Recovery of protein, protein isolate and/or starch from cereal grains

• US 5,410,021 A
• Filed: 09/01/1992
• Issued: 04/25/1995
• Est. Priority Date: 03/02/1990
• Status: Expired due to Term

• Current Assignee: Energenetics, Inc.
• Original Assignee: Energenetics, Inc.
• Inventors: Kampen, Willem H.
• Primary Examiner(s): Russel, Jeffrey E.
• Application Number:
  US07/923,929
• Time in Patent Office: 966 Days
• Field of Search: 530/370, 530/372, 530/373, 530/374, 530/375, 530/376, 530/414, 530/427, 536/127, 536/128, 127/67
• US Class Current: 530/372
• CPC Class Codes: A23J 1/12 from cereals, wheat, bran, or molasses
• CPC Class Codes: C08B 30/044 from corn or maize

Abstract

The protein/starch bond is broken mechanically by wet attrition milling rather than by cooking or with chemicals alone. The grain particles are milled to a particle size sufficiently small to break the bond between starch and protein and sufficiently large to retain substantially all of the starch granules intact. The protein is then extracted with ethanol and alkali solvents, separated and dried to form protein and/or protein isolate. The intact starch granules are cleaned and dried.

Claims

1. A process for recovering protein from cereal grains containing starch and protein bound into a matrix, the process comprising the steps of:

grinding said grains to a particle size appropriate for introduction to a wet attrition mill;

defatting said grain;

wet attrition milling particles of said grain to a size sufficiently small to break the bond between starch and protein, then

extracting the broken bond protein from the starch with at least one solvent, then

separating the resulting high liquid content portion containing the extracted protein from the resulting high solids content portion containing the starch, and then

subjecting the high liquid content portion containing the extracted protein to continuous cross-flow microfiltration with inorganic membranes for isolating the protein constituent,

concentrating the protein constituent into a dry powder.

3. A process according to one of claim 1 or claim 2 wherein the step of breaking by wet attrition milling comprises milling particles of grain or corn to the point that substantially none of the particles exceed 100 microns.

4. A process according to one of claim 1 or claim 2 further comprising the step of passing starch separated from the protein to a fermentation process as a feedstock.

5. A process according to claim 4 wherein said step of passing starch to a fermentation process comprises passing the starch to a bacterial fermentation process for the production of butanol.

6. A process according to claim 4 wherein said step of passing starch to a fermentation process comprises passing the starch to a yeast fermentation process for the production of ethanol.

2. A process for recovering protein from corn comprising the steps of:

grinding said corn to a particle size appropriate for introduction to a wet attrition mill;

defatting said corn;

wet attrition milling particles of said corn to a size sufficiently small to break the bond between starch and protein, then

extracting the broken bond protein from the starch with at least one solvent, then

separating the resulting high liquid content portion containing the extracted protein from the resulting high solids content portion containing the starch, and then

subjecting the high liquid content portion containing the extracted protein to continuous cross-flow microfiltration with inorganic membranes for isolating the protein constituent,

concentrating the protein constituent into a dry powder.

7. A process for recovering protein from cereal grains comprising the steps of:

grinding said grains to a particle size appropriate for introduction to a wet attrition mill;

defatting said grain;

adding water to ground particulate vegetable matter obtained from said cereal grains containing bound together protein and starch for making a first slurry in which the vegetable matter constitutes up to about 35 percent of the first slurry by weight,

passing the first slurry through an attrition mill and grinding the particulate vegetable matter to a particle size effective to break, by physical action, the bond between protein and starch in the vegetable matter,

adding alcohol to the milled slurry for making extraction slurry in which the alcohol constitutes at least about 50 percent of the extraction slurry be weight,

adjusting the pH of the extraction slurry to a range of from about 9 to about 12,

permitting the pH adjusted slurry to dwell for a sufficient time interval to cause solubilization of protein, then

separating the pH adjusted slurry into high solids content and high liquid content portions,

subjecting the high liquid content portion of the pH adjusted slurry which contains the solubilized protein to continuous cross-flow microfiltration with inorganic membranes for isolating the protein constituent, and then

concentrating and drying the protein constituent in order to form a protein isolate.

9. A process according to one of claim 7 or claim 8 wherein said step of adjusting the pH of the extraction slurry to a range of from about 9 to about 12 comprises adding an alkali.

10. A process according to claim 9 wherein the step of adjusting the pH comprises adding a quantity of at least one of sodium hydroxide and potassium hydroxide in a quantity sufficient for adjusting the pH of the extraction slurry to said range.

11. A process according to claim 10 wherein said step of adding a quantity of at least one of sodium hydroxide and potassium hydroxide further comprises agitating the slurry while adding the pH adjusting hydroxide.

12. A process according to one of claim 7 or claim 8 further comprising the step of adjusting the pH of the slurry to about 8 after passage of said sufficient time interval.

13. A process according to claim 12 wherein said step of adjusting the pH of the slurry to about 8 comprises adding a quantity of sulfuric acid sufficient for adjusting the pH of the slurry to about 8.

14. A process according to one of claim 7 or claim 8 wherein said step of grinding to a particle size effective to break, by physical action, the bond between protein and starch comprises grinding to the point that substantially none of the particles exceed 100 microns.

15. A process according to one of claim 7 or claim 8 further comprising, prior to the step of adding alcohol, the step of adjusting the temperature of the slurry to about 125°

Fahrenheit and maintaining the temperature of the slurry and the high liquid content portion thereof within five degrees of 125°

Fahrenheit throughout the process.

16. A process according to one of claim 7 or claim 8 wherein said step of permitting the slurry to dwell for a sufficient time interval comprises permitting the slurry to dwell for an interval in the range of from about thirty minutes to about two hours and agitating the slurry during the interval of dwell.

17. A process according to one of claim 7 or claim 8 further comprising the step of passing starch separated from the protein isolate to a fermentation process as feedstocks.

18. A process according to claim 17 further comprising the step of passing starch to a bacterial fermentation process for the production of butanol.

19. A process according to claim 17 further comprising the step of passing starch to a yeast fermentation process for the production of ethanol.

8. A process for producing protein isolate from corn comprising the steps of:

grinding corn to a particle size appropriate for defatting and the introduction to a wet attrition mill, then

defatting said corn, then

adding water to the ground corn particles for making a first slurry having corn constituting from about 30 to about 35 weight percent of the first slurry,

passing the first slurry through a wet attrition mill and grinding the corn particles to a particle size effective to break the bond between protein and starch in the corn particles by physical actions, then

adding alcohol to the milled slurry for making an extraction slurry in which the alcohol constitutes at least about 50 percent of the extraction slurry by weight,

adjusting the pH of the extraction slurry to a range of from about 9 to about 12,

permitting the pH adjusted slurry to dwell for a sufficient time interval to cause solubilization of protein, then

separating the pH adjusted slurry into high solids content and high liquid content portions,

subjecting the high liquid content portion of the pH adjusted slurry which contains the solubilized protein to continuous cross-flow microfiltration with inorganic membranes for isolating the protein constituent, and then

concentrating and drying the protein constituent in order to form a protein isolate.

20. A process for producing protein isolate from high lysine corn, comprising the steps of:

grinding high lysine corn having prolamine, glutelin, sugar and starch constituents into particles appropriate for defatting and the introduction to a wet attrition mill, then defatting the corn;

adding water to the ground corn particles for making a slurry having corn particles constituting from about 30 to about 35 weight percent of the slurry;

passing the slurry through an attrition mill and grinding the corn particles to a sufficiently fine particle size to mechanically break the chemical bond between the prolamine and glutelin and starch constitutents by physical action;

then

extracting the prolamine and glutelin constituents of the corn from the attrition milled particles into a solution;

then

separating the milled slurry into a high solids content portion containing starch and a high liquid content portion which contains the extracted prolamine and glutelin constituents of the corn;

subjecting the high liquid content portion of the milled slurry to continuous cross-flow microfiltration with inorganic membranes for isolating the protein constituents; and

then

concentrating and drying the protein constituents to form the protein isolate.

21. A process for producing protein and intact starch granules from cereal grains, comprising the steps of:

a) grinding the cereal grain to a particle size in the range of from about one-sixteenth to about three-sixteenths-inch nominal diameter;

b) defatting said grain;

c) adding water to the ground grain particles for making a slurry in which the grain constitutes from about 25% to about 35% by weight of the slurry;

d) passing the slurry through a wet attrition mill and further milling the ground grain particles to a particle size sufficiently small to break the bond between starch and protein and sufficiently large to retain substantially all of the starch granules intact by physical actions;

e) adding alcohol to the milled slurry for making an extraction slurry in which the alcohol constitutes at least about 50% of the extraction slurry by weight;

f) adjusting the pH of the extraction slurry to a range of from about 9 to about 12;

g) permitting the pH adjusted slurry to dwell for a sufficient interval to cause solubilization of protein;

h) separating the resulting high liquid content portion containing the extracted protein and the resulting high solids content portion containing the starch granules;

i) subjecting the high liquid content portion which contains the solubilized protein to cross-flow microfiltration with inorganic membranes for isolating the protein constituent;

j) concentrating and drying the protein constituent in order to form a protein product; and

k) cleaning and drying the starch granules.

22. The process according the claim 21 wherein the step of adjusting the pH of the slurry to a range of from about 9 to about 12 comprises adding alkali.

23. The process according the claim 22 wherein said step of adjusting the pH of the slurry to a range of from about 9 to 12 comprises adding at least one of sodium hydroxide and potassium hydroxide in a quantity sufficient for adjusting the pH of the slurry to the specified range.

24. The process according to claim 21 wherein in the step of defatting the cereal grain, the temperatures do not exceed 52°

C.

25. The process according the claim 23 wherein after step (g) the pH of the slurry is further adjusted to about 8 by adding a quantity of sulfuric acid sufficient for adjusting the pH of the slurry to about 8.

26. The process according to claim 21 wherein said particle size is obtained by setting the discs of the wet attrition mill with a spacing in the range of about 35-100 microns.

27. The process according to claim 21 wherein said particle size is obtained by setting the discs of said wet attrition mill with a spacing in the range of about 50-100 microns.

28. The process according to claim 21 wherein, after the cleaning and drying step, the pH of the starch granules is reduced to approximately 6.

29. The process according the claim 21 wherein during the extraction steps set forth in sub-paragraphs (e)-(g) the temperature is maintained within 5°

of 125°

Fahrenheit.

30. The process according to claim 21 wherein said step of permitting the slurry to dwell for a sufficient time interval comprises permitting the slurry to dwell for an interval of time in the range of from about 30 minutes to about 2 hours and agitating the slurry during the interval of dwell.

31. The process according to claim 21 and further after step (h) centrifuging the high liquid content portion of the slurry at a g-force in the range of 10,000-15,000×

g to recover dispersed particulate matter.

32. The process according to claim 21 wherein the cross-flow microfiltration step includes diafiltration in conjunction therewith.

33. A process for producing protein isolate from cereal grains containing starch and protein bound into a matrix, comprising the steps of:

grinding the grain to a particle size in the range of from about one-sixteenth to about three-sixteenths-inch nominal diameter;

defatting the ground grain particles;

adding water to the ground grain particles for making a first slurry having grain constituting up to about 35 weight % of the first slurry;

passing the first slurry through a wet attrition mill and grinding the grain particles to a particle size effective to break the bond between protein and starch in the grain by physical actions;

adding alcohol to the milled slurry for making an extraction slurry in which the alcohol constitutes at least about 50% of the extraction slurry by weight;

adjusting the pH of the extraction slurry to a range of from about 9 to about 12;

permitting the pH adjusted slurry to dwell for a sufficient time interval to cause solubilization of protein;

separating the resulting slurry into high solids content and high liquid content portions;

subjecting the high liquid content portion of the resulting slurry which contains the solubilized protein to microfiltration and diafiltration for isolating the protein constituent;

concentrating and drying the protein constituent in order to form a protein isolate.

34. The process according to claim 33 wherein said step of wet attrition milling to a particle size effective to break, by physical action, the bond between protein and starch comprises milling to the point that substantially none of the particles exceed 100 microns.

35. The process according to claim 33 wherein said step of microfiltration and diafiltration comprises subjecting the high liquid content portion of the slurry which contains the solubilized protein to a cross-flow microfiltering unit with inorganic membranes.