DISTILLATION AND MOLECULAR SIEVES: A … of Distillation.pdf · l viewpointl viewpoint. cincinnati, philip w. pres ohio u s a madson ident. fundam o distill mentals of lation. typical

ALCOHOL

DISTILLATDISTILLATMOLECULAMOLECULA

A PRACTICAA PRACTICAA PRACTICAA PRACTICA

L SCHOOL

ATION ANDATION ANDAR SIEVES:AR SIEVES:

L VIEWPOINTL VIEWPOINTL VIEWPOINTL VIEWPOINT

Cincinnati,

Philip W.Pres

Ohio U S A

. Madsonident

FUNDAMFUNDAMFUNDAMFUNDAMFUNDAMFUNDAMOO

FUNDAMFUNDAMOOOO

DISTILLDISTILLOO

DISTILLDISTILLDISTILLDISTILLDISTILLDISTILL

MENTALSMENTALSMENTALSMENTALSMENTALSMENTALSOFOFMENTALSMENTALSOFOFOFOFLATIONLATION

OFOFLATIONLATIONLATIONLATIONLATIONLATION

TYPICAL DITYPICAL DIRELATIORELATIO

TYPICAL DITYPICAL DIRELATIORELATIORELATIORELATIORELATIORELATIOVAPOURVAPOUR

LOWERTEMPERATURE

FEEDFEEDFEEDFEED`

THERMALTHERMALENERGYENERGY BOILING

VAPOUR

ENERGYENERGYHIGHER

TEMPERATURE

BOILINGLIQUID

BOTTOMS PRODBOTTOMS PROD

ISTILLATIONISTILLATIONONSHIPSONSHIPSISTILLATIONISTILLATIONONSHIPSONSHIPSONSHIPSONSHIPSONSHIPSONSHIPS

CONDENSERCONDENSER

REFLUXREFLUX OVERHEADOVERHEAD

COOLING WATERCOOLING WATER

REFLUXREFLUXLIQUIDLIQUID

OVERHEADOVERHEADPRODUCTPRODUCT

TRAYSTRAYS(CONTACTING DEVICES)(CONTACTING DEVICES)

DUCTDUCT

VAPOURVAPOUR--LIQUIDLIQUIDVAPOURVAPOUR--LIQUIDLIQUIDETHANOLETHANOLETHANOLETHANOL

D EQUILIBRIUMD EQUILIBRIUMD EQUILIBRIUMD EQUILIBRIUMLL--WATERWATERLL--WATERWATER

100

90

80

70

MOLE %ETHANOL

60

50ETHANOL

IN VAPOUR 40

30

20

10

0 10 20 30 40

MOLE % ET40 50 60 70 80 90 100

THANOL IN LIQUID

100

90

80

70

MOLE %ETHANOL

60

50ETHANOL

IN VAPOUR 40

30

20

10

0 10 20 30 40

(10 VOLUM(10 VOLUM

MOLE % ET40 50 60 70 80 90 100

ME % FEED)ME % FEED)

THANOL IN LIQUID

100

90

80

70

MOLE %ETHANOL

60

50ETHANOL

IN VAPOUR 40

30

20

10

0 10 20 30 40

(10 VOLUM(10 VOLUM

MOLE % ET40 50 60 70 80 90 100


THANOL IN LIQUID

100

90

80

70

MOLE %ETHANOL

60

50ETHANOL

IN VAPOUR 40

30

20

10

0 10 20 30 40

(10 VOLUM(10 VOLUM

MOLE % ET40 50 60 70 80 90 100


THANOL IN LIQUID

100

90

80

70

MOLE %ETHANOL

60

50ETHANOL

IN VAPOUR 40

30

20

10

0 10 20 30 40

(10 VOLUM(10 VOLUM

MOLE % ET40 50 60 70 80 90 100


THANOL IN LIQUID

100

90

80

70

MOLE %ETHANOL

60

50ETHANOL

IN VAPOUR 40

30

20

10

0 10 20 30 40

(10 VOLUM(10 VOLUM

MOLE % ET40 50 60 70 80 90 100


THANOL IN LIQUID

100

90

80

70

MOLE %ETHANOL

60

50ETHANOL

IN VAPOUR 40

30

20

10

0 10 20 30 40

(10 VOLUM(10 VOLUM

MOLE % ET

AZEOTROPE 194.4AZEOTROPE 194.4PROOFPROOF

40 50 60 70 80 90 100


THANOL IN LIQUID

100

90

80

70EQUILIBRIUM CURVEEQUILIBRIUM CURVE

MOLE %ETHANOL

60

50ETHANOL

IN VAPOUR 40

30

20

10

0 10 20 30 40

(10 VOLUM(10 VOLUM

MOLE % ET


40 50 60 70 80 90 100


THANOL IN LIQUID

STRUCTURING THSTRUCTURING THSTRUCTURING THSTRUCTURING THSYSTEM SSYSTEM SSYSTEM SSYSTEM S

HE DISTILLATIONHE DISTILLATIONHE DISTILLATIONHE DISTILLATIONSTRATEGYSTRATEGYSTRATEGYSTRATEGY

STRIPPING SYSTSTRIPPING SYST

100

RECTIFYINGRECTIFYING

90


MOLE %

70

60

EQUILIBRIUM CURVEEQUILIBRIUM CURVE

MOLE %ETHANOL

IN VAPOUR

50

40

30

20

(10 VOLUM(10 VOLUM

0 10 20 30 40

10

0STILLAGESTILLAGE

MOLE % ETHSTILLAGESTILLAGE

TEMTEM DEHYDRATIONDEHYDRATION

G SYSTEMG SYSTEMANHYDROUS ANHYDROUS PRODUCTPRODUCT

SYSTEMSYSTEM


PRODUCTPRODUCT

PROOFPROOF

SPIRITSPIRIT

E % FEED)E % FEED)

50 60 70 80 90 100

HANOL IN LIQUID

OPERATIOPERATIOPERATIOPERATIOPERATIOPERATIOPERATIOPERATILocus of possible coLocus of possible coliquid and vapour pliquid and vapour pa given energy inpua given energy inpua given energy inpua given energy inpu

ING LINEING LINEING LINEING LINEING LINEING LINEING LINEING LINEoncentrations of oncentrations of

passing in tower for passing in tower for utututut

100


80

70


MOLE %ETHANOL

60

50ETHANOL

IN VAPOUR 40

30 OPOPSTST20

10

STSTTYPICALTYPICAL

MOLE % E0 10 20 30 40

0STILLAGESTILLAGE

(0.02 WT. %)(0.02 WT. %)BEER FEEDBEER FEED MOLE % EBEER FEEDBEER FEED

(10 VOLUME %)(10 VOLUME %)

AZEOTROPEAZEOTROPE190 PROOF190 PROOFSPIRITSPIRIT

AZEOTROPEAZEOTROPE

PERATING LINEPERATING LINETRIPPINGTRIPPINGTRIPPINGTRIPPINGL L/V = 5.0L L/V = 5.0

THANOL IN LIQUID50 60 70 80 90 100

THANOL IN LIQUID

100


80

70


MOLE %ETHANOL

60

50ETHANOL

IN VAPOUR 40

30

20

10

MOLE % E0 10 20 30 40

0STILLAGESTILLAGE




AZEOTROPEAZEOTROPE

OPERATING LINEOPERATING LINERECTIFYINGRECTIFYINGRECTIFYINGRECTIFYING


THANOL IN LIQUID

100


80

70


MOLE %ETHANOL

60

50ETHANOL

IN VAPOUR 40

30 OPOPSTST20

10

STSTTYPICALTYPICAL

MOLE % E0 10 20 30 40

0STILLAGESTILLAGE




AZEOTROPEAZEOTROPE

OPERATING LINEOPERATING LINERECTIFYINGRECTIFYING

PERATING LINEPERATING LINETRIPPINGTRIPPING


TRIPPINGTRIPPINGL L/V = 5.0L L/V = 5.0


THANOL IN LIQUID

VAPOURVAPOUR--LIQUIDLIQUIDVAPOURVAPOUR--LIQUIDLIQUIDSTAGE ASTAGE ASTAGE ASTAGE A

D EQUILIBRIUMD EQUILIBRIUMD EQUILIBRIUMD EQUILIBRIUMANALYSISANALYSISANALYSISANALYSIS

TYPICAL - 14 REC- 8 STR

100


- 8 STR

80

7033


MOLE %ETHANOL

60

50 22

33

ETHANOLIN VAPOUR 40

30 1 OPOPSTST20

10

STSTTYPICALTYPICAL

MOLE % E0 10 20 30 40

0STILLAGESTILLAGE



CTIFYING STAGES RIPPING STAGES

88 99 1010 1111 121213131414

RIPPING STAGES

AZEOTROPEAZEOTROPE190 PROOF190 PROOFSPIRITSPIRIT44

55 66 77

AZEOTROPEAZEOTROPE


PERATING LINEPERATING LINETRIPPINGTRIPPING


TRIPPINGTRIPPINGL L/V = 5.0L L/V = 5.0


THANOL IN LIQUID

VAPOURVAPOUR--LIQUIDLIQUIDSTAGE ASTAGE A

VAPOURVAPOUR--LIQUIDLIQUIDSTAGE ASTAGE ASTAGE ASTAGE ASTAGE ASTAGE A

100

90

80MOLE %ETHANOL

70

60

IN VAPOUR33

44

60

50

100

90

80

70

60

50

40

190 PROOFSPIRIT

2

34

5 6

8 9 10 11121314

7EQUILIBRIUM CURVE

TYPICAL - 14 RECTIFYING STAGES - 8 STRIPPING STAGES

OPERATING LINERECTIFICATION

40 50MOLE % ETHANOL IN LIQUID

0 10 20 30 40 50 60 70 80 90 100

30

20

10

0

1

STILLAGE(0.02 WT. %)

BEER FEED(10 VOLUME %)

OPERATING LINESTRIPPING

TYPICAL L/V = 5.0

MOLE %

D EQUILIBRIUMD EQUILIBRIUMANALYSISANALYSISD EQUILIBRIUMD EQUILIBRIUMANALYSISANALYSISANALYSISANALYSISANALYSISANALYSIS

88 99 1010 1111 1212 1313 1414

55 66 77 190 PROOF190 PROOFSPIRITSPIRIT

44SPIRITSPIRIT


60 70 80 90 100

% ETHANOL IN LIQUID

VAPOURVAPOUR--LIQUIDLIQUIDVAPOURVAPOUR--LIQUIDLIQUIDSTAGE ASTAGE ASTAGE ASTAGE A

30

MOLE %ETHANOL 20ETHANOL

IN VAPOUR

20

10

1

2210

100

90

80

70

60

50

40

190 PROOFSPIRIT

2

34

5 6

8 9 10 11121314

7EQUILIBRIUM CURVE

TYPICAL - 14 RECTIFYING STAGES - 8 STRIPPING STAGES

OPERATING LINERECTIFICATION

3344

5566

7788

0

0STILLAGESTILLAGE

(0.02 WT. %)(0.02 WT. %)MOLE % ETHANOL IN LIQUID

0 10 20 30 40 50 60 70 80 90 100

30

20

10

0

1

STILLAGE(0.02 WT. %)

BEER FEED(10 VOLUME %)

OPERATING LINESTRIPPING

TYPICAL L/V = 5.088

M

D EQUILIBRIUMD EQUILIBRIUMD EQUILIBRIUMD EQUILIBRIUMANALYSISANALYSISANALYSISANALYSIS

OPERATING LINEOPERATING LINESTRIPPINGSTRIPPING

TYPICAL L/V = 5.0TYPICAL L/V = 5.0

BEER FEEDBEER FEED(10 VOLUME %)(10 VOLUME %)

10 20 30 40

MOLE % ETHANOL IN LIQUID

DISTILLATIODISTILLATIODISTILLATIODISTILLATIODISTILLATIODISTILLATIOCONSUMCONSUM

DISTILLATIODISTILLATIOCONSUMCONSUMCONSUMCONSUMCONSUMCONSUM

ON ENERGYON ENERGYON ENERGYON ENERGYON ENERGYON ENERGYMPTIONMPTION

ON ENERGYON ENERGYMPTIONMPTIONMPTIONMPTIONMPTIONMPTION

STEAM REQSTEAM REQSTEAM REQSTEAM REQETHANOL STRIPETHANOL STRIPETHANOL STRIPETHANOL STRIP

QUIREMENTSQUIREMENTSQUIREMENTSQUIREMENTSPPERPPER--RECTIFIERRECTIFIERPPERPPER--RECTIFIERRECTIFIER

50

40

45

BTU (In 1000’s) PER GALLON 30

35

ETHANOL (ANHYDROUS

BASIS)20

25

BASIS)

10

15

0

5

BEER CONC(VOLU

0 5

(VOLUCENTRATIONUME %)

CONSTRAINTS:• 190 PROOF PRODUCT

10 15

UME %) • 0.02% (WT.) BOTTOMS• SATURATED FEED

1112

91011

MJPER LITER 7

89

ETHANOL (ANHYDROUS

BASIS) 456

BASIS)

234

012

BEER CONC(VOLU

0 5



5 10 15


ENEENEENEENEENEENEENEENEEFFICIEFFICIEFFICIEFFICIEFFICIEFFICIEFFICIEFFICI

ERGYERGYERGYERGYERGYERGYERGYERGYIENCYIENCYIENCYIENCYIENCYIENCYIENCYIENCY

TRADITTRADITTRADITTRADIT

VAPOURVAPOUR CWCW

REFLUXREFLUX CONDENSECONDENSE

OVERHEADOVERHEADPRODUCTPRODUCTFEEDFEED FEEFEEFEEDFEED

TOWERTOWER

FEEFEE

STEAMSTEAM(ENERGY)(ENERGY)

TOWERTOWER11 STESTE

(EN(EN

BOTTOMSBOTTOMSPRODUCTPRODUCTPRODUCTPRODUCT

Energy InefficEnergy Ineffic

TIONALTIONALTIONALTIONAL

VAPOURVAPOUR CWCW

RR REFLUXREFLUX CONDENSERCONDENSER

OVERHEADOVERHEADPRODUCTPRODUCTEDEDEDED

TOWERTOWEREAMEAM

NERGY)NERGY)

TOWERTOWER22

BOTTOMSBOTTOMSPRODUCTPRODUCTPRODUCTPRODUCT

cientcient

ENERGY TRENERGY TRENERGY TRENERGY TRENERGY TRENERGY TRFORCEDFORCED -- CICIENERGY TRENERGY TRFORCEDFORCED -- CICIFORCED FORCED -- CICI

REBOREBOFORCED FORCED -- CICI

REBOREBOREBOREBOREBOREBO

RANSFER BYRANSFER BYRANSFER BYRANSFER BYRANSFER BYRANSFER BYIRCULATIONIRCULATION

RANSFER BYRANSFER BYIRCULATIONIRCULATIONIRCULATIONIRCULATION

OILEROILERIRCULATIONIRCULATION

OILEROILEROILEROILEROILEROILER

VAPOURVAPOURVAPOURVAPOUR

NGEC

TIFY

IN

FEEDFEEDMIXTUREMIXTURE

RENG

STEAM (ENERGY)STEAM (ENERGY)

STRI

PPIN

REBOILERREBOILERS

CONDENSATECONDENSATERETURNRETURN

TO BOILERTO BOILERTO BOILERTO BOILER

COOLING WATERCOOLING WATERCONDENSERCONDENSER

REFLUXREFLUX

COOLING WATERCOOLING WATER

LOWLOW-- BOILINGBOILINGPRODUCTPRODUCT

HIGH HIGH -- BOILING PRODUCTBOILING PRODUCT

ONE ONE --ONE ONE --ENEENEENEENEENEENEENEENE

CASCCASCCASCCASC

LEVELLEVELLEVELLEVELRGYRGYRGYRGYRGYRGYRGYRGY

CADECADECADECADE

ENERGY ENERGY ENERGY ENERGY

VAPOURVAPOUR

REFLUXREFLUX

FEEDFEEDFEEDFEED

RERETOWERTOWER


RERE11

BOTTOMSBOTTOMSPRODUCTPRODUCT OVERHEADOVERHEAD

PRODUCTPRODUCTPRODUCTPRODUCT

CASCADECASCADECASCADECASCADE

VAPOURVAPOURCONDENSERCONDENSER

REFLUXREFLUX

OVERHEADOVERHEADPRODUCTPRODUCTFEEDFEEDFEEDFEED

ECOVEREDECOVEREDTOWERTOWER

ECOVEREDECOVEREDENERGYENERGY 22

REBOILERREBOILER

BOTTOMSBOTTOMSBOTTOMSBOTTOMSPRODUCTPRODUCT

ENERGY CASCADEENERGY CASCADEENERGY CASCADEENERGY CASCADE

VAPOURVAPOUR

REFLUXREFLUXREFLUXREFLUX

HOTHOTFEEDFEEDFEEDFEED

RERETOWERTOWER


RERE11

BOTTOMSBOTTOMSPRODUCTPRODUCT OVERHEADOVERHEAD

PRODUCTPRODUCTPRODUCTPRODUCT

E E -- FEED PREHEATFEED PREHEATE E -- FEED PREHEATFEED PREHEAT

VAPOURVAPOUR FEEDFEED

REFLUXREFLUX CONDENSERCONDENSER

OVERHEADOVERHEADPRODUCTPRODUCTFEEDFEEDFEEDFEED

ECOVEREDECOVEREDTOWERTOWER

ECOVEREDECOVEREDENERGYENERGY 22

REBOILERREBOILER

BOTTOMSBOTTOMSBOTTOMSBOTTOMSPRODUCTPRODUCT

TWOTWO --TWOTWO --TWO TWO ENEENE

TWO TWO ENEENEENEENEENEENE

CASCCASCCASCCASC(3(3 –– TOTO(3(3 –– TOTO(3 (3 –– TOTO(3 (3 –– TOTO

LEVELLEVELLEVELLEVELLEVELLEVELRGYRGYLEVELLEVELRGYRGYRGYRGYRGYRGY

CADECADECADECADEOWER)OWER)OWER)OWER)OWER)OWER)OWER)OWER)

50

40

45

BTU (In 1000’s) PER GALLON 30

35

ETHANOL (ANHYDROUS

BASIS)20

25

BASIS)

10

15

0

5

BEER CONC(VOLU

0 5



10 15


1112

91011

MJPER LITER 7

89

ETHANOL (ANHYDROUS

BASIS) 456

BASIS)

234

012

BEER CONC(VOLU

0 5



5 10 15


ENEENEENEENEENEENEREQUIREREQUIRE

ENEENEREQUIREREQUIREREQUIREREQUIREREQUIREREQUIRE

BA

StrippingStripping--CoCopp gpp g14 lb STEAM per U.S14 lb STEAM per U.S

o1.7 Kg STEAM

o1.7 Kg STEAMgg

ERGYERGYERGYERGYERGYERGYEMENTSEMENTS

ERGYERGYEMENTSEMENTSEMENTSEMENTSEMENTSEMENTSSIC

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ENEENEENEENEENEENEREQUIREREQUIRE

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ADVANCED-I

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o1.1 Kg STEAM

o1.1 Kg STEAMgg

ERGYERGYERGYERGYERGYERGYEMENTSEMENTS

ERGYERGYEMENTSEMENTSEMENTSEMENTSEMENTSEMENTSNTEGRATED

oncentratingoncentratinggg. GALLON (absolute). GALLON (absolute)

orM per LITER orM per LITER

CONTACTINCONTACTINCONTACTINCONTACTIN(TRA(TRA(TRA(TRA((((

NG DEVICESNG DEVICESNG DEVICESNG DEVICESAYS)AYS)AYS)AYS)))))

DISTILLATION TRDISTILLATION TRDISTILLATION TRDISTILLATION TR• MIX RISING VAPOUR WITH FA• ALLOW FOR SEPARATION AFT• ALLOW FOR SEPARATION AFT• PROVIDE PATH FOR LIQUID T• PROVIDE PATH FOR VAPOUR PROVIDE PATH FOR VAPOUR

ENRICHEENRICHE

VV--LL

STRIPPEDSTRIPPEDLIQUIDLIQUID

RAY FUNCTIONSRAY FUNCTIONSRAY FUNCTIONSRAY FUNCTIONSALLING LIQUIDTER MIXINGTER MIXINGTO PROCEED DOWN THE TOWERTO PROCEED UP THE TOWERTO PROCEED UP THE TOWER

ED VAPOURED VAPOUR LIQUIDLIQUID

L MIXINGL MIXING

VAPOURVAPOUR

PERFORAPERFORAPERFORAPERFORA

OUTLET WEIROUTLET WEIR II

DOWNCOMERDOWNCOMERAREAAREA

ATED TRAYSATED TRAYSATED TRAYSATED TRAYS

NLET WEIRNLET WEIR

ENRICHEDENRICHED

DOWNCOMINGDOWNCOMINGLIQUIDLIQUID

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VV--L SEPARATIONL SEPARATION

VV--L MIXINGL MIXING

VV L SEPARATIONL SEPARATION

VAPOURVAPOUR STRIPPEDSTRIPPEDLIQUIDLIQUID

PERFORATED TPERFORATED TPERFORATED TPERFORATED T

ININOUTLET WEIROUTLET WEIR ININOUTLET WEIROUTLET WEIR


FROFROFROFRO

TRAY FROTHINGTRAY FROTHINGTRAY FROTHINGTRAY FROTHING

NLET WEIRNLET WEIRNLET WEIRNLET WEIRENRICHEDENRICHEDVAPOURVAPOUR


OTH ZONEOTH ZONE VV--LLOTH ZONEOTH ZONE SEPARATIONSEPARATION

VV--L MIXINGL MIXING

VAPOURVAPOURSTRIPPEDSTRIPPEDSTRIPPEDSTRIPPED

LIQUIDLIQUID

RELIABRELIABRELIABRELIABBEER STBEER ST

FOULFOUL

BILITYBILITYBILITYBILITYTRIPPERTRIPPERLINGLING

DISCDISC--DONUDONUDISCDISC--DONUDONU

DONDONDONDON

DISCDISC

UT TRAYSUT TRAYSUT TRAYSUT TRAYS

NUTSNUTSNUTSNUTSDESCENDINGDESCENDING

LIQUIDLIQUIDDESCENDINGDESCENDING

LIQUIDLIQUIDENRICHEDENRICHEDVAPOURVAPOUR

VAPOURVAPOUR

STRIPPED STILLAGESTRIPPED STILLAGE

BacaBacardirdi

DISCDISC--DONUDONUDISCDISC--DONUDONU

DONDONDONDON

DISCDISC

FOUFOU

UT TRAYSUT TRAYSUT TRAYSUT TRAYS

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LIQUIDLIQUIDENRICHEDENRICHEDVAPOURVAPOUR

VAPOURVAPOURLINGLING

STRIPPED STILLAGESTRIPPED STILLAGE

PERFORAPERFORAPERFORAPERFORA

OUTLET WEIROUTLET WEIR II


FOULINFOULIN

ATED TRAYSATED TRAYSATED TRAYSATED TRAYS

NLET WEIRNLET WEIR

ENRICHEDENRICHED


ENRICHEDENRICHEDVAPOURVAPOUR

VAPOURVAPOUR STRIPPEDSTRIPPEDNGNG

LIQUIDLIQUID

BAFFLEBAFFLE -- TRAYTRAYBAFFLEBAFFLE -- TRAYTRAYBAFFLE BAFFLE -- TRAYTRAYBAFFLE BAFFLE -- TRAYTRAY

• 39 COMMERCIAL SCOMMERCIAL S• 39 COMMERCIAL SCOMMERCIAL SSULFITE PULPING LIQUOSULFITE PULPING LIQUO-- SULFITE PULPING LIQUOSULFITE PULPING LIQUO

-- FERMENTED SULFITE LIFERMENTED SULFITE LIFERMENTED IGNOFERMENTED IGNO CECE-- FERMENTED LIGNOFERMENTED LIGNO--CELCEL

-- FERMENTED WHOLE GRFERMENTED WHOLE GR-- ALCELLALCELL PULPING LIQUOPULPING LIQUO-- FERMENTED CHEESE WFERMENTED CHEESE W-- FERMENTED CANE MOLFERMENTED CANE MOL

Y EXPERIENCEY EXPERIENCEY EXPERIENCEY EXPERIENCEY EXPERIENCEY EXPERIENCEY EXPERIENCEY EXPERIENCE

SYSTEMSSYSTEMSSYSTEMSSYSTEMSORORORORIQUORIQUOR

U OSE HYDRO YZATEU OSE HYDRO YZATELLULOSE HYDROLYZATELLULOSE HYDROLYZATERAINRAINOROR

WHEYWHEYLASSESLASSES

BAFFLE BAFFLE -- TRAYTRAYBAFFLE BAFFLE -- TRAYTRAY•• 5 YEAR CLEAN5 YEAR CLEAN

FERMENTED GFERMENTED G1 YEAR CLEAN1 YEAR CLEAN•• 1 YEAR CLEAN1 YEAR CLEANFERMENTED CFERMENTED C

•• ELIMINATED AELIMINATED ASCALANTSCALANTSCALANTSCALANT

•• 66--12 MONTH C12 MONTH CFERMENTED “FERMENTED “

Y EXPERIENCEY EXPERIENCEY EXPERIENCEY EXPERIENCENING CYCLE NING CYCLE GRAINGRAINNING CYCLENING CYCLENING CYCLE NING CYCLE CHEESE WHEYCHEESE WHEYANTIANTI--FOAM AND ANTIFOAM AND ANTI--

CLEANING CYCLE CLEANING CYCLE “C” MOLASSES“C” MOLASSES

RECOMMENDEDRECOMMENDEDRECOMMENDEDRECOMMENDEDRECOMMENDED RECOMMENDED RECOMMENDED RECOMMENDED

BEERSTILLS (ALL FOULING FEEDBEERSTILLS (ALL FOULING FEEDBEERSTILLS (ALL FOULING FEEDBEERSTILLS (ALL FOULING FEED

RECTIFIERSRECTIFIERS

EXTRACTIVE TOWERSEXTRACTIVE TOWERS

TECHNICAL ALCOHOL TOWERSTECHNICAL ALCOHOL TOWERS

TRAY DESIGNSTRAY DESIGNSTRAY DESIGNSTRAY DESIGNS TRAY DESIGNS TRAY DESIGNS TRAY DESIGNS TRAY DESIGNS

DSTOCKS)DSTOCKS) BAFFLE TRAYBAFFLE TRAYDSTOCKS)DSTOCKS) -- BAFFLE TRAYBAFFLE TRAY

-- PERFORATED TRAYPERFORATED TRAY

-- PERFORATED TRAYPERFORATED TRAY

-- PERFORATED TRAYPERFORATED TRAY-- PACKED ( < 24” )PACKED ( < 24” )

COCOCOCOCONTCONTCONTCONTSTRATSTRATSTRATSTRATSTRATSTRATSTRATSTRAT

OOOOTROLTROLTROLTROLTEGIESTEGIESTEGIESTEGIESTEGIESTEGIESTEGIESTEGIES

TEMPERATURE ANDTEMPERATURE ANDTEMPERATURE ANDTEMPERATURE AND

REFLUXREFLUX

CONDENSERCONDENSER

TOP TRAY

PRODUCTPRODUCT(190 PROOF SPIRITS)(190 PROOF SPIRITS)

TOP TRAY

RECTIFIER

TEMPERATURETEMPERATURETEMPERATURETEMPERATURE

BEER FEEDBEER FEED

STRIPPERSTRIPPER

BOTTOM TRAYSTILLAGESTILLAGE TRAY

D PROOF PROFILED PROOF PROFILED PROOF PROFILED PROOF PROFILE

TEMP. (°C)77

°GL95

77777878

94.59493

91 578798084

91.5898475

PROOFPROOF

84859398

75696040

ZONE OFZONE OFCONTROLCONTROL

98

102106

40

205106

106107107

51.50.5

0.005STEAMSTEAM 107 0.00005STEAMSTEAM

TEMPERATURE ANDTEMPERATURE ANDTEMPERATURE ANDTEMPERATURE AND

REFLUXREFLUX

CONDENSERCONDENSER

TOP TRAY

PRODUCTPRODUCT(190 PROOF SPIRITS)(190 PROOF SPIRITS)

TOP TRAY

RECTIFIER

TEMPERATURETEMPERATURETEMPERATURETEMPERATURE

BEER FEEDBEER FEED

STRIPPERSTRIPPER

BOTTOM TRAYSTILLAGESTILLAGE TRAY

D PROOF PROFILED PROOF PROFILED PROOF PROFILED PROOF PROFILE

TEMP. (°F)170

°PR. (U.S.)190

170171172173

189188186183

PROOFPROOF173174176184

183178168150

ZONE OFZONE OFCONTROLCONTROL

184191199208

15013812080208

216222

80

4010222

223224225

1031

0.01STEAMSTEAM 225 0.0001STEAMSTEAM

190 PROOF190 PROOFSPIRITSSPIRITS

FC

TCBEERBEERFEEDFEED FC

TC

FCSTEAMSTEAM

FC

STRIPPESTRIPPESTILLAGESTILLAGE

STRIPPESTRIPPERECTIFIRECTIFI

CONDENSERCONDENSER

REFLUXREFLUXREFLUXREFLUXDRUMDRUM

LC LC

ERERERER--IERIER

DEHYDRDEHYDRDEHYDRDEHYDRDEHYDRDEHYDRDEHYDRDEHYDRRATIONRATIONRATIONRATIONRATIONRATIONRATIONRATION

VAPOURVAPOUR--LIQUIDLIQUIDVAPOURVAPOUR--LIQUIDLIQUIDETHANOLETHANOLETHANOLETHANOL

D EQUILIBRIUMD EQUILIBRIUMD EQUILIBRIUMD EQUILIBRIUMLL--WATERWATERLL--WATERWATER

100

90

80


MOLE %ETHANOL

60

50ETHANOL

IN VAPOUR 40

30

20

10

0 10 20 30 40

(10 VOLUM(10 VOLUM

MOLE % ET


40 50 60 70 80 90 100


THANOL IN LIQUID

STRUCTURING THSTRUCTURING THSTRUCTURING THSTRUCTURING THSYSTEM SSYSTEM SSYSTEM SSYSTEM S

HE DISTILLATIONHE DISTILLATIONHE DISTILLATIONHE DISTILLATIONSTRATEGYSTRATEGYSTRATEGYSTRATEGY

STRIPPING SYSTSTRIPPING SYST

100


90


MOLE %

70

60


MOLE %ETHANOL

IN VAPOUR

50

40

30

20

(10 VOLUM(10 VOLUM

0 10 20 30 40

10

0STILLAGESTILLAGE

MOLE % ETHSTILLAGESTILLAGE

TEMTEM DEHYDRATIONDEHYDRATION

G SYSTEMG SYSTEMANHYDROUS ANHYDROUS PRODUCTPRODUCT

SYSTEMSYSTEM


PRODUCTPRODUCT

PROOFPROOF

SPIRITSPIRIT

E % FEED)E % FEED)

50 60 70 80 90 100

HANOL IN LIQUID

TERNTERNTERNTERNAZEOTAZEOTAZEOTAZEOTAZEOTAZEOTAZEOTAZEOT

DEHYDRDEHYDRDEHYDRDEHYDR

NARYNARYNARYNARYTROPETROPETROPETROPETROPETROPE

OOTROPETROPE

OORATIONRATIONRATIONRATION

ANHYDROUS ETHANHYDROUS ETHANHYDROUS ETHANHYDROUS ETHANHYDROUS ETHANHYDROUS ETHANHYDROUS ETHANHYDROUS ETH

190 PROOF 190 PROOF ETHANOL FEEDETHANOL FEED

STEAMSTEAMSTEAMSTEAM

DDCONDENSATECONDENSATE

DEHYDRATIONDEHYDRATIONTOWERTOWERTOWERTOWER

HANOL SYSTEMHANOL SYSTEMHANOL SYSTEMHANOL SYSTEMHANOL SYSTEM HANOL SYSTEM HANOL SYSTEM HANOL SYSTEM

ANHYDROUSANHYDROUSANHYDROUSANHYDROUSETHANOLETHANOL

WASTEWASTEWATERWATER

DECANTERDECANTER

ENTRAINERENTRAINERTOWERTOWER

WATERWATER

TOWERTOWER

MOLECULMOLECULMOLECULMOLECULMOLECULMOLECULDEHYDRDEHYDR

MOLECULMOLECULDEHYDRDEHYDRDEHYDRDEHYDRDEHYDRDEHYDR

VAPOUR PHAVAPOUR PHA

NO ENTRAINENO ENTRAINE

LOW ENERGYLOW ENERGYLOW ENERGYLOW ENERGY

LAR SIEVELAR SIEVELAR SIEVELAR SIEVELAR SIEVELAR SIEVERATIONRATION

LAR SIEVELAR SIEVERATIONRATIONRATIONRATIONRATIONRATION

SE ADSORPTIONSE ADSORPTION

ERER

YYYY

MOLECULAMOLECULAMOLECULAMOLECULATYPETYPETYPETYPE

CHEMICAL CHEMICAL (K2O • Na2O) • Al2(K2O • Na2O) • Al2

AR SIEVEAR SIEVEAR SIEVEAR SIEVEE 3AE 3AE 3AE 3A

FORMULA:FORMULA:O3 • 2SiO2 • XH2OO3 • 2SiO2 • XH2O

Molecular SieveMolecular SieveMediaMedia

TypeTypeTypeType3A3A3A3A

O

H

O

H

H

O

H C

O

H

C

CH

H

C

H

HH

O

H C

CH

OH

O C

H

HO

HH

H H

O

H C

CH

H H

HH

O

H C

CH

H H

HH

HH

O

O

H C

CHH

H H

HH

O

H C

CH

H H

MOLECULARMOLECULARMOLECULARMOLECULAR SIEVE BED SIEVE BED SIEVE BED SIEVE BED

INTERMEDIATE SUPPORTINTERMEDIATE SUPPORT

ADSORBENT BEDADSORBENT BED

INTERMEDIATE SUPPORTINTERMEDIATE SUPPORTINTERMEDIATE SUPPORTINTERMEDIATE SUPPORT

SUPPORT MEDIUMSUPPORT MEDIUM

MFGE DISTILLATIONMFGE DISTILLATIONPSA MOLECPSA MOLEC

MFGE DISTILLATIONMFGE DISTILLATIONPSA MOLECPSA MOLECPSA MOLECPSA MOLECPSA MOLECPSA MOLEC

BEERBEERFEEDFEED

STEAMSTEAM

RECTIFIERRECTIFIER

BEERBEER

STEAMSTEAM

FUSFUS

BEERBEERSTRIPPERSTRIPPER

REBOILERREBOILERREBOILERREBOILER FUSFUSDECDEC

STSTSTM.STM.

REBOILERREBOILERREBOILERREBOILER

CC

STILLAGESTILLAGE

REBOILERREBOILERWATERWATER

COND.COND.

N & DEHYDRATIONN & DEHYDRATIONULAR SIEVEULAR SIEVEN & DEHYDRATIONN & DEHYDRATIONULAR SIEVEULAR SIEVEULAR SIEVEULAR SIEVEULAR SIEVEULAR SIEVE

MFGEMFGEPRODUCTPRODUCT

WATERWATER

SEL OILSEL OIL

WATERWATER

BADEHYDRATIONDEHYDRATION

BEDSBEDS

VACUUMVACUUMPUMPPUMP

SEL OILSEL OILCANTERCANTERTEAMTEAMOND.OND. PUMPPUMP

MahiMahiildraildra

LAILAIICAICA

DISTILLATIONDISTILLATION--DISTILLATIONDISTILLATION--DISTILLATIONDISTILLATIONTECHNTECHN

DISTILLATIONDISTILLATIONTECHNTECHN

TYPETYPEDEHYDDEHYDTECHNTECHNTYPETYPE TECHNTECHN

1970’s STANDALONE AZEO

1980’s INTEGRATEDCOMPLEX

AZEO

1990’s INTEGRATEDUSER FRIENDLY

MOLESIEVE

2000’s ADDITIONALINTEGRATIONINTEGRATION

DEHYDRATIONDEHYDRATIONDEHYDRATIONDEHYDRATIONDEHYDRATIONDEHYDRATIONOLOGYOLOGYDEHYDRATIONDEHYDRATIONOLOGYOLOGY

DRATIONDRATIONNOLOGYNOLOGY

ENERGYENERGY(MJ/L) (BTU/G l)(MJ/L) (BTU/G l)NOLOGYNOLOGY (MJ/L) (BTU/Gal)(MJ/L) (BTU/Gal)

OTROPIC 9.5 34,000

OTROPIC 4.7 17,000

ECULARE

3.9 14,000

DISTILLATION AND MOLECULAR SIEVES: A … of Distillation.pdf · l viewpointl viewpoint. cincinnati, philip w. pres ohio u s a madson ident. fundam o distill mentals of lation. typical

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