IP Library Granted Patent US 7,812,153
Granted Patent B2
US 7,812,153 · App. 10/797,938 · Granted Oct 12, 2010

Process for manufacturing high purity xylose

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Quick Facts
Patent No.
US 7,812,153
App. No.
10/797,938
Granted
Oct 12, 2010
Kind
B2
Abstract

A process for manufacturing xylose by extracting hemicellulose from a cellulosic material, such as by a cold caustic extraction method, concentrating the extract, such as by nanofiltration, into a hemicaustic stream containing hemicellulose with greater than about 85 wt % xylan content, and subsequently hydrolysing the xylan from the hemicaustic stream to xylose. The high concentration of xylan within the concentrated hemicaustic stream enables hydrolyzation of the xylan to food-grade xylose and, optionally, hydrogenation of the xylose to xylitol without the need of a chromatographic separation step as previously required.

Claims (61)

1. A method of producing xylose from a cellulose material containing hemicellulose, comprising:

providing a pre-hydrolyzed cellulose pulp that is at least partially bleached and has a hemicellulose content that is predominantly xylan, and a lignin content that is less than 1 wt. %;

extracting the hemicellulose from the at least partially bleached pulp into a caustic solution thereby forming a hemicaustic solution;

separating the hemicaustic solution into a concentrated hemicellulose solution and a concentrated caustic solution; and,

hydrolyzing the hemicellulose from the concentrated hemicellulose solution to produce xylose.

2. The method of claim 1 , wherein the step of providing pulp comprises providing hardwood pulp wherein the pulp is greater than 4 wt % hemicellulose.

3. The method of claim 1 , wherein the step of providing pulp comprises providing hardwood pulp where the hemicellulose is greater than 85 wt % xylan.

4. The method of claim 1 , wherein the step of providing the at least partially bleached the pulp comprises providing a cooked cellulose pulp and subjecting the cooked pulp to a series of oxidation and extraction stages until greater than 80 wt % of the original lignin content of the pulp has been removed.

5. The method of claim 1 , wherein the step of proving the at least partially bleached pulp comprises providing a cooked cellulose pulp and subjecting the cooked pulp to a series of oxidation and extraction stages until the pulp has an ISO brightness of 88% or higher.

6. The method of claim 1 , wherein the step of extracting the hemicellulose from the pulp comprises extracting the hemicellulose using a cold caustic treatment.

7. The method of claim 6 , wherein the pulp has a consistency of about 2 wt % to about 50 wt % with respect to the caustic solution during cold caustic treatment.

8. The method of claim 7 , wherein the caustic solution has a pH greater than 13 during treatment.

9. The method of claim 8 , wherein a temperature of the caustic solution is from about 20° C. to about 50° C. during treatment.

10. The method of claim 6 , wherein the cold caustic treatment is continued until the treated pulp contains no more than 15 wt % hemicellulose.

11. The method of claim 10 , wherein the cold caustic treatment is continued until the treated pulp contains no more than 5 wt % hemicellulose.

12. The method of claim 6 , wherein a temperature of the caustic solution is less than 50° C. during treatment.

13. The method of claim 1 , wherein the step of extracting the hemicellulose from the pulp into a caustic solution comprises holding the pulp in the caustic solution for a period of time and thereafter washing the pulp with water, wherein the caustic solution, extracted hemicellulose, and wash water form the hemicaustic solution.

14. The method of claim 1 , wherein the step of separating the hemicaustic solution into a concentrated hemicellulose solution and a concentrated caustic solution comprises subjecting the hemicaustic solution to a separation technique selected from the group consisting of nanofiltration, distillation, centrifugation, and precipitation.

15. The method of claim 14 , wherein the step of separating the hemicaustic solution comprises filtering the solution through a nanofiltration apparatus wherein the permeate stream exiting the nanofiltration apparatus is the concentrated caustic solution having greater than about 80 wt % of the original caustic solution, and wherein the concentrate stream is the concentrated hemicellulose solution that constitutes from about 5 wt % to about 30 wt % hemicellulose.

16. The method of claim 1 , wherein the step of hydrolyzing the hemicellulose from the concentrated hemicellulose solution comprises

acidifying the concentrated hemicellulose solution with a mineral acid; and,

acid hydrolyzing the hemicellulose, whereby the xylan content of the hemicellulose is converted to xylose.

17. The method of claim 16 , further comprising the step of demineralizing the acidified concentrated hemicellulose solution prior to the acid hydrolyzing step.

18. The method of claim 17 , wherein the step of demineralizing is accomplished by filtration.

19. The method of claim 16 , further comprising the step of demineralizing the concentrated hemicellulose solution prior to the acidifying step.

20. The method of claim 19 , wherein the step of demineralizing is accomplished by ion exchange.

21. The method of claim 16 , further comprising the step of removing organic/inorganic acids, metal salts, and colored by-products from the hydrolyzed hemicellulose.

22. The method of claim 21 , wherein the step of removing acids, salts, and by-products from the hydrolyzed hemicellulose comprises contacting the hydrolyzed hemicellulose with a cationic ion exchange resin.

23. The method of claim 21 , wherein the step of removing acids, salts, and by-products from the hydrolyzed hemicellulose comprises contacting the hydrolyzed hemicellulose with an anionic ion exchange resin.

24. The method of claim 1 , wherein the resulting hydrolyzed hemicellulose has a xylose content of greater than 90 wt %.

25. The method of claim 1 , wherein the step of providing a pulp comprises

providing a hardwood selected from sweet gum, black gum, maple, oak, eucalyptus, poplar, beech, aspen, and mixtures thereof;

digesting the hardwood to a hardwood pulp; and,

at least partially bleaching the digested pulp.

26. The method of claim 1 , wherein the step of providing a pulp comprises

pre-hydrolyzing a hardwood feed material;

digesting the pre-hydrolyzed hardwood; and,

at least partially bleaching the digested pulp using a conventional pulp bleaching process.

27. A process for producing a xylose product from a cellulose material, comprising the steps of:

at least partially chemically bleaching a cooked pre-hydrolized cellulose pulp using a conventional pulp bleaching process to provide a pre-hydrolyzed cellulose pulp that is at least partially bleached and has a hemicellulose content that is predominantly xylan, and a lignin content that is less than 1 wt. %;

using a cold caustic treatment to extract hemicellulose from the at least partially bleached cellulose pulp into a caustic solution thereby forming a hemicaustic solution;

separating the hemicaustic solution by nanofiltration into a concentrated hemicellulose solution and a concentrated caustic solution; and,

hydrolyzing the hemicellulose from the concentrated hemicellulose solution.

28. The process of claim 27 , wherein the step of providing a cellulose pulp comprises providing a hardwood pulp wherein the hardwood is greater than 5 wt % hemicellulose.

29. The process of claim 28 , wherein the hemicellulose of the hardwood is greater than 85 wt % xylan.

30. The process of claim 27 , wherein the at least partially bleached pulp has an ISO brightness of 88% or higher.

31. The process of claim 27 , wherein the cold caustic treatment is continued until the treated pulp contains no more than 15 wt % hemicellulose.

32. The process of claim 31 , wherein the cold caustic treatment is continued until the treated pulp contains no more than 5 wt % hemicellulose.

33. The process of claim 27 , wherein the step of nanofiltering the hemicaustic solution comprises filtering the solution through a nanofiltration apparatus wherein the permeate stream exiting the nanofiltration apparatus is the concentrated caustic solution having greater than about 80 wt % of the original caustic solution, and wherein the concentrate stream is the concentrated hemicellulose solution that constitutes from about 5 wt % to about 30 wt % hemicellulose.

34. The process of claim 27 , wherein the step of hydrolyzing the hemicellulose from the concentrated hemicellulose solution comprises

neutralizing the concentrated hemicellulose solution with a mineral acid; and,

acid hydrolyzing the hemicellulose, whereby the xylan content of the hemicellulose is converted to xylose.

35. The method of claim 34 , further comprising the step of demineralizing the concentrated hemicellulose solution prior to the acid hydrolyzing step.

36. The process of claim 34 , further comprising the step of removing organic/inorganic acids, metal salts, and colored by-products from the hydrolyzed hemicellulose.

37. The method of claim 27 , further comprising the step of acidifying the concentrated hemicellulose solution prior to the hydrolyzing step.

38. The process of claim 27 , wherein the resulting hydrolyzed hemicellulose has a xylose content of greater than 90 wt %.

39. A method of producing xylose from a cellulose material containing hemicellulose, comprising:

providing a cellulose pulp that is at least partially bleached and has a hemicellulose content that is predominantly xylan, and a lignin content that is less than 1 wt. %;

extracting the hemicellulose from the at least partially bleached pulp into a caustic solution thereby forming a hemicaustic solution;

separating the hemicaustic solution into a concentrated hemicellulose solution and a concentrated caustic solution; and,

hydrolyzing the hemicellulose from the concentrated hemicellulose solution to produce a xylose product having a purity of 80 wt % or greater in the absence of an additional purification step.

Assignments (7)
RELEASE OF SECURITY INTEREST Recorded Nov 7, 2024
From: COMPUTERSHARE TRUST COMPANY, N.A. AS SUCCESSOR TO WELLS FARGO BANK
To: RAYONIER ADVANCED MATERIALS INC.; RAYONIER PERFORMANCE FIBERS, LLC
Reel/Frame 069190/0878 →
RELEASE OF SECURITY INTEREST Recorded Dec 28, 2020
From: BANK OF AMERICA, N.A.
To: RAYONIER ADVANCED MATERIALS INC.; RAYONIER PERFOMANCE FIBERS, LLC
Reel/Frame 054752/0295 →
SECURITY AGREEMENT Recorded Dec 23, 2020
From: RAYONIER PERFORMANCE FIBERS, LLC; RAYONIER ADVANCED MATERIALS INC.
To: WELLS FARGO BANK, NATIONAL ASSOCIATION, AS NOTES COLLATERAL AGENT
Reel/Frame 054843/0044 →
SECURITY AGREEMENT Recorded Dec 23, 2020
From: RAYONIER PERFORMANCE FIBERS, LLC; RAYONIER ADVANCED MATERIALS INC.
To: BANK OF AMERICA, N.A., AS COLLATERAL AGENT
Reel/Frame 054842/0950 →
SECURITY INTEREST Recorded Sep 9, 2014
From: RAYONIER PERFORMANCE FIBERS, LLC
To: BANK OF AMERICA, N.A.
Reel/Frame 033706/0065 →
NUNC PRO TUNC ASSIGNMENT Recorded Jun 23, 2014
From: RAYONIER PRODUCTS AND FINANCIAL SERVICES COMPANY
To: RAYONIER TRS HOLDINGS INC.
Reel/Frame 033158/0144 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 23, 2014
From: RAYONIER TRS HOLDINGS INC.
To: RAYONIER PERFORMANCE FIBERS, LLC
Reel/Frame 033159/0062 →