US008008516B2
`
`(12) United States Patent
`Cantrell et al.
`
`(10) Patent N0.:
`(45) Date of Patent:
`
`US 8,008,516 B2
`*Aug. 30, 2011
`
`(54) METHOD OF PROCESSING ETHANOL
`BYPRODUCTS AND RELATED SUBSYSTEMS
`
`(76)
`
`Inventors: David Fred Cantrell, Lakemont, GA
`(US); David J. Winsness, Alpharetta,
`GA (US)
`
`( * ) Notice:
`
`Subject to any disclaimer, the term of this
`patent is extended or adjusted under 35
`U.S.C. 154(b) by 662 days.
`
`This patent is subject to a terminal dis-
`claimer.
`
`(21) Appl.No.: 11/241,231
`
`(22)
`
`Filed:
`
`Sep. 30, 2005
`
`(65)
`
`Prior Publication Data
`
`US 2006/0041153 A1
`
`Feb. 23, 2006
`
`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.
`(2006.01)
`CIIB 1/00
`(52) U.S. Cl.
`......................................................... .. 554/8
`(58) Field of Classification Search ..................... .. 554/8
`See application file for complete search history.
`
`(56)
`
`References Cited
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`Primary Examiner — Deborah D Carr
`
`(57)
`
`ABSTRACT
`
`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 centrifuge. Other aspects of the invention
`include related methods and subsystems for recovering oil
`from thin stillage.
`
`11 Claims, 4 Drawing Sheets
`
`CA5
`who|Ts‘fl1Iage
`"M chlnlcll sapmuan"
`
`
`
`
`
`SOLENIS EXHIBIT 2025
`
`Hydrite v. Solenis, IPRZO15-01592
`
`SOLENIS EXHIBIT 2025
`Hydrite v. Solenis, IPR2015-01592
`
`

`

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`Page 2
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`
`

`

`US 8,008,516 B2
`Page 3
`
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`
`

`

`US 8,008,516 B2
`Page 4
`
`Preliminary Invalidity Contentions of Defendants ICM, Inc., Cardi(cid:173)
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`Ethanol Byproducts and Related Subsystems ('858) Patent Litiga(cid:173)
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`
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`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", Enzyne 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 of Winfield,
`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 8,008,516 B2
`
`Whole Stillage
`"Mechanical Secaration"
`Moisture Content of Distillers Wet Grains:
`
`CASE 1
`"BEFORE"
`65.0%
`
`Solids Concentration in Thin Stlllage:
`
`Moisture Concentration In Syrup:
`
`6.70%
`
`80.0%
`
`Total Capacity
`
`• Totl!I Moisture
`
`• Totl!I Solids
`
`Distillers Wet Grains
`GPM
`57.5
`37.4
`
`Total Volume
`MoisbJre:
`
`Total Sollda
`
`20~1
`
`~
`145
`
`118
`rr
`
`Lbs/Hr
`
`72,210
`
`58,702
`
`13.508
`
`I\
`
`Thin Stillage
`
`Lbs/hr
`28,634
`18,812
`10,022
`
`_%
`
`65.0%
`35'1.
`
`Total Volume
`Moisture:
`OllContant
`Solids:
`
`GPM
`87.5
`80.5
`
`1.1
`5.9
`
`Lbs/hr
`43,576
`40,090
`566
`2,920
`
`°lo
`
`92°J.
`1.3•.(,
`6.70%
`
`l Syrup
`
`Total Volume
`Moisture:
`011 Content
`Sollds:
`
`Operating Cost ($/hr)
`
`GPM
`35.0
`28.0
`1.1
`5.9
`
`Lbs/hr
`17,430
`13,944
`566
`2,920
`
`D/o
`
`80.0%
`3.2"1.
`17°/o
`
`Dried Product· having 10% moisture content (lbs/hr):
`Moisture to Evaporate (lbs/hr):
`or, in GPM:
`Fuel Required in Dryer (in Decatherms):
`Dryer Operating Cost@ $5.00 Decatherrn ($/hr):
`Product Value ($/hr):
`
`15,009
`31,055
`62.4
`52.4
`$262.22
`$600.36
`
`Fig. 1
`
`

`

`U.S. Patent
`
`Aug. 30, 2011
`
`Sheet 2 of 4
`
`US 8,008,516 B2
`
`Whole Stillage
`"Mechanical Separation"
`Moisture Content of Distillers Wet Grains:
`Solids Concentration in Thin SUllage:
`Moisture Concentration in Svrup:
`GPM
`145
`118
`27
`
`Total Capacity
`·Total Molswre
`• Total Solids
`
`Lbs/Hr
`72,210
`58,702
`13,508
`
`I \
`
`CASE1
`"AFTER"
`65.0%
`6.70%
`80.0%
`
`GPM
`87.5
`80.5
`1.1
`5.9
`
`Lbs/hr
`43,576
`40,090
`566
`2,920
`
`~
`
`92%
`1.3%
`6.70%
`
`Evaporator Removes
`26,146
`Lbs/hr of Water, or
`53
`GPM of Water
`$50.98
`Openiting Cost IS/hr)
`
`Distillers Wet Grains
`GPM
`57.5
`37.4
`20.1
`
`Total Volume
`Moisture:
`
`Total Solids
`
`Thin Stillage
`
`Lbs/hr ~
`28,634
`18,812
`
`65.0%
`35%
`
`10,022
`
`Total Volume
`MoisWre:
`Oii Content
`Solids:
`
`+
`I
`~11~~
`10~
`"°•
`
`,,
`
`.
`
`i
`
`>II·~
`
`Svrup (lbs/hr):
`-Wre:
`MoisWnt (lbs/hrl:
`Oii ~ (lblhr):
`
`Solids Content (Ibo/hr):
`
`16 892
`112.5%
`13,944
`
`28
`
`2,920
`
`j
`
`·Ir
`
`+
`
`011 Recovered, lbs/hr :
`
`538
`
`1.1
`
`Dried Product. having 10% moisture content (lbs/hr):
`Moisture to Evaporate (lbs/hr):
`or, in GPM:
`Fuel Required in Dryer (in Decatherms):
`Dryer Operating Cost@ $5;00 Decatherm ($/hr):
`Product Value ($/hr):
`
`14,411
`31,115
`62.5
`52.5
`$262.73
`$576.46
`
`Fig. 2
`
`

`

`U.S. Patent
`
`Aug. 30, 2011
`
`Sheet 3 of 4
`
`US 8,008,516 B2
`
`Whole Stillage
`"Mechanical Separation"
`Moisture Content of Distillers Wet Grains:
`
`CASE2
`"BEFORE"
`60.0%
`
`Solids Concentration in Thin Stillage:
`
`Moisture Concentration in Syrup:
`
`3.67%
`
`60.0%
`
`Total Capacity
`
`-Total Moisture
`
`- Total Solids
`
`Distillers Wet Grains
`GPM
`56.9
`34.1
`22.8
`
`Total Volume
`Moisture:
`
`Total Solids
`
`GPM
`
`145
`
`118
`
`Lbs/Hr
`
`72,210
`
`58,702
`
`27
`
`13,508
`
`/\
`
`Thin Stillage
`
`Lbs/hr
`28,325
`16,995
`11,330
`
`~
`
`60.0%
`40"/,
`
`Total Volume
`Moisture:
`Oil Content
`Solids:
`
`GPM
`88.1
`83.7
`1.1
`3.2
`
`Lbslhr
`43,885
`41,707
`
`566
`1,612
`
`~
`
`95%
`1.J•t.
`3.67%
`
`GPMofWater
`Operating Cost ($/hr)
`
`Syrup
`
`Total Volume
`Moisture:
`Oil Content:
`Solids:
`
`GPM
`10.9
`6.6
`1.1
`3.2
`
`Lbs/hr
`5,445
`3,267
`566
`1,612
`
`%
`
`60.0%
`10.4°/111
`30°/o
`
`Dried Product· having 10% moisture content (lbs/hr):
`Moisture to Evaporate (lbs/hr):
`or, in GPM:
`Fuel Required in Dryer (in Decathenns):
`Dryer Operating Cost @ $5.00 Decatherm ($/hr):
`Product Value ($/hr):
`
`Fig. 3
`
`15,009
`18,761
`37.7
`31.7
`$158.41
`$600.36
`
`

`

`U.S. Patent
`
`Aug. 30, 2011
`
`Sheet 4 of 4
`
`US 8,008,516 B2
`
`Whole Stillage
`"Mechanical Separation"
`Moisture Content of Distillers Wet Grains:
`Sollds Concentration in Thin Stlllage:
`Moisture Concentration in Syrup:
`GPM
`145
`118
`27
`
`Total Capacity
`-Total Moisture
`-Total Solids
`
`Lbs/Hr
`72,210
`58,702
`13,508
`
`I \
`
`CASE2
`"AFTER"
`60.0%
`3.67%
`60.0%
`
`GPM
`88.1
`83.7
`1.1
`3.2
`
`llil!1!
`43,885
`41,707
`
`666
`1,812
`
`'.'!!
`
`95%
`
`1.3%
`3.67%
`
`Evaporator Removes
`38,440
`Lbs/hr of Water, or
`77
`GPM of Water
`$74.96
`Operating Cost ($/hr)
`
`.b!l.!!l!1r
`5,445
`3,267
`
`666
`1,612
`
`~
`
`60.0%
`10.4%
`30%
`
`GPM
`10.9
`8.6
`1.1
`3.2
`
`I~
`
`Thin Stillage
`
`Total Volume
`Moisture:
`Oil Content
`Solids:
`
`+
`
`D«v '0-+
`
`.
`
`...
`'<II+
`Syrup
`Total Volume
`Moisture:
`Oil Content
`SOiids:
`
`Distillers Wet Grains
`~ Lbs/hr
`56.9
`28,325
`34.1
`18,995
`22.8
`11,330
`
`Total Volume
`Moisture:
`
`TabllSaHdll
`
`Syrup (lbs/hr):
`Moisture:
`Moisture (lbs/hr):
`Oii Content (lblhrl:
`
`Solids Co-.. (lbolluj:
`
`j
`
`.
`
`'.'!!
`
`60.0%
`40•1.
`
`4 907
`66.6%
`3,267
`
`28
`
`1,812
`
`+
`
`'. ··:U:ialhr ,
`:538
`-:0_1_11R_e_c_ov._· .-ce-re-d-.::_.l_,b_sl_.h_t_:_·c -: ._J
`Oil Value $/hr :
`$102 ·
`
`:•GPll ..
`·1 ,'1
`
`Dried Product· having 10% moisture content (lbslhr):
`Moisture to Evaporate (lbs/hr):
`or, in GPM:
`Fuel Required in Dryer (in Oecatherms):
`Dryer Operating Cost@ $5.00 Decatherm ($/hr):
`Product Value ($/hr):
`
`14,411
`18,821
`37.8
`31.B
`$158.92
`$576.46
`
`Fig. 4
`
`

`

`US 8,008,516 B2
`
`1
`METHOD OF PROCESSING ETHANOL
`BYPRODUCTS AND RELATED SUBSYSTEMS
`
`This application is a continuation of U.S. patent applica(cid:173)
`tion Ser. No. 11/122,859, filed May 5, 2005, now U.S. Pat.
`No. 7,601,858 which claims the benefit of U.S. Provisional
`Patent Application Ser. No. 60/602,050, filed Aug. 17, 2004,
`the disclosures of which are incorporated herein by reference.
`
`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
`undesirable emulsion phase requiring further processing.
`Moreover, the volume of thin stillage present is generally 2 to
`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
`
`2
`removing substantially all solids and recovering lactic acid
`and glycerol from the thin stillage without the need for evapo(cid:173)
`ration. Despite eliminating a step in the conventional process,
`the proposal results in a more complicated arrangement
`requiring multiple filtration steps. Wholesale elimination of
`the evaporator in the vast majority of existing plants is also
`unlikely and otherwise uneconomical. Filters, and especially
`the microfiltration and ultrafiltration types proposed in this
`patent, are also susceptible to frequent plugging and thus
`10 disadvantageously increase the operating cost. For these rea(cid:173)
`sons, the filtration process proposed in this patent has not
`gained widespread commercial acceptance.
`Accordingly, a need exists for a more efficient and eco(cid:173)
`nomical manner of recovering oil from a byproduct contain-
`15 ing it, such as thin stillage created during the dry milling
`process used to produce ethanol.
`
`SUMMARY OF THE INVENTION
`
`25
`
`20
`
`In accordance with one aspect of the invention, a method of
`processing a concentrated byproduct of a dry milling process
`for producing ethanol, such as by using com, is disclosed. In
`its most basic form, the method comprises recovering oil
`from the concentrated byproduct.
`In one embodiment, the byproduct comprises thin stillage,
`and the method includes the step of evaporating the thin
`stillage to form a concentrate. The recovering step may fur(cid:173)
`ther comprise separating the oil from the concentrate using a
`disk stack centrifuge. Preferably, the recovering step com-
`30 prises: (1) providing the concentrated byproduct at a tempera(cid:173)
`ture of between about 150 and 212° F. and, most preferably, at
`a temperature of about 180° F.; and/or (2) providing the
`concentrated byproduct having a pH of between about 3 and
`6 and, most preferably, between about 3.5 and 4.5. Addition-
`35 ally, it is preferred that the concentrated byproduct have a
`moisture content greater than 15% by weight, more prefer(cid:173)
`ably a moisture conte