Method for preparing powdery crystalline cellulose

• US 5,175,275 A
• Filed: 11/15/1991
• Issued: 12/29/1992
• Est. Priority Date: 05/28/1987
• Status: Expired due to Term

• Current Assignee: Deutsche Bank Trust Company Americas (Deutsche Bank)
• Original Assignee: Tosco Corporation (ConocoPhillips)
• Inventors: Dobashi, Shozaburo, Uchida, Hisaichiro, Ohara, Keiso
• Primary Examiner(s): Nutter, Nathan M.
• Application Number:
  US07/793,001
• Time in Patent Office: 410 Days
• Field of Search: 536/56, 536/124, 127/29, 127/34, 514/781, 435/99, 435/277
• US Class Current: 536/56
• CPC Class Codes: C08B 15/08 Fractionation of cellulose, e.g. separation of cellulose crystallites
• CPC Class Codes: C08J 2301/02 Cellulose; Modified cellulose
• CPC Class Codes: C08J 3/12 Powdering or granulating
• CPC Class Codes: C08J 3/122 Pulverisation by spraying
• CPC Class Codes: C12P 19/14 produced by the action of a carbohydrase (EC 3.2.x), e.g. by alpha-amylase , e.g. by cellulase, hemicellulase

Abstract

The present invention relates to powdery crystalline cellulose having an average particle size ranging from 3 to 30 μm and an average degree of polymerization ranging from 400 to 1,500. The powdery crystalline cellulose can be prepared according to a method comprising treating a starting cellulose material with a cellulase, subjecting the enzyme-treated cellulose material to acid hydrolysis under mild conditions, and then mechanically pulverizing the hydrolyzed cellulose material. The powdery crystalline cellulose is suitable for various applications of foods, cosmetics, medicines and various industrial products.

Claims

1. A method for preparing powdery crystalline cellulose having an average particle size ranging from 3 to 30 μ

m and an average degree of polymerization ranging from 400 to 1,500, comprising the steps of;

treating a starting cellulose material with a cellulase;

subjecting the cellulase-treated cellulose material to acid hydrolysis under mild conditions to yield a hydrolyzed cellulose material; and

mechanically pulverizing the hydrolyzed cellulose material to yield the powdery crystalline cellulose.

2. The method of claim 1, wherein the cellulase has a concentration ranging from 20 to 60 U/g.

3. The method of claim 1, wherein the cellulase is used in the form of an aqueous solution.

4. The method of claim 1, wherein the cellulase-treatment is performed at a pH value ranging from 5.0 to 6.5 and at a temperature ranging from 30°

C. to 50°

C. for 2 to 3 hours.

5. The method of claim 1, wherein the cellulase-treatment is carried out in the presence of a surfactant, a pH stabilizing agent, or both.

6. The method of claim 1, wherein the acid hydrolysis is performed at a mineral acid concentration ranging from 0.1 to 8.0N and a temperature ranging from 40°

C. to 125°

C. for 5 minutes to 9 hours.

7. The method of claim 6, wherein the mineral acid is hydrochloric acid and the acid hydrolysis is carried out at an acid concentration ranging from 0.1 to 2.5N and a temperature ranging from 60°

C. to 125°

C. for 5 to 120 minutes.

8. The method of claim 6, wherein the mineral acid is sulfuric acid and the acid hydrolysis is carried out at an acid concentration ranging from 0.2 to 8.0N and a temperature ranging from 40°

C. to 120°

C. for 30 minutes to 9 hours.

9. The method of claim 1, wherein the pulverization is conducted for 1 to 10 hours.

10. The method of claim 1, wherein the pulverization is conducted for 2 to 7 hours.

11. The method of claim 1, wherein the powdery crystalline cellulose is further sieved to control the particle size of the powdery crystalline cellulose.

12. The method of claim 11, wherein the size of the sieve ranges from 42 to 200 mesh.

13. A method for preparing powdery crystalline cellulose having an average particle size ranging from 3 to 30 μ

m and an average degree of polymerization ranging from 400 to 1,500, comprising the steps of;

treating a starting cellulose material with a cellulase at a pH value ranging from 5.0 to 6.5 and at a temperature ranging from 30°

C. to 50°

C. for 2 to 3 hours;

subjecting the cellulase-treated cellulose material to acid hydrolysis at a mineral acid concentration ranging from 0.1 to 8.0N and a temperature ranging from 40°

C. to 125°

C. for 5 minutes to 9 hours to yield a hydrolyzed cellulose material; and

mechanically pulverizing the hydrolyzed cellulose material to yield the powdery crystalline cellulose.