# US 9,040,270 B2 · De-fatted soy production process and value added by-products from de-fatted soy flour

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- Number: US 9,040,270 B2
- Document ID: US9040270B2
- Status: Granted
- Kind: B2
- Application number: 13/314,403
- Filed: 2011-12-08
- Published: 2012-07-05
- Granted: 2015-05-26
- Earliest claimed: 1999-01-13
- Assignees: Little Sioux Corn Processors, LLC.
- Applicants: John E. Prevost; Neal A. Hammond
- Inventors: John E. Prevost; Neal A. Hammond
- Web page: https://patentgrep.com/patent/US9040270B2

## CPC

- C12P 7/06: Ethanol, i.e. non-beverage
- A23J 1/14: from leguminous or other vegetable seeds; from press-cake or oil-bearing seeds
- A23L 11/07: {Soya beans, e.g. oil-extracted soya bean flakes (A23L11/30 takes precedence)}
- A23L 11/30: Removing undesirable substances, e.g. bitter substances
- A23L 11/33: {using enzymes; Enzymatic transformation of pulses or legumes}
- A23L 29/35: {Degradation products of starch, e.g. hydrolysates, dextrins; Enzymatically modified starches}
- C11B 3/008: {by filtration, e.g. including ultra filtration, dialysis (C11B3/005 takes precedence)}
- C12P 7/08: produced as by-product or from waste or cellulosic material substrate
- C12P 7/10: substrate containing cellulosic material
- C12P 2201/00: Pretreatment of cellulosic or lignocellulosic material for subsequent enzymatic treatment or hydrolysis
- C12P 2203/00: Fermentation products obtained from optionally pretreated or hydrolyzed cellulosic or lignocellulosic material as the carbon source
- Y02E 50/10: Biofuels, e.g. bio-diesel
- C12P: FERMENTATION OR ENZYME-USING PROCESSES TO SYNTHESISE A DESIRED CHEMICAL COMPOUND OR COMPOSITION OR TO SEPARATE OPTICAL ISOMERS FROM A RACEMIC MIXTURE {(brewing of beer C12C; producing vinegar C12J; producing specific peptides or proteins C07K; producing enzymes C12N9/00; DNA or RNA concerning genetic engineering, vectors, e.g. plasmids, or their isolation, preparation or purification C12N15/00; measuring or testing processes involving enzymes or microorganisms C12Q; measuring or testing processes involving nucleic acid amplification reactions C12Q1/6844; fermentation processes to form a food composition, A21 or A23; compounds in general, see the relevant compound class, e.g. C01, C07)}
- A23J: PROTEIN COMPOSITIONS FOR FOODSTUFFS; WORKING-UP PROTEINS FOR FOODSTUFFS; PHOSPHATIDE COMPOSITIONS FOR FOODSTUFFS
- A23L: FOODS, FOODSTUFFS OR NON-ALCOHOLIC BEVERAGES, NOT OTHERWISE PROVIDED FOR; PREPARATION OR TREATMENT THEREOF (preservation thereof A23B)
- C11B: PRODUCING, e.g. BY PRESSING RAW MATERIALS OR BY EXTRACTION FROM WASTE MATERIALS, REFINING OR PRESERVING FATS, FATTY SUBSTANCES, e.g. LANOLIN, FATTY OILS OR WAXES; ESSENTIAL OILS; PERFUMES (drying-oils C09F)
- Y02E: REDUCTION OF GREENHOUSE GAS [GHG] EMISSIONS, RELATED TO ENERGY GENERATION, TRANSMISSION OR DISTRIBUTION

## Abstract

An improved process for producing de-fatted soy utilizing a de-fatted soy flour and for producing value added by-products from de-fatted soy flour wherein soybeans are de-hulled and the de-hulled stream ground to a flour consistency. The ground soy flour is mixed with water and other additives to produce a vitamin and mineral enriched stream that is then filtered to various value added by-products. In a preferred embodiment the vitamin and mineral enriched stream is filtered through a 0.1-1.0 micron membrane to produce a de-fatted soy product stream and a fatted soy product stream. The fatted soy product stream can be dried to produce dry, less than 12% water by weight, product B for use in cosmetics and pharmaceutical products. The de-fatted soy product can be filtered through reverse osmosis (RO) filtration unit to obtain a vitamin and mineral enriched product stream that can be dried to powder form and used as a food supplement additive I. If desired the full fatted soy flour or the de-fatted soy product stream can be combined with whole stillage from an ethanol process and used in producing various other value added products.

## Claims

### Claim 1

An improved ethanol production process comprising:
(a) milling a carbohydrate-containing material to produce a carbohydrate-containing flour having a median particle size of less than about 100 microns;
(b) hydrolyzing the carbohydrate-containing flour under operating conditions to form a mixture comprising partially gelatinized carbohydrate-containing flour and cleaved terminal amylose groups, wherein the terminal amylose groups are cleaved from the carbohydrate-containing flour;
(c) milling soy hulls to produce a soy hull flour having a median particle size of less than about 100 microns;
(d) adding the soy hull flour to the mixture to form a slurry, the slurry comprising the partially gelatinized carbohydrate-containing flour, the cleaved terminal amylose groups, and the soy hull flour;
(e) fermenting the slurry to produce fermented slurry, the fermented slurry comprising ethanol and whole stillage; and
(f) distilling the fermented slurry to separate the ethanol from the whole stillage.

### Claim 2 (depends on 1)

The improved ethanol production process according to claim 1 further comprising:
(a) milling de-hulled soy meal to produce a de-hulled soy meal flour having a median particle size of less than about 100 microns;
(b) mixing water with the de-hulled soy meal flour to form a de-hulled soy meal flour slurry;
(c) filtering the de-hulled soy meal flour slurry through a microfilter having a pore size of about 0.1-1.0 microns to produce (i) a defatted soy solution comprising nutrients useful in the formulation of neutraceuticals or acrylic paint, and (ii) a retentate comprising soy oil, soy proteins and soy carbohydrates forming an emulsion;
(d) filtering the whole stillage through a microfilter to form a whole stillage permeate; and
(e) mixing said defatted soy solution with said whole stillage permeate.

### Claim 3 (depends on 2)

The improved ethanol production process according to claim 2, further comprising drying the emulsion under conditions to reduce the water content of the emulsion to less than about 12% to form a product useful in formulating cosmetic or pharmaceutical products.

### Claim 4 (depends on 1)

The improved ethanol production process according to claim 1, further comprising:
(a) milling de-hulled soy meal to produce a de-hulled soy meal flour having a median particle size of less than about 100 microns;
(b) mixing water with the de-hulled soy meal flour to form a de-hulled soy meal flour slurry; and
(c) mixing the de-hulled soy meal flour slurry with the whole stillage to form a stillage-slurry mixture.

### Claim 5 (depends on 4)

The improved ethanol production process according to claim 4, further comprising:
(a) mixing nutrients with the stillage-slurry mixture;
(b) extruding the stillage-slurry mixture and nutrients under extruding conditions comprising pressures of 300-3000 psi and temperatures of 100° C.-200° C. to form an extruded stream; and
(c) drying the extruded stream to form a protein enriched product having a water content less than about 12% by weight.

### Claim 6 (depends on 1)

The improved ethanol production process according to claim 1, further comprising:
(a) mixing water and additives with the carbohydrate-containing flour in step
(b) to form a slurry, wherein the additives comprise one or more enzymes in an amount of 0.5%-1.5% by dry weight.

### Claim 7 (depends on 6)

The improved ethanol production process according to claim 6 wherein the additives include nutrients, and the ratio of the carbohydrate-containing flour, water, enzymes and nutrients in the slurry is about 100:20:1.5:1 to about 100:15:0.5:0.5 by weight.

### Claim 8 (depends on 7)

The improved ethanol production process according to claim 7 wherein the mixing and hydrolyzing is performed in an extruder.

### Claim 9 (depends on 6)

The improved ethanol production process according to claim 6 wherein the operating conditions during hydrolyzing comprises extruding at pressures of 300-3000 psi, temperatures of 100° C.-200° C., and for a time to cleave 20%-40% of the terminal amylose groups from the carbohydrate-containing flour.

### Claim 10 (depends on 6)

The improved ethanol production process according to claim 6 wherein:
(a) the carbohydrate-containing material is whole corn kernels;
(b) the operating conditions during hydrolyzing comprise pressures of about 500 psi and temperatures of 80° C.-130° C., for 45-60 seconds; and
(c) at least one of the enzymes functions to promote hydrolyzing the slurry and cleaving the terminal amylose groups.

### Claim 11 (depends on 1)

The improved ethanol production process according to claim 1, further comprising filtering a dehulled soy flour of median particle size less than 100 microns, forming a permeate comprising a defatted soy solution and mixing the defatted soy solution with the whole stillage.

### Claim 12 (depends on 1)

The improved ethanol production process according to claim 1 further comprising:
(a) after said distillation of said ethanol, filtering the whole stillage through a microfilter having a pore size of about 0.1-1.0 microns to produce (i) a nutrient-containing permeate and (ii) a retentate comprising proteins, carbohydrates, fat globules, cell wall materials and oil;
(b) drying the retentate to form a product having a water content of less than about 12% by weight useful in the formulation of cosmetic or pharmaceutical products.

### Claim 13 (depends on 12)

The improved ethanol production process according to claim 12, further comprising:
(a) milling de-hulled soy meal flour to form a de-hulled soy meal flour slurry;
(b) filtering the de-hulled soy meal flour slurry through a microfilter having a pore size of about 0.1-1.0 microns to produce (i) a defatted soy solution and (ii) a retentate emulsion;
(c) mixing the defatted soy solution and the nutrient-containing permeate to form a modified whole stillage stream; and
(d) extruding the modified whole stillage stream to form a by-product containing feedstock.

### Claim 14 (depends on 13)

The improved ethanol production process according to claim 13, further comprising:
(a) filtering the by-product feedstock through an ultrafilter configured to have a molecular weight cut-off greater than about 1,000,000 to produce (i) a soy protein containing retentate and (ii) a first permeate stream; and
(b) drying the soy protein containing retentate under conditions to produce a soy protein containing product having a water content less than about 12% by weight.

### Claim 15 (depends on 14)

The improved ethanol production process according to claim 14, further comprising:
(a) filtering the first permeate stream through a reverse osmosis filtration unit capable of operating at pressures of at least 5000 psi and having a pore size configured to separate vitamins, minerals and soy carbohydrates from the first permeate stream to form (i) a low molecular weight material containing retentate and (ii) a water-rich permeate; and
(b) drying the low molecular weight material retentate under conditions to produce a low molecular weight containing product having a water content less than about 12% by weight.

### Claim 16 (depends on 15)

The improved ethanol production process according to claim 15, wherein said improved ethanol process is continuous and further comprises mixing at least a portion of the water-rich permeate with the carbohydrate-containing flour prior to hydrolyzing.

### Claim 17 (depends on 14)

The improved ethanol production process according to claim 14, wherein the carbohydrate-containing material is corn, and further comprising:
(a) filtering the by-product feedstock through a second ultrafilter having a pore size configured to have a molecular weight cut-off greater than about 50,000 to produce (i) a non-zein protein containing retentate and (ii) a second permeate stream containing zein corn proteins; and
(b) drying the non-zein protein containing retentate under conditions to produce a non-zein protein containing product having a water content less than about 12% by weight.

### Claim 18 (depends on 17)

The improved ethanol production process according to claim 17, further comprising;
(a) filtering the second permeate stream through a third ultrafilter having a pore size configured to have a molecular weight cut-off of about 10,000 to produce (i) a zein corn protein containing retentate and (ii) a third permeate stream containing medium and low molecular weight dextrins; and
(b) drying the zein corn protein containing retentate to produce a zein corn protein containing product having a water content less than about 12% by weight.

### Claim 19 (depends on 18)

The improved ethanol production process according to claim 18, further comprising:
(a) filtering the third permeate stream containing medium and low molecular weight dextrins through a nanofilter having a pore size configured to have a molecular weight cut-off less than about 10,000 to produce (i) a low and medium molecular weight dextrin containing retentate and (ii) a fourth permeate stream; and
(b) drying the low and medium molecular weight dextrin containing retentate to produce a dextrin containing product having a water content less than about 12% by weight.

### Claim 20 (depends on 18)

The improved ethanol production process according to claim 18, further comprising:
(a) mixing water and additives with said carbohydrate containing flour prior to hydrolyzing, wherein the additives comprise one or more enzymes, wherein one of the enzymes is alpha-amylase and another of the enzymes is an enzyme other than alpha-amylase having an activity to promote the production of cyclodextrins during the fermenting;
(b) filtering the third permeate stream through a nanofilter having a pore size configured to have a molecular weight cut-off of 2,000 to produce (i) a cyclodextrin containing retentate and (ii) a fourth permeate stream; and containing product having a water content less than about 12% by weight;
(c) drying the cyclodextrin containing retentate to produce a cyclodextrin.