US0080085l7B2
`
`(12) Ulllted States Patent
`Cantrell et al.
`
`(10) Patent No.:
`(45) Date of Patent:
`
`US 8,008,517 B2
`*Aug. 30, 2011
`
`(54) METHOD OF RECOVERING OIL FROM
`THIN STILLAGE
`_
`Inventors: David Fred Cantrell, Lakemont, GA
`(US); David J. Winsness, Alpharetta,
`GA (Us)
`
`(75)
`
`(73) Assignee: GS Cleantech Corporation, New York,
`NY (US)
`
`( * ) Notice:
`
`Subject to any disclaimer, the term of this
`patent is extended or adjusted under 35
`U.S.C. 154(b) by 0 days.
`This patent is subject to a terminal dis-
`Claimer.
`
`DE
`
`(21) Appl.No.: 12/559,136
`
`2
`1
`,
`,
`1,366,339 A
`2,206,024 A
`2,216,904 A
`2,216,905 A
`2,263,608 A
`2,439,177 A
`2
`2,524,718 A
`2,663,718 A
`2,929,150 A
`
`gel-aVa1
`aiton
`1/1921 Alexander
`8/1937 Brown
`10/1940 Brown
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`11/1941 Brown
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`Eglégln
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`(Continued)
`
`FOREIGN PATENT DOCUMENTS
`80874
`12/1966
`(Continued)
`
`OTHER PUBLICATIONS
`
`Ffled:
`
`(22)
`(65)
`
`Sep' 14’ 2009
`Prior Publication Data
`
`GEA Westfalia Separator: Inc. V. Greenshift Corporation, Complaint,
`Case No. 1:09-cv-07686-LMM; filed Sep. 3, 2009, pp. 1-28, stamped
`by Judge McKenna.
`
`Jan. 7, 2010
`US 2010/0004474 A1
`Related U.S. Application Data
`.
`.
`.
`.
`(63) Continuation of application No. 11/122,859, filed on
`May 5, 2005, now Pat. No. 7,601,858.
`
`(60) Provisional application No. 60/602,050, filed on Aug.
`17, 2004.
`
`(51)
`
`Int CL
`(200601)
`CUB 1/00
`554/8
`(52) U.S. Cl.
`.................................... ..
`(58) Field of Classification Search ..................... .. 554/8
`See application file for complete search history.
`
`
`
`(56)
`
`References Cited
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`U.S. PATENT DOCUMENTS
`
`313,665 A
`365,120 A
`
`11/1884 Greene
`6/1887 DeLaval
`
`on inue
`(C t.
`
`d)
`
`.
`.
`Primary Examiner — Deborah D Carr
`(74) Attorney] Agent] or Firm , Cantor Cojbum LLP
`
`ABSTRACT
`(57)
`In one aspect of the invention, a method recovers oil from a
`concentrated byproduct, such as evaporated thin stillage
`formed during a dry milling process used for producing etha-
`nol. The method includes forming a concentrate from the
`byproduct and recovering oil from the concentrate. The step
`of forming the concentrate may comprise evaporating the
`byproduct. Further, the step of separating the oil from the
`concentrate may comprise using a centrifuge and, in particu-
`lar, a disk stack centrifiige. Other aspects of the invention
`include related methods and subsystems for recovering oil
`from thin stillage.
`
`2 Claims, 4 Drawing Sheets
`
`
`
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`
`SOLENIS EXHIBIT 2026
`
`Hydrite v. Solenis, IPRZO15-01592
`
`SOLENIS EXHIBIT 2026
`Hydrite v. Solenis, IPR2015-01592
`
`

`
`US 8,008,517 B2
`Page 2
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`GEA Westfalia Separator, Inc. and Ace Ethanol, LLC v. Greenshift
`Corporation, Case No. 09 Civ. 7686 (LMM) ECF Case, First
`Amended Complaint, received in U.S. District Court S.D.N.Y, Oct.
`13, 2009, pp. 1-36.
`GS Cleantech Corporation v. GEA Westfalia Separator, Inc.; Ace
`Ethanol, LLC; ICM, Inc.; Lifeline Foods LLC; and Does 1-30, Inclu(cid:173)
`sive, First Amended Complaint for Patent Infringement; Civil Action
`No. 09-cv-08642-SAS, filed Oct. 23, 2009, pp. 1-11.
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`
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`
`

`
`US 8,008,517 B2
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`
`

`
`US 8,008,517 B2
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`Preliminary Invalidity Contentions of Defendants ICM, Inc., Cardi(cid:173)
`nal Ethanol, LLC, Big River Resoruces Galva, LLC, Big River
`Resources West Burlington, LLC and Lincolnland Agri-Energy,
`LLC; filed in the United States District Court; Southern District of
`Indiana; Indianapolis Division; In Re: Method for Processing
`Ethanol Byproducts and Related Subsystems ('858) Patent Litiga(cid:173)
`tion; 1:10-ml-02181-LJM-DML; dated Jan. 24, 2011, 9 pages.
`Blue Flint Ethanol, LLC's Preliminary Invalidity Contentions; filed
`in the United States District Court; Southern District of Indiana;
`Indianapolis Division; In Re: Method or Processing Ethanol
`Byproducts and Related Subsystems ('858') Patent Litigation; Case
`No. 1:10-ml-02181-LJM-DML; Exhibits A-F included, dated Jan.
`24, 2011; 77 pages.
`Adkins Energy LLC' s Preliminary Invalidity Contentions; filed in
`the United States District Court, Southern District oflndiana, India(cid:173)
`napolis, Division, in re: Method of Processing Ethanol Byproducts
`and Related Subsystems ('858) Patent Litigation; Master Case. No.
`1:10-ml-02181-LJM-DML; Associated Case No. 1:10-cv-08004-
`LJM-DML; dated Jan. 24, 2011, 19 pages.; Exhibit A, pp. 1-14 and
`Exhibit B, pp. 1-146.
`Al-Corn Clean Fuels' Preliminary Invalidity Contentions; filed in the
`United States District Court; Southern District oflndiana; Indianapo(cid:173)
`lis Division; In Re: Method of Processing Ethanol Byproducts and
`Related Subsystems ('858) Patent Litigation; Master Case No. 1: 10-
`ml-02181-LJM-DML; Associated Case No.1:10-cv-08004-LJM(cid:173)
`DML, dated Jan. 24, 2011; pp. 1-16.
`Gea Westfalia Separator, Inc. and Ace Ethanol LLLC. 's Preliminary
`Invalidity Contentions, filed in The United States District Court for
`the Southern District of Indiana; Indianapolis Division; In Re:
`
`Method of Processing Ethanol Byproducts and Related Subsystems
`('858) Patent Litigation; 1:10-ml-02181-LJM-DML; filed Jan. 24,
`2011: 28 pages.
`Preliminary Invalidity Contentions by Lincolnway Energy, LLC;
`filed In the United States District Court, Southern District oflndiana;
`Indianapolis Division; In re: Method for Processing Ethanol
`Byproducts and Related Subsystems ('858) Patent Litigation; Master
`Docket: 1:10-ml-02181-LJM-DML; dated Jan. 24, 2011; 18 pages.
`Amaizing Energy Preliminary Invalidity Contention; filed in the
`United States District Court for the Southern District of Indiana;
`Indianapolis Division; In Re: Method of Processing Ethanol
`Byproducts and Related Subsystems ('858) Patent Litigation; Master
`Case. No. 1:10-ml-02181-LJM-DML; Associated Case No. 1:10-
`CV-08001-LJM-DML; dated Jan. 24, 2011; 16 pages.
`Iroquois Bio-Energy Company, LLC's Preliminary Invalidity Con(cid:173)
`tentions; filed In the United States District Court for the Southern
`District of Indiana; Indianapolis Division; In Re: Method for Pro(cid:173)
`cessing Ethanol Byproducts and Related Subsystems ('858) Patent
`Litigation; MDL Master Case No.: 1:10-ml-02181-LJM-DML;
`dated Jan. 24, 2011; 25 pages.
`Abstract of JP54064683A; published May 24, 1979, 1 page.
`Dominguez, H., et al. "Enzymatic pretreatment to enhance oil extrac(cid:173)
`tion from fruits and oilseeds: a review", Food Chemistry 49 (1994),
`pp. 271-286.
`Puertollano, et al., "Separation of the Oil and Protein Fractions in
`Coconut", J. Agr. Food Chem., vol. 18, No. 4, 1970, pp. 579-685.
`Rosenthal et al., "Aqueous and enzymatic processes for edible oil
`extraction", Enzyme Microb. Technol., vol. 19, Nov. 1, 1996, pp.
`402-420.
`Stanton, W.R., "Fermentation Assisted Byproduct Recovery in the
`Palm Oil Industry", Agricultural Wastes 6, (1983), pp. 31-63.
`Sweeten et al., "Removal and Utilization of Ethanol Stillage Con(cid:173)
`stituents" Energy in Agriculture, 1 (1981-1983), Elsevier Science
`Publishers B.V.; pp. 331-345.
`Digital Copy of a Book provided by Google-Thesis ofWINFIELD,
`Harriet The oil of maize (Zea mays); Library of the University of
`Wisconsin, New York, 1899; pp. 1-61.
`* cited by examiner
`
`

`
`U.S. Patent
`
`Aug. 30, 2011
`
`Sheet 1of4
`
`US 8,008,517 B2
`
`w-IOLE STI LLAGE
`II ME CHAN I CAL SEPARATION II
`MOISTURE CONTENT OF DISTILLERS WET GRAINS:
`SOLIDS CONCENTRATION IN THIN STILLAGE:
`MOISTURE CONCENTRATION IN SYRUP:
`GPM
`145
`118
`27
`
`TOTAL CAPACITY
`-TOTAL MOISTURE
`-TOTAL SOLIDS
`
`LBS/HR
`72,210
`58,702
`13,508
`
`CASE I
`11 BffORE 11
`65.0%
`6.70%
`80.0%
`
`DISTILLERS WET GRAINS
`LBS/HR
`GPM
`57.5 28,634
`TOTAL VOLUME
`MOISTURE:
`37.4 18,612 65.0%
`TOT AL SOLIDS 20.1 10,022 35. 0 7.
`
`7.
`
`THIN STILLAGE GPM
`LBS/HR %
`- - -
`TOTAL VOLUME 87.5 43,576
`80.5 40,D90 92.07.
`MOISTURE:
`OIL CONTENT: I. I
`566
`I. 307.
`SOLIDS:
`5.9
`2,92D G. 707.
`
`EVAPORATOR REMOVES
`2o, 146 LBS/HR OF WATER , OR
`GPM or WATER
`53
`8 50. 98 OPERATING COST ($/HR )
`
`SYRUP
`TOTAL VOLUME
`--------1 MOISTURE:
`OIL CONTENT:
`SOLIDS
`
`GPM
`35.0
`26.0
`I. I
`5.9
`
`LBS/HR
`17,430
`13,944
`566
`2,920
`
`%
`
`80.0%
`3.2 7.
`17.07.
`
`DRIED PRODUCT-HAVING 107. MOISTURE CONTENT (LBS/HR):
`MOISTURE TO EVAPORATE (LBS/HR):
`OR, IN GPM:
`FUEL REQUIRED IN DRYER (IN DECATHERMS):
`DRYER OPERATING COST @Ss.oo OECATHERM ($/HR):
`PRODUCT VALUE ($/HR):
`
`I S,009
`31,055
`62.4
`52.4
`s 262 .22
`$600.36
`
`

`
`U.S. Patent
`
`Aug. 30, 2011
`
`Sheet 2 of 4
`
`US 8,008,517 B2
`
`WHOLE ST ILLAGE
`11 MECHANICAL SEPARATION"
`MOISTURE CONTENT OF DISTILLERS WET GRAINS:
`SOLIDS CONCENTRATION IN THIN STILLAGE:
`MOISTURE CONCENTRATION JN SYRUP:
`GPM
`145
`118
`27
`
`TOTAL CAPACITY
`-TOTAL MOISTURE
`-TOT AL SOL! OS
`
`LBS/HR
`72,210
`58, 702
`13,508
`
`CASE I
`11AFTER 11
`65.0%
`6. 707.
`80 .07.
`
`DISTILLERS WET GRAINS
`GPM
`LBS/HR
`TOTAL VOLUME
`57.5 28,634
`MOISTURE:
`37.4 18,612 65.07.
`TOTAL SOLIDS 20.1
`I0,022 35.07.
`
`7.
`
`THIN STILLAGE
`TOT AL VOLUME
`MOISTURE:
`0 IL CONTENT :
`SOLIDS:
`
`GPM
`87.5
`80.5
`I. I
`5.9
`
`7.
`LBS/HR
`- - -
`43,576
`40,090 92. 0 7.
`5fifi
`J .307.
`2,920 6. 707.
`
`Ft9. 2
`
`SYRUP (LBS/HR):
`MOISTURE:
`MOISTURE (LBS/HR :
`OIL CONTENT (LB/HR):
`SOLIDS CONTENT (LBS/HR):
`
`I fi,892
`82.5%
`13 944
`28
`2,920
`
`EVAPORATOR REMOVES
`LBS/HR or WATER' OR
`2fi, 14&
`GPM or WATER
`53
`OPERA TI NG COST ($/HR)
`$SO. 98
`
`SYRUP
`TOT AL VOLUME
`MOISTURE:
`OIL CONTENT:
`SOLIDS
`
`GPM
`35.0
`28.0
`J.J
`5.9
`
`LBS/HR
`17,430
`13,944
`566
`2,920
`
`7.
`
`80. 0 7.
`3.2 %
`17.0%
`
`14
`
`....---------'
`OIL RECOVERED (LB/HR):
`OIL VALUE (8/HR)
`
`LBS/HR GPH
`538
`I. I
`$102
`
`10
`
`DRIED PRODUCT-HAVING 107. MOISTURE CONTENT (LBS/HR):
`MOISTURE TD EVAPORATE (LBS/HR):
`OR, IN GPM:
`FUEL REQUIRED IN DRYER (IN DECATHERMS):
`DRYER OPERATING COST @$5.00 DECATHERM ($/HR):
`PRODUCT VALUE ($/HR):
`
`14,41 I
`31,115
`62.S
`52.5
`$ 262. 73
`$576.46
`
`

`
`U.S. Patent
`
`Aug. 30, 2011
`
`Sheet 3 of 4
`
`US 8,008,517 B2
`
`WHOLE STILLAGE
`11 MECHAN!CAL SEPARAT!ON 11
`MOISTURE CONTENT OF DISTILLERS WET GRAINS:
`SOLIDS CONCENTRATION IN THIN STILLAGE:
`MOISTURE CONCENTRATION IN SYRUP:
`GPM
`145
`118
`27
`
`TOTAL CAPACITY
`-TOTAL MOISTURE
`-TOT AL SOL! OS
`
`LBS/HR
`72,210
`58,702
`13,508
`
`CASE 2
`11 BEFORE 11
`60.07.
`3.677.
`&0.07.
`
`DISTILLERS ~T GRAINS
`LBS/HR
`GPM
`56.9 26,325
`TOT AL VOLUME
`MOISTURE:
`34. J
`l&,995 &0.07.
`TOTAL SOLIDS 22.8 11,330 40.07.
`
`7.
`
`THIN STILLAGE GPM
`TOTAL VOLUME 88.1
`MOISTURE:
`63.7
`OIL CONTENT: 1.1
`SOLIDS:
`3.2
`
`LBS/HR J_
`43,885
`41,707 95.07.
`5&6
`1.30%
`l,&12 3.&7%
`
`EVAPORATOR REMOVES
`38,440
`LBS/HR OF WATER , OR
`77
`GPM OF WATER
`$ 74. 96
`OPERA TING COST ($/HR)
`
`SYRUP
`TOT AL VOLUME
`- - - - - MOISTURE:
`OIL CONTENT:
`SOLIDS
`
`GPM
`10.9
`6.6
`J. I
`3. 2
`
`.i.
`
`LBS/HR
`5,445
`3,267 60.0%
`5&6
`10.4%
`30 . 0 .i.
`I ,612
`
`DRIED PRODUCT-HAVING 107. MOISTURE CONTENT (LBS/HR):
`MOISTURE TO EVAPORATE (LBS/HR):
`OR, IN GPH:
`FUEL REQUIRED IN DRYER (IN DECATHERMS):
`DRYER OPERATING COST @$5.00 OECATHERM ($/HR):
`PRODUCT VALUE ($/HR):
`
`15,009
`16, 761
`37.7
`31. 7
`s 158.41
`$ 600.36
`
`Ft9. 3
`
`

`
`U.S. Patent
`
`Aug. 30, 2011
`
`Sheet 4 of 4
`
`US 8,008,517 B2
`
`WHOLE STILLAGE
`11 MECHANICAL SEPARATION"
`MOISTURE CONTENT OF DISTILLERS WET GRAINS:
`SOLIDS CONCENTRATION IN THIN STILLAGE:
`MOISTURE CONCENTRATION IN SYRUP:
`GPM
`145
`118
`27
`
`TOTAL CAPACITY
`-TOTAL MOISTURE
`-TOTAL SOLi OS
`
`LBS/HR
`72,210
`SB, 702
`13,SOB
`
`DISTILLERS WET GRAINS
`LBS/HR %
`GPM
`- - -
`56.9 28,325
`34. I 16, 995 60. 0 %
`22.B 11,330 40.0i.
`
`TOTAL VOLUME
`MOISTURE:
`TOTAL SOLIDS
`
`THIN STILLAGE
`TOTAL VOLUME
`MOISTURE:
`OIL CONTENT:
`SOLIDS:
`
`CASE 2
`11AFTER 11
`&O .O %
`3.67%
`&0.0%
`
`---43,885
`LBS/HR %
`
`GPM
`BB. I
`B3.7 41, 707 95.0%
`566
`J .30%
`I. I
`1,612 3.677.
`3.2
`
`a-o Q.
`
`:--l]rti
`
`0-'
`0
`
`EVAPORATOR REMOVES
`LBS/HR OF WATER, OR
`3B,440
`GPH or WATER
`77
`OPERATING COST ($/HR)
`874.%
`
`SYRUP
`TOTAL VOLUME
`MOISTURE:
`OIL CONTENT:
`SOLIDS
`
`GPH
`10.9
`fi .6
`J. I
`3.2
`
`7.
`
`LBS/HR
`5,445
`3,267 60. 07.
`10.47.
`566
`1,612 30. 07.
`
`4, 907 ---------c;'I
`SYRUP (LBS/HR):
`1 - - - - - - - - - - - ' - -o - t
`66.6%
`MOISTURE:
`MOISTURE (LBS/HR):
`3 26 7
`OIL CONTENT (LB/HR):
`28
`SOL IDS CONTENT (LBS/HR):
`1,612
`
`14
`
`______ ___,
`
`OIL RECOVERED (LB/HR):
`OIL VALUE ($/HR)
`
`LBS/HR GPM
`538
`J.1
`$ 102
`
`DRIED PRODUCT-HAVING 1D7. MOISTURE CONTENT [LBS/HR):
`MOISTURE TO EVAPORATE (LBS/HR):
`OR, IN GPM:
`FUEL REQUIRED IN DRYER (IN OECATHERMS):
`DRYER OPERA Tl NG COST @ $ 5. 00 DECA THERM ($/HR):
`PRODUCT VALUE ($/HR):
`
`14,411
`IB,821
`37.8
`31.B
`$158.92
`$576.46
`
`

`
`US 8,008,517 B2
`
`1
`METHOD OF RECOVERING OIL FROM
`THIN STILLAGE
`
`The present application is a Continuation Application of
`U.S. application Ser. No. 11/122,859, filed May 5, 2005, now
`U.S. Pat. No. 7,601,858, which claims the benefit of priority
`under 35 USC 119(e) to U.S. Provisional Application No.
`60/602,050, filed on Aug. 17, 2004, and is related to U.S.
`patent application Ser. No. 11/688,425, filed Mar. 20, 2007;
`U.S. patent application Ser. No. 12/475,830, filed Jun. 1,
`2009; U.S. patent application Ser. No. 11/241,231, filed Sep.
`30, 2005; and U.S. patent application Ser. No. 12/475,781,
`filed Jun. 1, 2009; all of which are incorporated by reference
`in their entireties.
`
`COPYRIGHT STATEMENT
`
`A portion of the disclosure of this document contains mate(cid:173)
`rial subject to copyright protection. No objection is made to
`the facsimile reproduction of the patent document or this
`disclosure as it appears in the Patent and Trademark Office
`files or records, but any and all rights in the copyright(s) are
`otherwise reserved.
`
`TECHNICAL FIELD
`
`The present invention relates generally to recovering oil
`and, more particularly, to recovering oil from a byproduct of
`the dry milling process used to form ethanol.
`
`BACKGROUND OF THE INVENTION
`
`Over the past thirty years, significant attention has been
`given to the production of ethyl alcohol, or "ethanol," for use
`as an alternative fuel. Ethanol not only bums cleaner than
`fossil fuels, but also can be produced using grains such as
`corn, which are of course renewable resources. At present,
`approximately sixty-nine "dry milling" plants in the United
`States produce over two billion gallons of ethanol per year.
`Additional plants presently under construction are expected
`to add over four hundred million gallons to this total in an
`effort to meet the current high demand.
`As noted in the foregoing discussion, a popular method of
`producing ethanol is known as "dry milling," and in the
`United States is typically practiced using corn. As is well
`known in the industry, the dry milling process utilizes the
`starch in the com or other grain to produce the ethanol
`through fermentation, and creates a waste stream comprised
`of byproducts termed "whole stillage" (which may be further
`separated into products known as distillers wet grains and
`"thin stillage"). Despite containing valuable oil, this whole
`stillage has for the most part been treated as waste and used
`primarily to supplement animal feed (mostly in the form of
`distillers dried grains with solubles (DDGS), which is created
`by evaporating the thin stillage, recombining the resulting
`concentrate or syrup with the distillers wet grains, and drying
`the product to have a low moisture content; see, e.g., U.S. Pat.
`Nos. 5,662,810 and 5,958,233, the disclosures of which are
`incorporated herein by reference).
`Efforts to recover the valuable oil from this byproduct have
`not been successful in terms of efficiency or economy. For
`example, one approach involves attempting to separate the oil
`from the thin stillage before the evaporation stage, such as
`using a centrifuge. However, spinning the thin stillage at this
`stage does not produce usable oil, but rather merely creates an 65
`undesirable emulsion phase requiring further processing.
`Moreover, the volume of thin stillage present is generally 2 to
`
`2
`10 times greater than the syrup, which requires considerable
`capital to purchase the number of centrifuges required.
`Together, these obstacles make attempts to recover oil from
`thin stillage highly inefficient and uneconomical.
`U.S. Pat. No. 5,250,182 (the disclosure of which is incor(cid:173)
`porated herein by reference) describes the use of filters for
`removing substantially all solids and recovering lactic acid
`and glycerol from the thin