from 3 to 20 minutes to complete the acetylation reaction; then adding a neutralizing agent to completely neutralize said sulfuric acid in the acetylation reaction mixture, then placing the acetylation reaction mixture in a closed vessel and blowing steam thereinto to raise the temperature of the contents of said vessel to an ripening reaction temperature of from 110° to 120° C. and maintaining said contents of said vessel at said ripening reaction temperature for from 2 to 10 hours to effect hydrolysis; and then treating said contents to recover said cellulose acetate.