IP Library Granted Patent US 10,595,551
Granted Patent B2
US 10,595,551 · App. 14/745,927 · Granted Mar 24, 2020

Insoluble biomass gel (IBG) and methods of preparing

Inventors: Madhav P. Yadav (North Wales, PA); Kevin B. Hicks (Malvern, PA); David Johnston (Wyndmoor, PA); Kyle A. Hanah (Mount Prospect, IL); Madhuvanti S. Kale (Flourtown, PA)
Assignees: The United States of America, as represented by the Secretary of Agriculture; AgriFiber Holdings LLC
A23L29/262C08H8/00
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Quick Facts
Patent No.
US 10,595,551
App. No.
14/745,927
Granted
Mar 24, 2020
Kind
B2
Abstract

Processes for the preparation of an insoluble biomass gel involving: (a) mixing ground agricultural materials and hexane to produce de-oiled agricultural materials, (b) treating the de-oiled agricultural materials with thermostable α-amylase to produce de-oiled and de-starched agricultural materials, (c) mixing alkali with the de-oiled and de-starched agricultural materials to produce a first residue, (d) mixing hydrogen peroxide with the first residue to form a second residue, and (e) mixing the second residue in water and collecting an insoluble material which is an insoluble biomass gel.

Claims (67)

1. A process for the preparation of an insoluble biomass gel, the process comprising:

(a) mixing ground corn bran and hexane to produce a de-oiled corn bran,

(b) treating said de-oiled corn bran with thermostable α-amylase to produce a de-oiled and de-starched corn bran,

(c) mixing alkali with said de-oiled and de-starched corn bran to produce a first residue,

(d) mixing hydrogen peroxide with said first residue to form a second residue, and

(e) mixing said second residue in water and collecting the insoluble biomass gel;

wherein said insoluble biomass gel contains (i) protein, (ii) xylose and arabinose in the form of a branched arabinoxylan polymer with a β-1,4 linked xylan backbone, and (iii) glucose polymer present in an amount greater than both said xylose and said arabinose.

2. The process according to claim 1 , comprising:

(a) mixing ground corn bran and hexane at room temperature for about one hour followed by filtering to produce de-oiled corn bran,

(b) treating said de-oiled corn bran with thermostable α-amylase at a temperature of about 90° C. to about 95° C. and at a pH of about 6.5 for about 1 hour followed by filtering to produce de-oiled and de-starched corn bran,

(c) mixing alkali with said de-oiled and de-starched corn bran at a pH of about 11.5 and at a temperature of about 100° C. for about 1 h, cooling to room temperature, centrifuging at about 6000×g for about 20 minutes to produce a supernatant and a residue to produce the first residue,

(d) mixing hydrogen peroxide with said first residue to form the second residue at a pH of about 11.5 and a temperature of about 100° C. for about 1 h, centrifuging at about 6000×g for about 20 minutes to produce a second supernatant and the second residue, and

(e) mixing said second residue in water and adjusting the pH to about 5.5 to about 6 at room temperature for about 15 minutes and collecting the insoluble biomass gel.

3. The process according to claim 1 , wherein said alkali are selected from the group consisting of KOH, NH 4 OH, NaOH, Ca(OH) 2 , and mixtures thereof.

4. The process according to claim 1 , wherein said alkali are NaOH and Ca(OH) 2 .

5. The process according to claim 1 , wherein said insoluble biomass gel is an antioxidant with an oxygen radical absorbance capacity of at least 810 μmole Trolox/100 gram insoluble biomass gel.

6. The process according to claim 1 , wherein said insoluble biomass gel contains the following glycosyl residue linkages:

t-Araf (terminally linked arabinofuranosyl residue),

t-Xylp (terminally linked xylopyranosyl residue),

2-Araf (2-linked arabinofuranosyl residue),

t-Glc (terminally linked glucopyranosyl residue),

t-Gal (terminally linked galactopyranose residue),

4-Xylp (4-linked xylopyranosyl residue),

4-Glc (4-linked glucopyranosyl residue),

3,4-Xylp (3,4-linked xylopyranosyl residue), and

4,6-Glc (4,6-linked glucopyranosyl residue) and 2,3,4-Xylp (2,3,4-linked xylopyranosyl residue).

7. The process according to claim 1 , wherein said insoluble biomass gel contains the following glycosyl residue linkages:

t-Araf (terminally linked arabinofuranosyl residue),

t-Xylp (terminally linked xylopyranosyl residue),

2-Araf (2-linked arabinofuranosyl residue),

t-Glc (terminally linked glucopyranosyl residue),

3-Araf (3-linked arabinofuranosyl residue),

t-Gal (terminally linked galactopyranose residue),

3-Xylp and 4-Arap or 5-Araf (3-linked xylopyranose residue and 4-linked arabinopyranose residue or 5-linked arabinofuranose residue),

4-Xylp (4-linked xylopyranosyl residue),

3-Glc (3-linked glucopyranosyl residue),

6-Glc (6-linked glucopyranosyl residue),

4-Glc (4-linked glucopyranosyl residue),

3,4-Xylp (3,4-linked xylopyranosyl residue),

3,4-Glc (3,4-linked glucopyranosyl residue),

2,4-Glc (2,4-linked glucopyranosyl residue), and

4,6-Glc (4,6-linked glucopyranosyl residue) and 2,3,4-Xylp (2,3,4-linked xylopyranosyl residue).

8. The process according to claim 1 , wherein said insoluble biomass gel contains about 2.12% dry weight basis protein.

9. The process according to claim 1 , wherein said insoluble biomass gel contains about 54.92 wt. % glucose, about 24.64 wt. % xylose, and about 11.48 wt. % arabinose.

10. The process according to claim 1 , wherein said process consists essentially of:

(a) mixing corn bran and hexane to produce de-oiled corn bran,

(b) treating said de-oiled corn bran with thermostable α-amylase to produce de-oiled and de-starched corn bran,

(c) mixing alkali with said de-oiled and de-starched corn bran to produce the first residue,

(d) mixing hydrogen peroxide with said first residue to form the second residue, and

(e) mixing said second residue in water and collecting the insoluble biomass gel;

wherein said insoluble biomass gel contains (i) protein, (ii) xylose and arabinose in the form of a branched arabinoxylan with a β-1,4 linked xylan backbone, and (iii) glucose polymer present in an amount greater than both said xylose and said arabinose.

11. The process according to claim 1 , wherein said process consists of:

(a) mixing corn bran and hexane to produce de-oiled corn bran,

(b) treating said de-oiled corn bran with thermostable α-amylase to produce de-oiled and de-starched corn bran,

(c) mixing alkali with said de-oiled and de-starched corn bran to produce the first residue,

(d) mixing hydrogen peroxide with said first residue to form the second residue, and

(e) mixing said second residue in water and collecting the insoluble biomass gel;

wherein said insoluble biomass gel contains (i) protein, (ii) xylose and arabinose in the form of a branched arabinoxylan with a β-1,4 linked xylan backbone, and (iii) glucose polymer present in an amount greater than both said xylose and said arabinose.

12. A process for the preparation of an insoluble biomass gel, the process comprising:

(a) mixing ground corn bran and hexane to produce a first residue containing a de-oiled corn bran,

(b) removing said hexane from said first residue,

(c) treating said first residue with thermostable α-amylase to produce a second residue

(d) washing said second residue to remove maltodextrin,

(e) mixing alkali with said second residue from step (d) to produce a third residue,

(f) mixing hydrogen peroxide with said third residue to form a fourth residue, and

(g) mixing said fourth residue in water and collecting the insoluble biomass gel;

wherein said insoluble biomass gel contains (i) protein, (ii) xylose and arabinose in the form of a branched arabinoxylan polymer with a β-1,4 linked xylan backbone, and (iii) glucose polymer present in an amount greater than both said xylose and said arabinose.

Assignments (5)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Aug 10, 2017
From: KALE, MADHUVANTI S.
To: AGRIFIBER HOLDINGS LLC
Reel/Frame 043263/0578 →
SECURITY INTEREST Recorded Mar 20, 2017
From: AGRITECH WORLDWIDE, INC.
To: KAHN, AS AGENT, JONATHAN
Reel/Frame 041646/0349 →
SECURITY INTEREST Recorded Mar 13, 2017
From: AGRITECH WORLDWIDE, INC.
To: GKS FUNDING LLC, AS ADMINISTRATIVE AGENT
Reel/Frame 041563/0333 →
MERGER Recorded Mar 1, 2017
From: Z TRIM HOLDINGS, INC.
To: AGRITECH WORLDWIDE, INC.
Reel/Frame 041412/0822 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 22, 2015
From: YADAV, MADHAV; HICKS, KEVIN B.; JOHNSTON, DAVID
To: THE UNITED STATES OF AMERICA, AS REPRESENTED BY THE SECRETARY OF AGRICULTURE
Reel/Frame 035988/0650 →
Continuity (2)
Provisional Application 62016186 · Jun 24, 2014
Related Publication 20150366244A1 · Dec 24, 2015