IP Library › Granted Patent US 6,984,731
Granted Patent B2
US 6,984,731 · App. 10/439,809 · Granted Jan 10, 2006

Process for manufacturing cellulose acetate

Assignee: Nihon Zaikei Kabushiki Kaisha
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Quick Facts
Patent No.
US 6,984,731
App. No.
10/439,809
Granted
Jan 10, 2006
Kind
B2
Abstract

The invention provides a process for manufacturing at low cost cellulose acetate, which is useful as a biodegradable plastic, using corncob meal which has hitherto been thrown away as a raw material. More specifically, the invention provides a process for manufacturing cellulose acetate, which comprises the steps of: steaming corncob meal at a temperature of 150 to 250° C. and a pressure of 20 to 29 MPa; filtering the steamed corncob meal to obtain a solid product; and dehydrating and acetylating by adding acetic anhydride and sulfuric acid to the solid product. The steaming is preferably carried out by using a pressure vessel and the filtering is preferably carried out by using a filtering device.

Claims (32)

1. A process for manufacturing cellulose acetate, comprising the steps of:

steaming a corncob meal in a sub-critical state at a temperature of 150 to 250° C. and a pressure of 20 to 29 MPa for 10 to 30 minutes to obtain a mixture of a solid product and a solution product, said solid product comprised of cellulose, said solution product comprised of soluble hemicelluloses and polyphenol converted from lignin separated from lignocelluloses in the corncob, said sub-critical state being such that the solid product and the solution product are obtained from the corncob meal solely due to the temperature and pressure conditions of the state;

filtering the mixture to separate the solid product;

dehydrating the solid product; and

acetylating the dehydrated solid product in the presence of acetic anhydride and sulfuric acid to obtain cellulose acetate from the solid product.

2. The process according to claim 1 , wherein the steaming is carried out in a pressure vessel and the filtering is carried out by a filtering device.

3. The process according to claim 1 , wherein the steaming is carried out at a temperature of 180 to 200° C. and a pressure of 25 to 28 MPa.

4. The process according to claim 1 , wherein, in the steaming step, 10 to 1000 parts by weight of water is added relative to 100 parts by weight of corncob meal.

5. The process according to claim 1 , wherein, in the steaming step, a sulfurous acid compound is added to the corncob meal.

6. The process according to claim 5 , wherein the sulfurous acid compound is added in the amount of 1 to 10 parts by weight for 100 parts by weight of the corncob meal.

7. The process according to claim 5 , wherein, in the dehydrating and acetylating step, the sulfuric acid is added in the amount of 1 to 10 parts by weight, and the acetic anhydride is added in the amount of 1 to 20 parts by weight, relative to 100 parts by weight of dry cellulose.

8. The process according to claim 1 , wherein the dehydrating and acetylating is carried out under conditions of a pressure of 5 to 15 MPa, a temperature of 60 to 100° C., a stirring speed of 30 to 100 rpm and a treatment time of 15 to 30 hours.

9. A process for manufacturing cellulose acetate, comprising the steps of:

steaming a corncob meal at a temperature of 150 to 250° C. and a pressure of 20 to 29 MPa;

filtering the mixture to separate the solid product;

dehydrating the solid product; and

acetylating the dehydrated solid product in the presence of acetic anhydride and sulfuric acid at a temperature of 60 to 100° C. and a pressure of 5 to 15 MPa for 15 to 30 hours as a single process to obtain cellulose acetate from the solid product.

10. A process for manufacturing xyloligosaccharides, comprising:

steaming a corncob meal under conditions of a temperature of 150 to 250° C. and a pressure of 20 to 29 MPa;

filtering the steamed corncob meal to obtain a filtrate from which solid has been removed;

performing an enzyme treatment by reacting xylanase with soluble xylan in the filtrate to hydrolyze the soluble xylan;

removing any suspended matter from a reaction product obtained during the enzyme treatment; and

drying the reaction product.

11. The process according to claim 10 , wherein the steaming is carried out in a pressure vessel and the filtering is carried out by a filtering device.

12. The process according to claim 10 , wherein the steaming is carried out under conditions of a temperature of 180 to 200° C. and a pressure of 25 to 28 MPa.

13. The process according to claim 10 , wherein, in the steaming, 10 to 1000 parts by weight of water is added relative to 100 parts by weight of corncob meal.

14. The process according to claim 10 , wherein the steaming is carried out for 10 to 30 minutes.

15. The process according to claim 10 , wherein, in the steaming, a sulfurous acid compound is added to the corncob meal.

16. The process according to claim 15 , wherein the sulfurous acid compound is added in the amount of 1 to 10 parts by weight for 100 parts by weight of the corncob meal.

17. The process according to claim 10 , wherein the xylanase is added in the amount of 0.1 to 5 parts by weight relative to 100 parts by weight of the filtrate.

18. The process according to claim 10 , wherein the enzyme treatment is carried out under conditions of a pH of 3 to 8, a temperature of 30 to 50° C., a stirring speed of 60 to 200 rpm and a treatment time of 15 to 30 hours.

19. The process according to claim 10 , wherein the steaming is performed by two or more sequentially connected extruders having pressure-sealed cylinders; the levels of temperature and pressure set rise gradually, beginning with the first connected extruder until the last connected extruder; and the steaming conditions for the last connected extruder satisfy the conditions of a temperature of 150 to 250° C. and a pressure of 20 to 29 MPa.

Assignments (2)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 2, 2005
From: NIHON ZAIKEI KABUSHIKI KAISHA
To: CELJAN CO., LTD.
Reel/Frame 016972/0933 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded May 16, 2003
From: MATSUO, SHUNICHI; TAKAMURA, TAKATSUGU
To: NIHON ZAIKEI KABUSHIKI KAISHA
Reel/Frame 014091/0538 →
Priority Claims (1)
JP 2002-186476 · Jun 26, 2002 · national
Continuity (1)
Related Publication 20040002598A1 · Jan 1, 2004