Method for producing microcrystalline cellulose

• US 5,769,934 A
• Filed: 01/15/1997
• Issued: 06/23/1998
• Est. Priority Date: 01/15/1997
• Status: Expired due to Term

• Current Assignee: Dupont Nutrition USA Inc. (International Flavors & Fragrances Incorporated)
• Original Assignee: FMC Corporation
• Inventors: Landi, Carol D., Ha, Ewan Y. W.
• Primary Examiner(s): BRUNSMAN, DAVID M
• Application Number:
  US08/783,776
• Time in Patent Office: 524 Days
• Field of Search: 106/162.8, 536/56
• US Class Current: 106/162.8
• CPC Class Codes: C08B 15/02 Oxycellulose; Hydrocellulose; Cellulosehydrate, e.g. microcrystalline cellulose

Abstract

A method for producing microcrystalline cellulose by the steps of subjecting a cellulose source material to steam explosion treatment, extracting the steam treated cellulosic material to remove hemicellulose and lignin, and recovering microcrystalline cellulose that is substantially colloidal in particle size and essentially free of fibrous cellulose.

Claims

1. A process for the production of microcrystalline cellulose consisting essentially of

(i) introducing a cellulose source material in divided form into a pressurizable reactor;

(ii) subjecting the cellulosic material in the reactor to a steam explosion treatment, by contacting the cellulosic material with pressurized steam at a temperature of at least about 170°

C. for a period of time sufficient to hydrolyze the cellulosic material, the temperature and time being sufficient to provide a depolymerized cellulosic material containing microcrystalline cellulose having a true level off degree of polymerization of about 100 to about 400, and thereafter explosively releasing the steam pressure when the level off degree of polymerization is reached;

(iii) extracting the steam exploded cellulosic material to remove hemicellulose and to remove lignin; and

(iv) recovering microcrystalline cellulose that is substantially colloidal in particle size and that is essentially free of fibrous cellulose.

2. The process of claim 1 wherein the cellulosic material is subjected to a single steam explosion treatment step.

3. The process of claim 1 wherein the steam treatment time is about 1 minute to about 20 minutes.

4. The process of claim 1 wherein the temperature during the steam treatment is from about 180°

C. to about 350°

C.

5. The process of claim 1 wherein the steam explosion treatment is carried out under temperature and time conditions to have a logarithm of the severity, S, of the steam explosion treatment with a value of about 3.5 to about 6, where S is calculated as ##EQU3##

6. The process of claim 5 wherein the logarithm of severity S of the steam explosion treatment has a value of about 4 to about 5.

7. The process of claim 5 wherein the time is about 1 minute to about 20 minutes.

8. The process of claim 5 wherein the temperature during steam explosion treatment is from about 180°

C. to about 350°

C.

9. The process of claim 5 wherein the logarithm of severity S of the steam explosion treatment has a value of 4.7 or more.

10. The process of claim 1 wherein the cellulose source material is a lignocellulose material.

11. The process of claim 10 wherein the cellulose source material is wood chips.

12. The process of claim 10 wherein the lignocellulose material is selected from the group consisting of hardwood, soft wood, corn hulls, soy hulls, oat hulls, corn stalks, corn cobs, bagasse, wheat straw, oat straw, rice straw and barley straw.

13. The process of claim 1 wherein the cellulose source material is selected from the group consisting of cotton and regenerated cellulose.

14. The process of claim 1 wherein the cellulose source material is not subjected to hydrolysis with a strong acid.

15. The process of claim 1 wherein the steam exploded cellulosic material is extracted with a hot aqueous medium to extract hemicellulose.

16. The process of claim 15 wherein the hemicellulose extraction step uses an aqueous medium at a temperature of from about 50°

C. to about 100°

C.

17. The process of claim 16 wherein the hot aqueous medium used in the hemicellulose extraction step is water.

18. The process of claim 1 wherein the steam exploded cellulosic material is extracted with a lignin-solubilizing solvent to remove lignin.

19. The process of claim 18 wherein the lignin extraction step uses an aqueous alkali solution or an alcohol solvent.

20. The process of claim 19 wherein the lignin extraction step uses an aqueous alkali solution that is aqueous sodium hydroxide.

21. The process of claim 1 wherein the recovered microcrystalline cellulose comprises at least about one-third submicron size particles and has a mean particle size of less than about 10 microns.

22. The process of claim 1 wherein the recovered microcrystalline cellulose has a mean particle size of less than about 1 micron.

23. The process of claim 1 wherein the microcrystalline cellulose has a level off degree of polymerization of from about 150 to about 300.

24. The process of claim 1 wherein the microcrystalline cellulose is recovered as a bleached product by bleaching the steam exploded and extracted cellulosic material.

25. The process of claim 1 wherein the microcrystalline cellulose is recovered as a dry free flowing product.

26. A process for the production of microcrystalline cellulose consisting essentially of

(i) introducing a cellulose source material in divided form into a pressurizable reactor;

(ii) subjecting the cellulosic material in the reactor to a steam explosion treatment, by contacting the cellulosic material with pressurized steam at a temperature of at least about 170°

C. for a period of time sufficient to hydrolyze the cellulosic material, the temperature and time being sufficient to provide a depolymerized cellulosic material containing microcrystalline cellulose having a true level off degree of polymerization of about 100 to about 400, and thereafter explosively releasing the steam pressure when the level off degree of polymerization is reached;

(iii) extracting the steam exploded cellulosic material to remove hemicellulose and to remove lignin;

(iv) attriting the steam exploded and extracted cellulosic material under high shear; and

(v) recovering microcrystalline cellulose that is substantially colloidal in particle size and that is essentially free of fibrous cellulose.

27. The process of claim 26 wherein the microcrystalline cellulose is recovered as a bleached product by bleaching the steam exploded and extracted cellulosic material.

28. The process of claim 26 wherein the microcrystalline cellulose is recovered as a dry free flowing product.

29. A process for the production of microcrystalline cellulose consisting essentially of

(i) introducing a cellulose source material in divided form into a pressurizable reactor;

(ii) subjecting the cellulosic material in the reactor to a steam explosion treatment, by contacting the cellulosic material with pressurized steam at a temperature of at least about 170°

C. for a period of time sufficient to hydrolyze the cellulosic material, the temperature and time being sufficient to provide a depolymerized cellulosic material containing microcrystalline cellulose having a true level off degree of polymerization of about 100 to about 400, and thereafter explosively releasing the steam pressure when the level off degree of polymerization is reached;

(iii) extracting the steam exploded cellulosic material to remove hemicellulose and to remove lignin;

(iv) coprocessing the steam exploded and extracted cellulosic material under high shear with a hydrocolloid or a surfactant; and

(v) recovering microcrystalline cellulose that is substantially colloidal in particle size and that is essentially free of fibrous cellulose.

30. The process of claim 29 wherein the cellulosic material is coprocessed with a hydrocolloid selected from carboxymethylcellulose, xanthan gum, guar gum, locust bean gum, alginate, starch and maltodextrin.

31. The process of claim 29 wherein the microcrystalline cellulose is recovered as a bleached product by bleaching the steam exploded and extracted cellulosic material.

32. The process of claim 29 wherein the microcrystalline cellulose is recovered as a dry free flowing product.

33. A process for the production of microcrystalline cellulose consisting essentially of

(i) introducing a cellulose source material in divided form into a pressurizable reactor;

(ii) subjecting the cellulosic material in the reactor to a steam explosion treatment, by contacting the cellulosic material with pressurized steam at a temperature of at least about 170°

C. for a period of time sufficient to hydrolyze the cellulosic material, the temperature and time being sufficient to provide a depolymerized cellulosic material containing microcrystalline cellulose having a true level off degree of polymerization of about 100 to about 400, and thereafter explosively releasing the steam pressure when the level off degree of polymerization is reached;

(iii) extracting the steam exploded cellulosic material to remove hemicellulose and to remove lignin;

(iv) attriting the steam exploded and extracted cellulosic material under high shear;

(v) coprocessing the steam exploded and extracted cellulosic material under high shear with a hydrocolloid or a surfactant, such coprocessing being carried out either concurrently with the attrition step or after the attrition step; and

(vi) recovering microcrystalline cellulose that is substantially colloidal in particle size and that is essentially free of fibrous cellulose.

34. The process of claim 33 wherin the microcrystalline cellulose is recovered as a bleached product by bleaching the steam exploded and extracted cellulosic material.

35. The process of claim 33 wherein the microcrystalline cellulose is recovered as a dry free flowing product.