111111
`
`1111111111111111111111111111111111111111111111111111111111111111111111111111
`US 20070238891Al
`
`(19) United States
`c12) Patent Application Publication
`Winsness et al.
`
`(10) Pub. No.: US 2007/0238891 A1
`Oct. 11, 2007
`(43) Pub. Date:
`
`(54) METHOD OF FREEING THE BOUND OIL
`PRESENT IN WHOLE STILLAGE AND THIN
`STILLAGE
`
`(76)
`
`Inventors: David J. Winsness, Alpharetta, GA
`(US); John W. Davis, Chesapeake
`Beach, MD (US); Gregory Paul
`Barlage, Sandstron, VA (US); David
`Fred Cantrell, Lakemont, GA (US)
`
`Correspondence Address:
`KING & SCHICKLI, PLLC
`247 NORTH BROADWAY
`LEXINGTON, KY 40507 (US)
`
`(21) Appl. No.:
`
`111688,425
`
`(22) Filed:
`
`Mar. 20, 2007
`
`Related U.S. Application Data
`
`(63) Continuation of application No. PCT/US07/62301,
`filed on Feb. 16, 2007.
`
`(60) Provisional application No. 60/773,947, filed on Feb.
`16, 2006.
`
`Publication Classification
`
`(51)
`
`Int. Cl.
`(2006.01)
`CllB 1104
`(52) U.S. Cl. ................................................. 554/8; 134/105
`
`(57)
`
`ABSTRACT
`
`A method is provided for recovering oil from stillage
`including oil resulting from a process used for producing
`ethanol. In one embodiment, the method includes heating
`the stillage to a temperature sufficient to at least partially
`separate, or unbind, the oil therefrom The method further
`includes recovering the oil from the stillage.
`
`Whole Stillage
`""Mechanical Separaticn"
`Modtunl Contl!ll1't cf Oi&ID'-nli Wet Gnains:
`Solldl Cant::mrtnditxl in Thin Stillage:
`
`CA5E 1
`"BEFORE"
`6.5.1!1'1.
`
`6..70%
`
`80.0%
`
`-
`
`-"'""""'""lnltionin5Yf11!1:
`GPM
`146
`
`Totol c.p.c1ty
`-T-1 . . . . .
`
`,,
`
`zr
`
`~.
`
`IJ!..off
`Tl,2.1D
`
`!ii,7D2
`
`.,.,....
`
`IThin Stillage
`
`1\
`
`-'Tol:al5obill
`
`Tata!Valu11110
`
`DistlHers Wet Grains
`!!!!!!!
`57.5
`37-4
`
`, ... _ 211.1
`-
`
`~r !.
`211,634
`,....,
`.....
`11,-12
`
`S5.0%
`
`Total 111Diurne:
`llai5:a.:
`aoc-
`-~
`
`~ ~ ~
`87.5
`43.575
`,.,..
`""""
`IUl5
`1.1
`S.7D%
`
`...
`
`......
`...
`"""'
`
`.
`
`211,146
`53
`$50.98
`
`..,..,,rw.mr.ar
`
`GPMafw.t.r
`~Cm;:t{Mn1
`
`~
`. '
`I [1
`d~~----
`L ~
`··~· l
`
`,_
`
`~ ~ :!!
`17,430
`35.0
`,..
`,_,
`21.0
`,.,.
`
`B-D.D%
`
`, ..
`'""
`
`Syrup
`
`Total Volume
`--~;
`Ollr-atriii:D±:
`locolildl::
`
`..
`
`Orit!rl Pmdoct -hawi-ng 1 O"k mmmlll!! com:ent (lbslhr):
`Moiftll"l!IDE~(~rj:
`ar, ill GPM:
`Fuol ~ in tlryo< {in Do=tllemls~
`01y« o,..mtmg Cost@ SS.DO Oecalhorm {S/llr):
`?rnduciVdueiS!nj:
`.
`
`15,009
`31,055
`GUo
`S:U
`$262.22
`$600.31!
`
`SOLENIS EXHIBIT 2001
`Hydrite v. Solenis, IPR2015-01592
`
`

`
`Patent Application Publication Oct. 11, 2007 Sheet 1 of 10
`
`US 2007/0238891 A1
`
`Whole Stillage
`"Mechanical Se!laration"
`Momull! Cllniloni of DistllleB Wet G.-..ins:
`Solidi Contenlmlion in Thin 511\lage:
`Moistu">.e-:-tration in Sytup:
`GPM
`146
`1'111
`
`~-
`
`J.il!ll:lr
`77,2111
`
`li~,7112
`
`-
`Total c..p.city
`-l··~
`
`-T-I.oilk
`
`CA-sE 1
`"BEFORE"
`65.0%
`
`G.70%
`
`BO.O%
`
`ZT
`
`1l,!lllll
`
`/\
`
`Thin Stillage
`
`Distillers Wet Grains
`GPIIIl
`57.5
`37.4
`21!.1
`
`T fltal VoiUI'III!
`
`--.., T--
`
`l:!!:!!!!!:
`ZB,634
`11,81:
`'111.11%2
`
`~
`
`Sfi.O%
`35"JJ.
`
`Total Volume
`-..,
`Dla.allf:
`llaMds:
`
`~ Jdl!l!![
`87.5
`43,576
`&115
`.0,111(1
`1.1
`5..8
`
`li&li
`:2,!12!1
`
`~
`
`1!2:"1.
`1.:J'l'.
`li.70%
`
`1
`[1 . • 26,146
`D~~·---
`c~, l
`
`..
`
`"""'"'W..•.m
`GPM ofWat!!r
`o,..r-.u Cod: ISIIn1
`
`53
`$5(1.98
`
`Syrup
`
`Total Volume
`
`-..,
`
`Dlleon..t
`
`-=
`
`~
`35.0
`2&J!
`1..1
`53
`
`:'61.
`
`L..hsft'lr
`17,430
`llO.O%
`T.l.M4
`~ 1..!1"1.
`11"1.
`%.1m
`
`Dried Produe! - ha\'ing 1 D"k moimJre conu:nt (lbslhrl:
`Moi.nure 11> E.WipO<W1!! (ll>slllr):
`or, in GPM:
`Fuel RaqWr.l in llrye' (in ~s}:
`DTyer Opln!ing Cost@ 55.00 OecatiJelll (Sihrl:
`Product V.._ CSlbrj:
`
`15,009
`31,1155
`62,...4
`5:'l.A
`$262.22
`5600.31!
`
`Fig. 1
`
`

`
`Patent Application Publication Oct. 11, 2007 Sheet 2 of 10
`
`US 2007/0238891 A1
`
`CJ"SE 1
`RAFTER"
`BS.IY/U
`5.7m~
`UO.O%
`
`Tam!~
`
`Whole Stillage
`RMechanical Separation"
`c-aant at DiRtiiMn; I'IIM Gmi=
`-
`Solids~ 1n lbin:stll._:
`Maistuno Canarntnsllan In SYTlJll;
`~ ~
`14S
`7'2,210
`111
`~TOZ
`13,11011
`71
`
`·T--
`·T"""'-
`
`Totld Volume _,
`, .... _
`
`\Distillers Wet Gralns
`liPM ~ :1!!
`57.5
`2li,&:W
`111,1112.
`'D.A
`2!1.1
`
`66.0%
`:11:1'!;
`
`1D,IIZ!
`
`1\
`_,
`lllleonwrt: -
`
`Tllilll Volmne
`
`~~=------------------,
`Thln Stillage
`~ .1l!
`4:1,576
`,,.,.,
`.til,-
`6.70%
`
`~
`87.5
`8IUI
`
`1.1
`u
`
`...
`
`2.120
`
`11%'11
`
`/d.
`
`/0
`
`1B.Il92
`o::z.mlo
`18,M4
`
`..
`
`:z.am
`
`S}lrup (lbs/hrl:
`_ ,
`-~~
`~--
`
`~--.,_-
`
`1
`
`1
`
`on.! f>TDduct- homo; 11J'l\o ~ .... I'UillBnt !Jirnlltr):
`
`-in ~(ll>slltrj:.
`
`«, tn.GPM;:
`Fuel~ i<t Dryoor (In Oe=:!ln~i'
`o.y.. 0~ Colt 4!l S!iJJO Ollcltham (51111'):
`l'mdul:% v-..IS/IIrt:
`
`Fig. 2
`
`HEATING SYSTEM
`
`1.1
`
`14,.411
`~1.115
`112.5
`li2.S
`$262.7.3
`$576.-46
`
`

`
`Patent Application Publication Oct. 11, 2007 Sheet 3 of 10
`
`US 2007/0238891 A1
`
`Whole Stillage
`"Mechanical Separation"
`~ Canlt!nt cf Cisi!llon Wl!t Gndns=
`
`Salicl& C<>ncentrrion in Thin Stillage:
`
`Maimll'!! ~tr.ditln In Syrup:
`m!!
`148
`
`~aral~
`-Torlal-
`
`LboiHr
`
`72,210
`
`51.7ln
`
`-CASE 2
`"BEFORE"
`60.0%
`3.67%
`
`50.0%
`
`118
`
`Tl
`
`-T<*illcllid:ll
`
`TDtlll Volume -T_._
`
`Distillers Wet Grains
`GPM ~ ~
`56.9
`21,325
`a4.1
`111,ft5
`Z2.ll
`
`50.0%
`
`1:1,50a 1\
`-1'1,1117 -
`11;1311 -
`-
`l
`[1 . :__.,
`IT~~--~·-
`'~ 1
`
`i
`
`Thin Stillage
`
`Total Votunw
`-..,
`
`OIIC:U.O..:
`
`Sif!'!'!
`BB.1
`111
`1.1
`:1.2
`
`Llmlhr.
`C,IIB5
`
`~
`
`!Ia
`1$12
`
`1.3%
`3.67%
`
`38,44D
`77
`$74.96
`
`Lbolhr ofWall!r. or
`GPM af Walar
`~c.m:l$lbrl
`
`~
`
`h!!!!!:!r.
`5,445
`~ 60.0%
`
`- "''P.oll%
`
`1$12
`
`311%
`
`Syrup
`
`Total Volum"
`-...,
`
`011~
`llalkls:
`
`~
`10.9
`lUI
`1-1
`3.2
`
`•
`
`Dried Pt'Ddua • hmng 10'% mot.lul'!! contl!flt {lbolhrj:
`Moilri:!Jre ID Ev~ {ibd>r):
`m, in GPM:
`Fiiei Requi<ed in Dcyoo" (in Oe=ftH!nmr):
`Dryer OpemliJlg Co~ !;g 5&.00 Ol=dllmm ($/IU):
`Prnduct VIIU!! (:ilbfl:
`
`15,009
`18,7!11
`:rr.7
`3~.7
`$158.41
`$600.36
`
`Fig. 3
`
`

`
`Patent Application Publication Oct. 11, 2007 Sheet 4 of 10
`
`US 2007/0238891 A1
`
`Whole Stillage
`"Mechanical Separation"
`MaiJI;IIJm ~ or 01st111e1s w.t Gnllta;:
`Bolld!l ~ in Tltin st!JUQa:
`IADimml c
`wntlcn in SlfRIC:
`!!!!!!!
`141i
`118
`XI
`
`T,._l~
`
`·T--
`
`·T-IkiiiJia
`
`CASE 2
`"AFTER•
`SC,IJ%
`J,lfT'/o
`ea.. a%
`
`l.l!!!!:!!
`T.I,::'IC
`111!,71>2
`
`Distillers Wet Grains
`2f!!ll
`5B.9
`31..1
`21.11
`
`Total VoQn!! -, ___
`
`U>sillr ~
`2B,JZii
`,.,_
`RO.!I%
`,,~ '"""
`
`Total Voiune
`
`00.,.,._..,
`
`~~.!IIlii 1\
`_,
`-
`
`~----------------------------
`Thin Stillage
`.%
`
`~ bl!!n!r
`43,886
`88.1
`111.7
`41,:ro7
`
`~~
`
`1.1 - 1.3'1.
`
`:u
`
`1,8:'12
`
`3.67%
`
`Syrup
`Tota!Voimne
`
`-Dl.,_,
`
`~ .Y!!1!!!
`10.9
`5~
`
`!!
`
`GO.O%
`
`._.,__,
`
`~rup llbs/hrl: --~ .. -~
`1
`
`"'
`
`4,907 _.,.
`..
`
`:1.31
`
`1,1112.
`
`1
`
`O!icl Pmducl:-~ 11:1'4 lb>lstu.,. =nt.oort (IDs.llrr):
`_ . . , ~(Jmilnl:
`Df,ln GPM:
`Fual R.ooquind in Drl-1' (lnllt<:Sft"m''=l!
`Do-yoor 0~ CMt@ Ri..DD ~ ($/llrj:
`Pn>duCt V-IS'hrt:
`
`14,411
`11l,SZ1
`:17'.8
`l!1.B
`$158.92
`$576..46
`
`Fig. 4
`
`

`
`Patent Application Publication Oct. 11, 2007 Sheet 5 of 10
`
`US 2007/0238891 A1
`
`Fig. 5
`
`HEATING SYSTEM (optional) 1---- 24
`1
`""
`
`RAW MATERIAL
`011
`Selle•
`lwa1et
`
`l!.3"11.
`
`111.::1'1.
`
`lb!llnr
`200,000
`4,600
`32,620
`162.560
`
`50 mmgy Ethanol Plant
`
`lbslhr
`
`!-""'""'
`
`lbnlllr
`tJB,35!i
`
`1
`·~
`L-------------~~~D~·~~~·~~~r~L~Iq~u~lo~------~1:3B~·~3S~9j ---.....
`
`j
`
`lbslhr
`61,841
`3,34H
`23,160
`35138
`
`Ol11tU1an Wat Gnins
`Olt
`~.~"-
`:n.M'i.
`57,m;.
`
`lbslhr
`1JB,359
`1,454.4
`Q,-4430
`1:t1,4d4
`
`'-"'
`lUI....
`VJ.1~
`
`}d.,
`
`lbalhr
`101.m
`
`IViat~rEvttDIIrn;Bd
`
`1---------+1 ~
`1'-'~t1'~
`r
`,-r..lft
`
`HEATINii SYSTEM (uptlllnlll)
`
`I Corn 011
`
`llll'lihr
`1.309
`
`HEATING SYSTEM (optional)
`
`-
`
`L - - - - - - - - - ' lbslhr
`12,9().4
`Canal ....... n .... .,.
`011
`146.4
`c,J07
`Solid•
`Walor
`6,452
`
`,,,.,.
`••·""'
`50-""
`
`;E~v~a~o~o~rnwto~r~~~~----~~~b~·~'h~r----.r
`
`jw..ur£vnocrnlntl
`
`19.014
`
`l,
`
`Wrat Gr.~ ina+ Svrup
`011
`:l.nr,..
`Sc!ict~
`Watar
`
`:ll.J~
`
`""'~
`~
`~ =n
`I 8
`+~~ L.J
`1)'1
`l\ C=-,;;:q(
`+
`POG5
`011
`Scild.s
`Waier
`
`"~
`~:ll'JI.
`
`'-""'
`
`lbs/hr
`98.011
`~.401
`32,620
`41!,317
`
`Drver
`lwatt~r £!\lnPtJI"ii!Da
`
`4l,177
`
`lbslhr
`J9.251
`3,491
`32,6:!0
`3 140
`
`OP'ERATING CCS'r.5
`
`'"'"u~l P,:q:uuw~ By D~r IOI!ci!·urrtn!l)
`Op!lnllttn:} Cell" Ddt na.Jr m s.!JDatauumn
`KWH r~u•1111a"'' Ds:.anlf!l . .-1 100 tarl':Jih.Jl)t
`Ou.Biflg Ccn MtiH:t.rDI S.D~K~
`FLHI~ RI!QUimd By EVIItDWII (l)~JCGtnii1TIIII
`
`OiJolril~ G;l:q ;H'rnDUrol1 ~rm
`.tcttl Dtw~r:!itnr: C01.! ~l/111"'1
`
`7J.Il
`
`34UI
`
`!!!U
`
`Slllr
`
`::11101
`
`317.0~
`
`~
`rr=
`
`fmcud V11.h.1u
`
`00351C-atl•c1y!
`
`\l~lil~ e.tS7C."':Cn
`c.c:m o~ !C:.aP•dfl
`VIUMJ at s:JCIDI1nn
`
`l>llilr
`311~1.1
`
`llO!.Il
`
`lllir
`
`H.:rn.t;
`
`~
`
`lat~IVIIU111Jnt1
`
`n.!!TtL1~
`
`

`
`Patent Application Publication Oct. 11, 2007 Sheet 6 of 10
`
`US 2007/0238891 A1
`
`Fig. 6
`
`RAIN MATERIAL
`011
`5 ell d5
`111/otsr
`
`~ ...
`ID.OI"o
`
`B1.J'-'
`
`t
`
`lbslhr
`200,01][)
`4,BCO
`32,620
`1il:?,sac
`
`50 mmgy Ethanol Plant
`
`tb.slhr
`JlrWrnlt~Em=u~a~ln~n--------~5~,~81~~~~---------------,
`
`,, -----~] I~=-·~··;·:·~--';;
`
`lbslhr
`...............
`lc;"-"'-;..;,__::..;_ __ ~!iB~.=S"l~1~1
`
`Wul! Wmr
`a
`73,9701
`fLowOileo-rt""
`,
`lb9/lu
`r.:o"'J•'"'H'"LI,..a=n~w=at:-:G"'n=l~n=.---'---.6~1Fi,64itt1;--l · - - - - - - - -
`l!
`011
`....
`3,346
`~.Jrlllo
`SoUds.
`2J,1SD
`-+JW.,.hWat.rR•wm
`1 I
`Wa!!or
`"'·"""
`35.138
`(-·--··--·--;~-~ :
`
`77.4711
`
`t=====:l:tm:l:h:r===:_ ______ _j
`
`VllotGnin• + Wuh Wat&r
`au
`aY.
`Solltis
`11.1"'
`Wotllr
`llll.11'110
`
`135,611
`:J,34G
`2:1,160
`1CB,105
`
`I
`
`!:Thin ll!Uiage
`on
`SoiiO•
`I W•mr
`
`2.1.,.
`e.711
`gt:>%
`
`141,BBDJ
`~n:5e.a
`9,460
`129.440
`
`.
`
`2 Phaso DOlCDnlor-
`
`:
`
`! ---- /;f.
`~
`________.~-- -~~~r------ .l~r~~ ,.,.....,,_=·--~ltm;;::;lhiii;ri"'l
`I r l![Wo~ta'!:!.r..=E:!!•·~]JO!li!!:!!!:::IIIII~----='.::;DD:.:•.:.46"-1'-'
`w .. h.d "'Wat G.......
`l 8'
`l
`"t .....
`
`011
`Solids
`W-Atft:r
`
`1.2i'o
`'"·""
`n.l:rli.
`
`5H,140
`1,1140
`2:1,1 80
`3:!,1.40
`
`ltmlhr
`r.~~~~-~~n~mw~= •• -.---741~.~39~9~
`m
`'·'"'
`2ese.g
`Solid>
`"-""
`9,460
`28.979
`7DD%
`Wa~r
`
`24
`
`HEATING SYSTEM (option"l)
`
`lba/hr
`99,539
`l,\~6
`J~.620
`92.119
`
`Drver
`/WaLOr E'l,f;lpcrnUJd
`
`56,QS7
`
`lbslhr
`37,776
`2,138
`32,!!20
`3,022
`
`!Corn 011
`
`ID.sihr
`2.664
`
`!Woo Grains ~ 5yrup
`~'"
`Oil
`Solido
`:!l.ll~
`Water
`M.t'Ki
`
`l
`~f$bl1J">
`~o'U
`.. ~,.
`rOGS
`ou
`'·""
`Sollos
`Wnter
`
`a.~
`
`jo,ORATING COm
`
`FIJ•I ftaqurtd By O.ryw {0-CIIil.-m.~l
`OPdi"'DilQ co:~ par I'Qlf.; :l.51Dtra:ltrtellm
`KWt-lrMOUnc!'l;:f~l'-II.WC~I
`CpetRr~Q: ~n PH ra..uml.~
`"Fva!li.KI'tllfl~ By :n.ID'ItW (Oae~tnMmt'
`O!XI"'~n;l~ pMil:IUrlii:l~rm
`T.atat O~ntrllg CDW~ !M1J1
`
`!]g.IJ
`
`=·
`
`$~
`
`Jllll
`
`J.lll92T
`
`l:!lA!
`
`u=
`
`U11!..i.5
`
`Pmduct V-llltUI'
`
`DCGEiiiC..a•at't1
`
`'.'al\laGII-IUI;YWl1
`C::ctttOIIIC-an.l£:1t.;l
`Vlllld lil,flllOJ\Dr1
`
`UWlll
`:lmu
`
`:m•:u
`
`llnr
`
`~~.l:::..:;!4
`
`~
`
`Totlll,/•111111 IL'hr'J
`
`11,Tl"UJ
`
`

`
`Patent Application Publication Oct. 11, 2007 Sheet 7 of 10
`
`US 2007/0238891 A1
`
`Fig. 7
`
`RAW MATERIAl.
`011
`Solids
`Walor
`
`:to%
`
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`

`
`Patent Application Publication Oct. 11, 2007 Sheet 8 of 10
`
`US 2007/0238891 A1
`
`Fig. 8
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`50 mmgy Ethanol Plant
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`
`Patent Application Publication Oct. 11, 2007 Sheet 9 of 10
`
`US 2007/0238891 A1
`
`• -u.
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`

`
`Patent Application Publication Oct. 11, 2007 Sheet 10 of 10
`
`US 2007/0238891 A1
`
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`

`
`US 2007/0238891 AI
`
`Oct. 11, 2007
`
`1
`
`METHOD OF FREEING THE BOUND OIL
`PRESENT IN WHOLE STILLAGE AND THIN
`STILLAGE
`
`[0001] This application is a continuation of International
`Application PCT/US07/62301, filed Feb. 16, 2007, which
`claims the benefit of U.S. Provisional Patent App. Ser. No.
`60/773,947, filed Feb. 16,2006, the disclosures of which are
`both incorporated by reference.
`
`COPYRIGHT STATEMENT
`
`[0002] A portion of the disclosure of this document con(cid:173)
`tains material 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 copy(cid:173)
`right(s) are otherwise reserved.
`
`TECHNICAL FIELD
`
`[0003] The present invention relates generally to recover(cid:173)
`ing oil from corn and, more particularly, to recovering oil by
`freeing the bound oil present in byproducts of a process used
`to produce ethanol.
`
`BACKGROUND OF THE INVENTION
`[0004] 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 burns cleaner
`than fossil fuels, but also can be produced using corn, a
`renewable resource. At present, more than sixty-nine "dry
`milling" plants in the United States produce billions of
`gallons of ethanol per year. Additional plants presently
`under construction are expected to add hundreds of millions
`gallons to this total in an effort to meet the current high
`demand.
`
`[0005] As noted in the foregoing discussion, a popular
`method of producing ethanol from corn is known as "dry
`milling." As is well known in the industry, the dry milling
`process utilizes the starch in the corn to produce the ethanol
`through fermentation, and creates a waste stream comprised
`of byproducts termed "whole stillage" (which may be fur(cid:173)
`ther separated into products commonly referred to as "dis(cid:173)
`tillers wet grains" and "thin stillage"). Despite containing
`valuable oil, these byproducts have for the most part been
`treated as waste and used primarily to supplement animal
`feed. This feed is mostly distributed in the form of distillers
`dried grains with solubles, 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 moisture content ofless than about 10% by weight.
`
`[0006] Efforts to recover the valuable oil from these
`byproducts 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 is
`generally 2 to 10 times greater than the syrup, and thus
`involves a considerable capital requirement to purchase the
`number of centrifuges required. Together, these obstacles
`make attempts to recover oil from corn thin stillage prior to
`evaporation highly inefficient and uneconomical.
`
`[0007] U.S. Pat. No. 5,250,182 (the disclosure of which is
`incorporated herein by reference) describes the use of filters
`for removing substantially all solids and recovering lactic
`acid and glycerol from the thin stillage without the need for
`evaporation. Despite eliminating a step in the conventional
`process, the proposal results in a more complicated arrange(cid:173)
`ment requiring multiple filtration steps. Wholesale elimina(cid:173)
`tion of the evaporator in the vast majority of existing plants
`is also unlikely and otherwise uneconomical. Filters, and
`especially the microfiltration and ultrafiltration types pro(cid:173)
`posed for use in this patent, are also susceptible to frequent
`plugging and thus deleteriously increase the operating cost.
`For these reasons, the filtration process proposed in this
`patent has not gained widespread commercial acceptance.
`
`[0008] Accordingly, a need exists for more efficient and
`economical manners of recovering oil from byproducts
`created during the production of ethanol.
`
`SUMMARY OF THE INVENTION
`
`[0009]
`In one aspect of the invention, a method of recov(cid:173)
`ering oil from stillage including oil resulting from a process
`used for producing ethanol is provided. The method com(cid:173)
`prises heating the still age to a temperature sufficient to at
`least partially separate the oil therefrom. The method further
`comprises recovering the oil from the stillage.
`
`[0010]
`In one preferred embodiment, the heating step
`comprises heating to a temperature above 212° F. and the
`method further includes the step of pressurizing the heated
`stillage to prevent boiling. More preferably, the heating step
`comprises heating to a temperature of about 230° F., but less
`than about 250° F. In any case, the pressurizing step pref(cid:173)
`erably includes maintaining a pressure on the stillage of at
`least a vapor pressure necessary to allow the stillage to reach
`the desired temperature for separating at least part of the oil
`without boiling the stillage. Most preferably, the method
`includes the step of allowing the stillage to return to atmo(cid:173)
`spheric pressure after the heating and pressurizing steps but
`before the recovering step.
`
`[0011]
`In the foregoing or other embodiments, the recov(cid:173)
`ering step comprises separating the oil from the stillage
`using gravity separation. Preferably, the step of using gravity
`separation includes passing the stillage through a centrifuge
`or delivering the stillage to a settling tank.
`
`[0012]
`In still other embodiments, the heating step com(cid:173)
`prises passing the stillage through at least two heat exchang(cid:173)
`ers in series. The method may her include the step of cooling
`the stillage after the heating step and before the recovering
`step. Preferably, the cooling step comprises cooling the
`stillage to a temperature of less than 212° F. It is also
`preferable for the method to include the step of elevating the
`pressure of the stillage to above atmospheric pressure prior
`to the heating step. In any case, the method may further
`include the step of cooling the stillage and allowing the
`stillage to return to atmospheric pressure prior to the recov(cid:173)
`ering step. Alternatively, the method may further include the
`step of elevating the pressure of the stillage to above
`atmospheric pressure prior to the heating step and recover(cid:173)
`ing oil from the stillage at the elevated pressure.
`
`[0013]
`In accordance with another aspect of the invention,
`a system is provided for recovering oil from pressurized
`stillage resulting from a process used for producing ethanol.
`
`

`
`US 2007/0238891 AI
`
`Oct. 11, 2007
`
`2
`
`The system comprises a first heater for receiving and super(cid:173)
`heating the pressurized stillage. The system further com(cid:173)
`prises a separator downstream of the first heater for recov(cid:173)
`ering oil from the stillage.
`
`[0014]
`In one preferred embodiment, a second heater
`preheats the pressurized stillage before delivery to the first
`heat exchanger. More preferably, at least one of the first and
`second heaters comprises a wide gap plate and frame heat
`exchanger and the other is a scraped surface shell and tube
`heat exchanger. The first heater may comprise at least two
`heat exchangers.
`
`[0015]
`In this or another embodiment, the separator com(cid:173)
`prises a gravity separator. Preferably, the gravity separator
`comprises a centrifuge or a settling tank. The separator may
`also comprise a hermetically sealed centrifuge.
`
`[0016] According to a further aspect of the invention, a
`system for recovering oil from thin stillage resulting from a
`process used for producing ethanol is disclosed. The system
`comprises an evaporator for concentrating the thin stillage to
`form a syrup. A pump is also provided for elevating the
`pressure of the syrup to above atmospheric pressure. A first
`heater receives and pre-heats the pressurized syrup, and a
`second heater receives and superheats the pre-heated pres(cid:173)
`surized syrup. A separator downstream of the second heater
`recovers oil from the syrup.
`
`[0017] Preferably, the first heater comprises a wide gap
`plate and frame heat exchanger and the second heater is a
`scraped surface shell and tube heat exchanger. Likewise
`preferable is for the second heater to comprise at least two
`heat exchangers. The separator preferably is a gravity sepa(cid:173)
`rator, such as a centrifuge or a settling tank. The separator
`may also comprise a hermetically sealed centrifuge.
`
`[0018] Still another aspect of the invention is a method of
`recovering oil from concentrated stillage including oil
`resulting from a process used for producing ethanol. The
`method comprises pressure cooking the stillage to unbind
`the oil, and then recovering the unbound oil. Preferably, the
`method further includes concentrating the stillage prior to
`the pressure cooking step.
`
`[0019] Yet another aspect of the invention is a method of
`a method of recovering oil from stillage including oil
`resulting from a process used for producing ethanol. The
`method comprises hydrolyzing solids in the stillage, con(cid:173)
`centrating the stillage, and recovering the oil from the
`stillage. The hydrolyzing step makes the oil available for
`recovery and reduces viscosity during the concentrating
`step.
`
`[0020]
`In one embodiment, the step of hydrolyzing solids
`in the stillage includes heating the stillage. Preferably, the
`heating is to a temperature greater than 212° F. and is done
`under a pressure greater than atmospheric pressure. Most
`preferably, the method includes cooling the stillage before
`recovering oil.
`
`[0021]
`In this or another embodiment, the concentrating
`step comprises evaporating the stillage after the hydrolyzing
`step, such as by using a scraped surface heat exchanger. The
`recovering step may comprise using gravity separation.
`
`[0022] Preferably, the stillage comprises whole stillage,
`and the method further includes the step of obtaining thin
`stillage from the whole stillage after the step of hydrolyzing
`
`solids. Still more preferably, the method includes the step of
`obtaining thin stillage from the whole stillage, and the step
`of hydrolyzing solids is performed on the thin stillage. Most
`preferably, the method further includes the step of obtaining
`thin stillage from the whole stillage and the step of concen(cid:173)
`trating the thin stillage before the step of hydrolyzing solids.
`
`[0023]
`In accordance with yet another aspect of the inven(cid:173)
`tion, a system for of recovering oil from pressurized whole
`stillage resulting from a process used for producing ethanol
`is provided. The system comprises a first heater for receiving
`and superheating the pressurized whole stillage, a decanter
`for obtaining thin stillage from the whole stillage, an evapo(cid:173)
`rator for concentrating the thin stillage, and a separator
`downstream of the first heater for recovering oil from the
`thin stillage. The system may further include a second heater
`upstream of the evaporator for receiving and superheating
`the pressurized thin stillage, as well as a heat exchanger
`downstream of the evaporator for further concentrating the
`thin stillage. A dryer may also be provided downstream of
`the separator for receiving a byproduct leftover upon recov(cid:173)
`ering oil from the thin stillage.
`
`BRIEF DESCRIPTION OF THE DRAWINGS
`
`[0024] FIG. 1 is a partially schematic flow chart illustrat(cid:173)
`ing the processing of co-products formed during the ethanol
`extraction process;
`
`[0025] FIG. 2 is a partially schematic flow chart illustrat(cid:173)
`ing the recovery of oil from a syrup formed by evaporating
`the thin stillage;
`
`[0026] FIG. 3 is a schematic view similar to FIG. 1;
`
`[0027] FIG. 4 is a schematic view similar to FIG. 2;
`
`[0028] FIG. 5 is a schematic flow chart illustrating the
`strategic positioning of a separator relative to the evapora(cid:173)
`tion of thin stillage;
`
`[0029] FIG. 6 is a schematic flow chart illustrating one
`technique and system for washing whole stillage to maxi(cid:173)
`mize oil recovery;
`
`[0030] FIG. 7 is a schematic flow chart illustrating another
`technique and system for washing whole stillage to maxi(cid:173)
`mize oil recovery;
`
`[0031] FIG. 8 is a schematic flow chart illustrating yet
`another technique and system for washing whole stillage to
`maximize oil recovery;
`
`[0032] FIG. 9 is a schematic flow chart illustrating a
`technique and system for the further processing of stillage,
`such as by superheating or "pressure cooking" to maximize
`oil recovery; and
`
`[0033] FIG. 10 is a schematic diagram illustrating an
`overall technique and system for maximizing oil recovery
`from stillage.
`
`DETAILED DESCRIPTION OF THE
`INVENTION
`
`[0034] One aspect of the invention relates to a method of
`recovering oil from a byproduct resulting from the produc(cid:173)
`tion of ethanol from com, such as by using a dry milling
`technique (which is extensively described in the above(cid:173)
`referenced ' 182 patent). This byproduct, known as "thin
`
`

`
`US 2007/0238891 AI
`
`Oct. 11, 2007
`
`3
`
`stillage," is recovered by separating the distillers wet grain
`from the "whole stillage" leftover after fermentation is
`complete. As is known in the art, tis mechanical separation
`may be accomplished using a press/extruder, a decanter
`centrifuge (also simply known as a "decanter"), or a screen
`centrifuge. Moisture is then removed from the unfiltered thin
`stillage to create a concentrate or syrup, such as through
`evaporation. Usable oil is then easily recovered from this
`concentrate through mechanical processing, without the
`prior need for multiple stages of filtration or other expensive
`and complicated forms of processing.
`
`In one embodiment, oil is recovered from the
`[0035]
`concentrate by passing it through a centrifuge and, in
`particular, a disk stack centrifuge (and, most preferably, a
`self-cleaning bowl type). Preferably, the concentrate deliv(cid:173)
`ered to the disk stack centrifuge is at a temperature of
`between about 150 and 212° F. (and ideally 180° F.), a pH
`of between about 3 and 6 (ideally between about 3.5 and 4.5)
`and, as a result of the preceding evaporation step, has a
`moisture content of less than about 90% (ideally about
`60-85%). Under these process conditions, the disk stack
`centrifuge is able to separate the oil in usable form from the
`concentrate in an efficient and effective marmer, despite the
`relatively high level of solids present (which may be recov(cid:173)
`ered from the centrifuge in a continuous or intermittent
`fashion, depending on the particular process conditions).
`
`[0036] Besides creating usable oil, the concentrate or
`syrup recovered from the disk stack centrifuge is considered
`more valuable. This is because the post-evaporation pro(cid:173)
`cessing to remove the oil improves the efficiency of the
`drying process used on the combined concentrate syrup and
`distillers wet grains. A stable, flowable product for supple(cid:173)
`menting animal feed results, which thus further comple(cid:173)
`ments the value of the oil recovered.
`
`[0037] To illustrate the potential benefits that may be
`obtained by this aspect of the invention, the following
`examples are presented.
`
`EXAMPLE 1
`
`[0038] Reference is made to FIGS. 1 and 2 to illustrate
`schematically a first example demonstrating the efficacy of
`the present method. FIG. 1 represents one technique for
`processing whole stillage to create distillers dried grains
`with solubles. The whole stillage leftover after deriving the
`ethanol is mechanically separated into distillers wet grains
`(approx. 35% solids) and thin stillage (approx. 8% solids)
`using a centrifugal decanter. The thin stillage is then intro(cid:173)
`duced to an evaporator to create a concentrate, or syrup,
`having a moisture content of approximately 80% and about
`17% solids. This syrup is then recombined with the distillers
`wet grains, introduced to a drum dryer, and dried to reduce
`the overall moisture content to approximately 10%. At
`present, an estimated total value of the resulting distillers
`dried grains with solubles is $600.36 per hour.
`
`Alfa Laval Model No. 510, 513, or 617 or equivalent device.
`At an infeed rate of approximately 35 gallons per minute,
`this centrifuge 14 recovers usable oil at a rate of 538 pounds
`per hour and produces syrup having a having a moisture
`content of 82.5%, but with far less oil in view of the
`preceding recovery step.
`
`[0040] Recombining the syrup (which is substantially free
`of oil) from the centrifuge 14 with the distillers wet grains
`and drying in a drum dryer to a moisture content of 10%
`results in a product having a value of $576.46 per hour.
`However, the 538 pounds per hour of oil recovered has a
`product value of approximately $102 per hour. Accordingly,
`the total product value using the inventive method is
`$678.46 per hour, which is approximately 12% greater than
`the $600.36 per hour product value resulting from use of the
`conventional set-up shown in FIG. 1. Moreover, removal of
`the majority of the oil before the drying step makes the
`process more efficient, and results in an estimated energy
`savings of approximately 10%, or $26.27 per hour. As a
`result, product value per hour ($678.46) less the estimated
`dryer operating cost ($236.46 per hour with the 10% sav(cid:173)
`ings) and less the estimated ev