Distillation and Rectification Guide
Distillation and Rectification Guide
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SUMMARY
[Link] Page
[Link] 1
[Link].. 1
[Link]'slaw 2
I.4. The
........n.o..n.d-i.e.a.([Link].s)[Link].n. 7
I.5. Therectification…………………………………………………… 9
[Link].. 10
[Link]
Parts
II.1-Theregimeisdiscontinuous.. . 11
[Link].. 11
II.1.1.1Theoverallmaterialbalance.. . 12
II.1.1.2Theoverallenergybalance………………………….. 12
II.1.1.3Theenergyflowofthecondenser.. 12
II.1.1.4Theequationoftherectificationline....... . 13
II.1.1.5Therefluxrate( ) …………………………………… 13
[Link]……………………………………. 14
II.1.2.1Theoverallmaterialbalance…………………………….. 15
II.1.2.2Theoverallenergybalance…………………………… 15
II.1.2.3Theenergyflowofthereboiler………………….. 16
II.1.2.4Theequationoftheexhaustionline.. . 16
II.1.2.5Thetraycolumn………………………………….. 17
II.1.2.5.1Theperforatedplates……………………………… 17
II.1.2.5.2Theplateaus{domes…………..… …………… 18
II.1.2.5.3Theeffectivenessofrealplates.. . 19
II.1.2.5.4Thenumberoftheoreticalplates……………… 20
[Link]………….. 21
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[Link]
andTheile
[Link]…………………………………………… 25
[Link]……………………………….. 26
[Link]…………… 26
[Link]{boiling………………… 27
[Link](coldsupply)…… 27
[Link].. 28
[Link]
ofPoncho-Savary
[Link]……………………………………. 31
IV.1.1Theglobalmassbalance……………………………… 32
IV.1.1.2Theoverallenergybalance.. . 33
IV.1.1.3Theequationofthecorrectionlines.. 33
[Link] 34
IV.2.1Theoverallmaterialbalance……………………………….. 35
IV.2.2Theoverallenergybalance.. 35
IV.2.2.3Theequationoftheexhaustionlines.. . 36
IV.2.2.4Theequationofthelineafeeding(right
principal)………………………………………………. 37
IV.2.2.4.1Theoverallmaterialbalance………………………. 37
IV.2.2.4.2Theoverallenergybalance.. 38
IV.2.2.4.3ThetracingofthePonchodiagramn-Savari.. 40
[Link]
columns
[Link]-Wood 42
V.1.1Introduction.. 42
V.1.2Themethodofusingthediagram………… 42
[Link]{trays……………… 44
[Link]………………………………… 44
[Link]………………………………. 45
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[Link].. . 45
Exercises……………………………………………………………………. 49
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Distillation&rectification
[Link]
[Link]
Distillationisanoperationofseparationofabinaryliquidmixture
homogeneousinitstwocomponentsbyvaporizationbasedonthedifference
betweentheirboilingpoints(ortheirpressuresteam(initspurestate).
Exampleofmisciblemixtures:Waterandaceticacid,benzeneand
toluene,ethanol,andwater
[Link]
An ideal solution is said to beif there are no forces or interactions
entresesmolécules,ousielleobéitàlaloideRaoult.
Raoult'sLaw:
A solution is said to be ideal if the partial pressure of each of its
constituents in the vapor phase is given as a function of its fraction
molarintheliquidmixtureanditsvaporpressure{purestateby
therelationship
= . (I.1)
: beingthepartialpressureofthecomponent(i)inthevaporphase.
: beingthevaporpressureofthecomponent(i)whenitisalone(inthestate
pur).
Themolefractionofcomponent(i)intheliquidmixture.
Consider an ideal liquid mixture of two components (A) and (B) completely
miscible withoutchemicalreaction(Fig.I.1),assumingthattheconstituent
(A)ismorevolatilethancomponent(B),inotherwords,wecanwrite:
> Orelse: ( ) < ( )
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Vapor phase
= +
Ideal solution
Thevaporpressureofeachofitsconstituentsinthevaporphaseis
givenbytherelation(I.1):
= . ° (I.2)
= . ° (I.3)
[Link]'sLaw
The total pressure in the vapor phaseaabove a liquid mixture
anyisthesumofthepartialpressuresofitsconstituents:
= = (I.4)
= (I.5)
: being the mole fraction of the constituent (i) in the vapor phase .In
applying the equation (I.4) and (I.5) for the previous mixture, we can
write
= + (I.6)
Andsince: + = (I.7)
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And + = (I.8)
By combining the relations (I.2), (I.3), (I.6), and (I.8), we can easily derive the
° ° °
= − + (I.9)
° °
= °− (I.10)
+° °
= ( ) Iscalled:thecondensationcurve(isotherm)orthecurve
ofdew,whichisahyperboleoftheform:y= (figI.2).
+
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T= Constante
P
PT=f(xA) PT=f(yA)
Vap
PA=f(xA)
L+V
PB=f(xA)
Liq
XA 1
0
P=f(xA, andA)
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PTConstant
Byapplyingtheequation(I.5)forthemostvolatileconstituent(A)weextract
for the same temperature the molar fraction( )whichwilbewritenunderthe
shape:
° °
−
= ( ° ) (I.12)
− °
The boiling curve T=f( ) and the dew point curve T=f( ) are
representedbyfigure(I.4)atconstantpressure,theyarethencalledthe
isothermsT=f( , ). (Fig.I.4).
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PTConstant
T
Rosée Vap
Teb(B)
L+V
Teb(A)
Boiling
Liq
0 XA, andA 1
Bydividingtheequation(I.13)numeratoranddenominatorby( ) andin
definingtherelativevolatilitycoefficient( )bytherelationship:
°
( )= ° 1 (I.14)
TheequilibriumcurveofMcCabreandTheilebecomes:
= (
(I.15)
−) +
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yA
Equilibrium curve
The diagonal
xA
I.4. Thenon-idealsolution(real)
A solution is said to be real if it exhibits forces or interactions.
intermolecular, in this case Raoult's law is not applicable.
Someofthesesolutionspresentpointsforgivenfractions.
azeotropicpointsforwhichthemixturebehaveslikea
[Link]
the volatility coefficient is equal to one( = ) or in other words:
( = ).
In this case, the boiling curves,fromdew and balance are traced
inanexperimentalway.
(Benzene-Ethanol),(Water-Aceticacid),(Fig.I.6)and(Fig.I.7).
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yA
Equilibrium curve
The diagonal
Azeotropic point
xA
PT= Constante
Dew
Teb(B)
Boiling
Teb(A)
Azeotrope
xA, yA
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I.5. Therectification
Whenseparatingabinarymixturebyvaporization,itisassumedthat
each constituent has a different vapor pressure in its pure stateof
[Link]{asinglestage
(fig.I.8). In this type of distillation, it is impossible to make a
complete separation of the two constituents, to improve this we will do
callforrectificationwhichisarepeateddistillationoradistillation
[Link]
the plateau offood supply in two sections a correction section
Condenser
Vap
Distillate
Liq
Residue
Distiller
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Condenser
Vap
Reflux
Distillate
Liq
Residue
Distiller
[Link]
Theplateauortheoreticalstageisanidealstageof100%efficiency,by
againsttherealorpracticalstagepresentsaneffectiveness<100%.
The exchange of heat and matter is all the morefast and more
more important than the contacts andthe degree of freedom tea and turbulence is
grand.
Atheoreticalfloormusthavethefollowingcharacteristics:
Thetwophases,liquidandvapor,mustbehomogeneous(theredoesnotexist
noconcentrationgradient.
Thevaporphaseandtheliquidphaseareinequilibrium.
Thesteamdoesnotcarrytheliquid.
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ChapterII
CalculationofacColumntobecorrectedaccordingtoMcCabeandThiele
Theregimeisdiscontinuous
Thediscontinuousmodemeansthatthecolumnisseparatedintoitstwosections.
rectification(indicatedv)andexhaustion(indicatedA)withoutthesesections..
areconnectedbyapowersupply.
The equations of the rectification and exhaustion lines obtained in this
modes are independentof food andremain valid in
modedietarycontinuethatwewillseelater.
[Link]
The rectifying section, also known as the enrichment section in constituting
volatile, is the upper part of the column or column headShe
includes a condenser (K) that condenses the vapors ∗ ) and the
[Link]
shape of a reflux( ∗ which helps to improve the quality of the separation,
while the other part constitutes the distillate ∗ ) with a purity( ),
([Link].1).
Condenser
Reflux Distillate
Steam
∗ , , ′
∗ , , ′
∗ , , ′′
Liq
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II.1.1.1Theoverallmaterialbalance
To establish the balance of the global molar flow rate, it is necessary to set up the balance.
next:(Incomingmaterialflow=outgoingmaterialflow).
∗ = ∗ + ∗ (II.1)
∗ is the molar flow rate in (mol/h) of the ascending vapors towards the
condenser.
∗ isthemolarflowratein(mol/h)oftherefluxliquid.
∗ isthemolarflowratein(mol/h)oftheliquiddistillate.
To find the overall mass balance of the most volatile constituent, we
multiply each term of the equation (II.1) by the mole fraction
correspondingtothesameconstituent,itcomes:
. ∗ = . ∗ + . ∗ (II.2)
II.1.1.2Theoverallenergybalance
Toestablishtheenergybalance,wemultiplythethe terms of the equation (II.1)
by the corresponding molar enthalpies since here the energy is
conveyedbymatter(convection)withoutforgettingtoaddrighttothedebit
heatabsorbedbythecondenser(K).Thenitcomes:
′′ . ∗ = ′ . ∗ + ′. ∗+ ∗ (II.3)
With: ′′ , ′ ′ respectively, the molar enthalpies of the phases
vapor,liquid,anddistillate.
II.1.1.3Theenergyflowofthecondenser
The heat flow rate( ∗ ) the condenser (K) represents the quantity of
heatperunitoftimeabsorbedbytherefrigerantfluid(waterorair).
Fromequation(II.1)wetire
∗ = ∗ − ∗ (II.4)
Bytaking: ′ ≅ ′ and∆ = ′′ − ′ and by replacing (II.4) in (II.3),
weendedupwith:
∗ = ∗ .∆ (II.5)
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Note:
Generally in calculations, an average value of the molar enthalpy
ofvaporization(∆ ) [Link],we
calculatetheaverageenthalpyofvaporizationatthetopofthecolumnby:
(∆ ) = . (∆ (
)( ) + 1− )
. (∆ )( ) With: (A) and (B) designating
respectively,thevolatilecomponentandtheleastvolatile.
II.1.1.4Theequationoftherectificationline
In the Mc Cabre and Theile diagram, the equation of the line of
rectification (main line), it is the affine relation deduced in
Replacingequation(II.4)inequation(II.2),hence:
∗ ∗
= ∗ + ∗ (II.6)
Shecutsthediagonalatthepoint: ( , )Itsslopeis:
∗
( ) = ∗ <1 (II.7)
II.1.1.5Therefluxrate( )
Therefluxratioindistillationisdefinedastheratiobetweenthe
refluxflowrate (
∗ andtheflowrateofthedistilate ∗ ),soitiswritten:
∗
= ∗ (II.8)
= + (II.9)
+ +
Itcaneasilybededucedthatthislinealsopassesthroughthepoint( 0, )
+
([Link].2).
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Equilibrium curve
yA
Right of
+
rectification
xA XD
[Link]
The sectiondexhaustion also called section ofdeprivation in
volatileconstituent,formsthelowerpartofthecolumnorbaseofthe
column. It includes a reboiler (B) that vaporizes the liquid
∗ ) ∗
descendant and( transforms a part into ascending vapors (. )
while the otherthe part of the liquid less rich in volatile constituents is
extractedintheformofaresidue( ∗) ofmolarfraction( ),([Link].3).
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Steam Liquid
∗ ′′ ∗ , , ′
, ,
∗ Residue
∗ , , ′
Distiller
II.1.2.1Theoverallmaterialbalance
To establish the overal molar flow balance, it is necessary to establish the balance.
next:(Input=output).
∗ = ∗ + ∗ (II.10)
∗ is the molar flow rate in (mol/h) of the ascending vapors to the
rectifyingsection.
∗ isthemolarflowratein(mol/h)ofthedescendingliquid.
∗ isthemolarflowratein(mol/h)ofthedrawnliquidresidue.
Pour trouver le bilan de matière global du constituant le plus volatil, on
multiply each term of equation (II.10) by the fractionin molar
correspondingtothesameconstituent,itcomes:
. ∗ = . ∗ + . ∗ (II.11)
Letusrememberthatindex(A)meanstheexhaustionsection.
II.1.2.2Theoverallenergybalance
Toestablishtheenergybalance,andsincetheenergyhereisconveyedbythe
matter (convection)we multiply the terms of the equation (II.1 by the
corresponding molar enthalpies without forgetting to addto the left
(input)theheatoutputgivenoffbytheboiler(B).Thenitcomes:
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′ . ∗ + ∗= ′′ . ∗ + ′. ∗ II.12
With: ′′ , ′ ′ respectively, the molar enthalpies of the phases
steam,liquid,andresidue.
II.1.2.3Theenergyflowofthereboiler
The heat flow rate( ∗ ) the reboiler (B), represents the quantity of
heat per unit time transferred by the reboiler to vaporize the
liquidfromthebotomofthecolumn.
Apfromtheequation(II.10)andbysubstitutingin(II.12)andtaking:
′ ≅ ′ and∆ = ′′ − ′ wetalkedaboutit:
∗ = ∗ . (∆ ) (II.13)
Note:
Generally in calculations, an average value of molar enthalpy
ofvaporization(∆ ) [Link],we
calculate the average enthalpy of vaporizationaat the botom of the column bythe
relation:
(∆ ) = . (∆ )( ) + (1− .)(∆ )( ) With: (A) and (B) designating
respectively,thevolatileconstituentandthelessvolatileone.
II.1.2.4Theequationoftheexhaustionline
In the Mc Cabre and Theile diagram, the equationto the right of
exhaustion is the affine relationship derived by replacing the equation
(II.10)inequation(II.11rf)omwhere:
∗ ∗
= ∗ − ∗ (II.14)
The line of exhaustionthe measurement and the correction pass through a point
common ( , ) Whatisthepowersupplypointofthecolumn.
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(yA)
+
Right
S exhaustion
(xA) XD
XS
II.1.2.5Thetraycolumn
Different types of trays (levels) exist in the columns, and each
type of board is diferent from the other from a construction point of view and
[Link].:
II.1.2.5.1Perforatedplates
They were the first trays used in the [Link] columns to
rectifiers. They are cheaper, easier to clean, but they are also
less profitable (less effective) and present ofthe risks
trainingoftheliquidbytherisingsteam,andincaseofafalfromthe
underpressure,thesetraysrainwithliquid([Link].5).
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II.1.2.5.2Thedomeplates
Theycreatealargesurfaceandagoodcontactbetweentheliquidphaseandthe
vapor phase, they do not present any dripping issues or
of training because in the event of a drop in pressure, the caps will
They are therefore more profitable and more efficient than the trays.
perforated, on the other hand they are dificult to clean and more expensive
([Link].6).
Liquide
Vapeur
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Liquid
Steam
II.1.2.5.3Theeffectivenessofrealplates
A theoretical plateau is effective at 100%, while a real plateau or
practice has an efficiency always lower than 100%, so in practice the
the number of practical plates is always greater than the number of
[Link]
(I.6), the non-theoretical (real) plateau can present problems of
concentration gradient, liquid entrainment by the vapor, and/or
of non-achieving balance between the phaseliquid and vapor phase.
Efficiencyso expresslthe gap compared to the ideality of a real floor.
([Link].7)
According to this figure, the efficiency (S) is expressed by a ratio of
segments or distances or by the ratio between the number of
theoreticalplateausandthenumberofpracticalplateaus:
−
S= ( ) − −
(II.16)
é −
( é )
S= (II.17)
( )
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Equilibrium curve
(yn)eq
yn
Xn-1 Xn
II.1.2.5.4Thenumberoftheoreticalstages
After the tracingfromtheequilibriumcurveanddthe rights of rectification and
a theoretical plateau is obtained by drawing a line
verticalstartingfromthepoint ( , ) untiltheequilibriumcurvefolow-up
from a horizontal line to the intersection with therightofexhaustion
(in the areadandhteexhaustion) or with the rectification line (in the
rectification zone), the tracing of theoretical plates continues until the
point ( , ) ([Link].8)
Note:
Ifthelastplatereachespoint(D)yet,anotherplateau(a
only)isaddedevenifweexceedtothispoint.
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Theoretical plateaus
Equilibrium curve
(yA)
2 D
P Right of
1
rectification
+
Right
of exhaustion
S
(xA) XD
XS
[Link]
As we have just seen in paragraph (II.1.1.5), and given by the relation
(II.8),therefluxrateisdefinedastheratiobetweentheflowrateof
reflux ∗ ) and the distilate flow rate( ∗ ), so the increase or the
reductionofoneofthetwoflows( ∗
)or( ∗ influence on performance.
Wecandistinguishthreepossiblecases:
( → 0,therectificationlineishorizontal.
( → ∞),thelineofcorrectionisthediagonal,inthiscase
Therefluxistotalandthenumberoffloorsisminimal.
( → ), the point(p) intersection between the line of
rectification and the exhaustion line is located on the curve
of equilibrium, then the number of theoretical trays in this
caseisinfiniteandtheperformanceismaximum.
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= +
+ (II.18)
+
(yA)
E
P D
Right
of exhaustion
S
XS (xA) XD
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Note:
In practice, and after studies of variationinvestment costs,
ofoperationandtotalfeesbasedontherefluxrate( ),([Link].10),
we findanoptimalrefluxratioaccordingtotherelationship:
1.3 ≤ ≤4 (II.20)
Fees
investment
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ChapterIII
CalculationofacColumntoberectifiedaccordingtoMcCabeandThiele
III.1-Theregimeiscontinuous
Danscemode,lesdeuxrectificationanddepletionsectionsarerelated
in material flowstire and energyby a continuous power supply, this
foodation does not influence the equations of the rectification lines and
exhaustionrespectively (II.6) and (II.14) found earlier. The
Thecolumnworkingincontinuousoperationisillustratedbyfigure([Link].1)
Condenser
∗ , , ′′
Reflux Distillate
∗ , , ′
∗ , , ′
Nutrition
∗ , , ′ ,
∗ , , ′
∗ , , ′′
∗ Residue
∗ , , ′
Distiller
A-Data:
Generally, the molar flow rate is given.( ∗) or massive( ∗) of
thesupply,itsinlettemperature( ) inthecolumn,itstemperature
boiling( )anditsmolarpercentage(fraction)( ) ormassive( ′)
volatilecompound.
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B-Specifications:
Thepurity( ) thedistillate,andthemolefractionofthevolatileconstituentin
theresidue( ),aretheessentialspecifications.
C-Operationalchoice:
During the operation, we choose as necessary the reflux rate that remains.
generallyinthemarginsindicatedbyrelation(II.18).
This reflux rate varies according to the operating [Link]
purity,yield…etc.
III.1.1Theoverallmaterialbalance
[Link]
(outgoing material flow rate), by applying this equality to the column, we
find:
∗ = ∗+ ∗ (III.1)
To find the overall mass balance of the most volatile component, we
multiplyeach term of the equation (III.1) by the molar fraction
Correspondingtothesameconstituent,itcomes:
. ∗= . ∗+ . ∗ (III.2)
Bysubstitutingequation(III.1)into(III.2),wederivethemolarflowrateof
distillate ∗ whichwilbegivenbytheequation:
∗= − ∗
( ) (III.3)
−
Themolarflowrateoftheresidue( ∗ )isdeducedinthesameway
∗= − ∗
( ) III.4
−
[Link]
Sometimes, in cases of a cold diet, it occurs a
condensation at the level of the feeding tray of a quantityof
ascending vapors from the exhaust section, this phenomenon leads to
généralementàuntauxdebouillageplusélevé.
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III.1.2.1Thefeederioncomestoaboil
In this case,the food between {its temperatureboiling or in
other terms, { an equal temperaturàe cthe liquid from the tray
of food. In this case,There is no condensation of the
upward vaporsfrom the exhaustion [Link] can easily shoot at
toleaveof the material balance of the liquid around the feed tray, the
followingrelations:
= (III.5)
∗ = ∗ (III.6)
∗ = ∗ + ∗ (III.7)
III.1.2.2Condensationcase(coldsupply)
Inthiscase,lthetemperatureofthefoodislowerthanthetemperature
boiling of the liquid on the trayelfoodBy meeting a
cold plateau, the ascending vaporsto the rectification section
partially condense by releasing their condensation heat to
[Link],wehave:
> (III.8)
Thisphenomenonhelpspreheatthecoldfood.
be(tL
iet∆ ∗ ) Themolarflowrateofthecondensedvapors,thematerialbalanceof
theequation(III.7)thenbecomes:
∗ = ∗ + ∗ +∆ ∗ (III.9)
Theenergybalancearoundthefoodplateaubecomes:
∆ ∗ . (∆ ) = ∗. ( − ) (III.10)
Onecanalsowrite:
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( − )=( ′ − ′) (III.11)
With:
′ , ′ : The molar enthalpies of the feed respectively {
.
: Themolarspecificheatofthefeed(J/mol.K).
Byintroducingthedimensionlessterm( ) definedby:
( − )
= + (III.12)
(∆ )
Fromequation(III.12)and(III.10),wecandeduce:
∆ ∗ =( − ) ∗ (III.13)
Andequation(III.9)becomes:
∗ = ∗ + . ∗ (III.14)
Conclusion:We can summarize the two cases (III.1.2.1) and (III.1.2.2) by considering
basedonthevalueof( ) :
1/If( = )⇒ = 1Thereisnocondensation.
2/If( < )⇒ 1hey’aune partialcondensationofthevaporsat
leveloftheplateaudnutrition.
[Link]
The supply line is the line that divides the column into two.
sections: rectification and exhaustion, and since the plateau of
food is a common platform between the two sections, so there
the power line must also pass through the point ( , ) ofintersection
ofthetwolinesofrectificationandexhaustion.
Tofindtheequationofthesupplyline,abalancemustbeestablished.
matteraroundthefeedingtray([Link].1),itcomes:
∗ + ∗ = ∗ + ∗+ ∗ (III.15)
To obtain the balance of the volatile constituent, one multiplies each flow rate.
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. ∗ + . ∗ = . ∗ + . ∗+ . ∗ (III.16)
= −
− −
(III.17)
Thislineisveryimportantinrectification,because:
- Shecutstheequilibriumcurveandthelineof( ) atpoint(E).
- ShecutsthediagonalatpointF( , ).
- Itintersectsthex-axisatpoint(, 0 ).
- Sheintersectsthelinesofrectificationandexhaustionatthepoint
common ( , ).
Note:
- 1/Accordingtoequation(III.17),if 1(condensationcase),theslope
ofthisline:Tg = 1. ([Link].2)
−
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P
D
+
+
Right
S of food
xF/µ xF
XS XD
P
D
+
+
Right
S of food
xF
XS XD
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ChapterIV
Calculationofacolumn{rerectifieraccordingtothePonchon-Savarimethod
Itisamoreenergeticthanquantitativemethod.
Itisbasedonthemolarenthalpydiagramasafunctionofthefractions.
molars: = ( , ) ormfwher = ( ) designates the boiling curve, and = ( )
designatesthedewcurve.
Note:
The use of a mass enthalpy diagram as a function of
mass concentrations or in terms of mass fractions, remains
valid, but the choice of molar quantities facilitates the transition between this
diagramandthepreviousdiagramofMcCabe-Thiele(theoverlap
ofthetwodiagrams).
IV.1Thecorrectionsection
In the correction section illustrated by figure (IV.1), and
unlike the case of Mc Cabre-The distillate leaves the exchanger of
reflux (K) in the form of vapor that will be condensed in another
exchanger (D). So the exchanger (K) in this case only condenses the
quantitythatreturnsinthecolumnasreflux( ∗ ).
Thisdivisionoftheexchanger(K)intotwoothersthe exchangers proposed by
PonchoSavaryclarifiesandfacilitatesthestudyandunderstandingofthediagram
proposed.
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Reflux condenser
Steam distillation
Reflux ∗ ′′
Steam , ,
∗ , , ′
∗ , , ′′
∗
Liquid
Liquid distillate
Distillate condenser
∗ , , ′
IV.1.1Theoverallmaterialbalance
Theoverallmaterialbalanceandthatofthevolatileconstituentareindifferentto
thosefromMcCabe-Theilealreadyseeninparagraph(II.1.1).
To establish the balance of the global molar flow rate, it is necessary to establish the balance.
next:(incomingmaterialflow=outgoingmaterialflow).
∗ = ∗ + ∗ (IV.1)
To find the overall material balance of the most volatile component, we
multiply each term of the equation (IV.1) by the molar fraction
correspondingtothesamevolatileconstituent,itcomes:
. ∗ = . ∗ + . ∗ (IV.2)
Note:
Thevolatileconstituentfractionofthesteamdistilate( ) andthatofthedistilate
liquid ) areequal( = ) sincethedistillateisafinishedproduct .
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IV.1.1.2Theoverallenergybalance
Toestablishtheenergybalance,wemultiplythetermsofequation(IV.1)
by the corresponding molar enthalpies since here the energy is
conveyedbymatter(convection)withoutforgettingtoadd{righttheflow
heat absorbed by the condenser (K), and taking into account that the
[Link]:
′′ . ∗ = ′. ∗ + ′′ . ∗+ ∗ (IV.3)
IV.1.1.3Theequationoftherectifyinglines
Unlike the case of Mc Cabre-Theile, the equation we will see in this
paragraph represents several lines (equal to the number of floors of the
correctionsection.
Toestablishthisequation,wewillusethepreviousmaterialbalances.
andenergy.
Byreplacingltheequation(IV.1)intheequation(IV.2),wefind:
∗ ( − )= ∗( − ) (IV.5)
Bysubstitutingequation(IV.1)intoequation(IV.3),wefind:
∗
∗ ( ′′ − ′ )= ∗( ′′ + −∗ ′ ) (IV.6)
Thespecificrefluxheatisdefinedas ) bytheterm:
∗
= ∗ (IV.7)
Startingfromequation(IV.4),andtakingintoaccountaccountofthedefinitionoftherateof
reflux(II.8),wehaveit:
= (∆ ) (IV.8)
By dividing the equation (IV.6) pin equation (IV.5) taking into account
(IV.7)onaboutit{theequationrectificationlinesundertheform:
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( ′′ − ′ ) [( ′′+ )− ] ′
= (IV.9)
( − ) ( − )
This equation is a first degree [Link] it is a straight line,
itexpressesthealignmentofthreepoints([Link].2):
- Thevariablepoint: ( , ′) belongingtotheboilingcurve.
- Thevariablepoint: ( , ′′ ) belongingtothedewpointcurve.
- The point fix ( , ′′ + ) called the pole of rectification, it
locatedabovethedewpoint.
h (J/mol)
Dew Pv
qK
L+V G1v
′′
G2v
′ ′′
L1v L2v
Boiling
x1V y2V yD
[Link]
[Link]
( ∗ )
includes a reboiler (B) that vaporizes the descending liquid and
transformapartintoascendingvapors ∗ ) whiletheotherparty
the liquid less rich in volatile constituents is drawn off in the form of
residue( ∗ ) withafraction( )([Link].3).
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Steam Liquid
∗ ′′ ∗ , , ′
, ,
∗ Residue
∗ , , ′
Boiler
Ponchon-safari
IV.2.1Theoverallmaterialbalance
To establish the balance of the overal molar flow rate, it is necessary to establish the balance.
next:
∗ = ∗ + ∗ (IV.10)
To find the overall material balance of the most volatile component, we
multiplyi.e. each term of the equation (IV.10) by the mole fraction
correspondingtothevolatileconstituent,itcomesfrom:
. ∗ = . ∗ + . ∗ (IV.11)
Bysubstitutingequation(IV.10)intoequation(IV.11),onefind:
∗ ( )= ∗
− ( − ) (IV.12)
IV.2.2Theoverallassessmentofenergy
Toestablishtheenergybalance,wemultiplythetermsofequation(IV.10)
bythecorrespondingmolarenthalpieswithoutforgettingtoaddutotheleft
theheatoutputgivenoffbytheboiler(B).Thusitfollows:
′ . ∗ + ∗= ′′ . ∗ + ′. ∗ (IV.13)
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Specificboilingheatisdefinedas ) bytheterm:
∗
= ∗ (IV.16)
IV.2.2.3Theequationoftheexhaustionlines
Unlike the Mc Cabe case-The equation that we will seeris in this
paragraph is the equation of several lines (equal to the number of etages
oftheexhaustionsection) .
Toestablishthisequation,wewillusethepreviousmaterialbalances.
andenergy.
By dividing equation (IV.15) by equation (IV.12) taking into account
(IV.16),aboutit{theequationoftheexhaustionlines:
′ − ′′ [( ′ − )− ]′
( )
= (IV.17)
− ( − )
Thisequationisafirst-orderequation.,soit'saline,it
expressthealignmentofthreepoints([Link].4):
- Thevariablepoint: ( , ′) belongingtotheboilingcurve.
- Thevariablepoint: ( , ′′ ) belongingtothedewpointcurve.
- Thefixedpoint: ( , ′− ) calledthepoleoflexhaustion,itislocated
undertheneckboilingpoint.
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h (J/mol)
Dew
G1A
(∆ ) L+V G2A
′′
′
L1A (∆ )
L2A
′
qB
Boiling
PA Constituent (A)
Constituent (B)
xS x2A y2A
Ponchon-savari
IV.2.2.4Theequationofthesupplyline(mainline)
To find the equation of the supply line, it is enough to establish the
massandenergybalanceeentryandexitforthecolumn.
IV.2.2.4.1Theoverallmaterialbalance
The overall balance of matter is based on [Link] flows
entering the column = material outputs from the column), in
applyingthisequality,wefind:
∗ = ∗ + ∗ (IV.18)
To find the overall material balance of the most volatile component, we
multiplyeach term of the equation (IV.18) by the mole fraction
correspondentofthesameconstituent,itcomes:
. ∗ = . ∗+ . ∗ (IV.19)
Bysubstituting(IV.18)into(IV.19),wededuce:
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∗(
− )
= (∗ − ) IV.20
IV.2.2.4.2Theoverallenergybalance
Toestablishtheenergybalance,wemultiplythetermsoftheequation(IV.18)
by the corresponding molar enthalpies without forgetting to add { right
the heat flow absorbed by the condenser (K), and to the left the flow
heatcededbytheboiler(B),itcomes:
′ . ∗ + ∗= ′. ∗ + ′′ . ∗+ ∗ (IV.21)
Byreplacingthefeedrateoftheequation( IV.18)intheequation
(IV.21), taking into account the equalities(IV.7) and (IV.16) of heats
specific,weobtain:
∗( ′′+ −) =′ [ ∗
−(′ − ′ )] (IV.22)
Bydividingequation(IV.22)byequation(IV.20),weobtaintheequationof
thepowersupplyline:
′′
+ − ′ [ ′ −( ′ − )]
( )
= (IV.23)
− ( − )
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h(J/mol)
Power supply line
PV
′′
F ′
PA
xS xF xD
Ponchon-ride
Remark:
- If the supply is between { its boiling point (there is no
condensation),point(F)islocatedontheboilingcurve.
- Ifthepowersupplyisbelowitstemperature
atboiling,point(F)islocatedbelowtheboilingcurve
([Link].6).
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h(J/mol)
Power supply line
PV
′′
′
PA
xS xF xD
IV.2.2.4.3ThetracingofthePoncho-Savarydiagram
ThePoncho-Savarydiagramincludesadewpointcurveandanotherone.
boilingcurve.
To facilitate the tracing of these curves, we wil take into account the
followingsimplifications:
1 / OLetusassumethatthesetwocurveshavealinearshape.
2/ItisassumedthatwhenT=0°Ch=0J/mol,[Link]°Cfor
thetemperatures,byshiftingthemolarenthalpiesof([Link]).
Thetracingbeginswiththevolatilecomponent(A)(rightaxis):
′= . ∈ { laboilingcurve(y-axis).
′′ = ′+ ∆ ∈ tothedewpointcurve(rightaxis).
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Forthelessvolatileconstituent(B)(leftaxis):
′= . ∈ { laboilingcurve(leftaxis).
′′ = ′+ ∆ ∈ atthedewpointcurve(leftaxis).
Finally,weconnectbyaline. ′ with ′ and ′′ with ′′ .([Link].7)
h(J/mol)
PV
′′
(∆ ) ′′
′
(∆ )
PA
XS XF XD
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ChapterV
Gillilanddiagramandcolumnsizing
[Link]-WoodMethod
V.1.1Introduction
GillyLandproposedadiagrambearinghisnamethatillustratesvariation.
é −( é) −
from ) depending on ( ) by fixing a domain
é +1 +1
−
ofoperation(Fig.V.1): 0.1≤ ≤ 0.36. (V.1)
+1
Log x 1 *x
D S
1 x x
η ( they)min = D S
1 (V.2)
Log
V.1.2Themethodofusingthediagram
1-Firststep:
Theoperationalrefluxrate( )ischosen.
2-Secondstep:
−
Wechooseavalueforlabscissa( ) intheoperationalfield
+1
[Link],thevalueof( )isthereforefixed.
3-Thirdstep:
Wereadinthesamediagramthecorrespondingvalueoflordered
é −( é)
( ).
é +1
4-Fourthstep:
η ( thi)minbytheequationofFunksUnderWood.
Wecalculate(
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5-Fifthstep:Thenumberoftheoreticalplates( é ) iscalculated
sobyreplacingthevalueof(η ( thi) min) in
é −( é)
( ).
é +1
Remark
The set reflux rate, the calculated minimum reflux rate, the fractions
molars , and the volatility coefficient α, allow for the calculation of the
numberoffloorstheoriches by the McCabe Thiele method, and thus of
comparebetweenthetwomethods.
Operation domain
0.8
0.6
0.4
0.2
0.1
0.08
0.06
0.04
0.02
0.01
0.04 0.06 0.1 0.2 0.4 0.6 0.8 1
0.02
−
( )
+
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[Link]{trays
In this paragraph, we will only look at the simplest method of
approximate calculation of the diameter and height of the column without too much
details.
[Link]
Afterthecalculationofthedistilateflowrate( ∗ ), and after fixing a taux of
operational reflux ), we can easily deduce the flow rate of the vapors
ascendants( ∗ ).
Thevolumetricflowrateofvapors( ∗ isrelatedtothemolarflowratebytheequation
stateofgases:
∗ .
∗= (V.3)
Z:thecompressibilityfactorofvapors.(Z=1foridealgases)
R:theidealgasconstant(8.32J/mol.K=[Link]/mol.K)
Pthevaporpressure{insidethecolumn(forthecolumn
atmospheric,P=1atm.
T:thetemperatureoftherisingvapors.
Theflowofvapors ∗ islinkedtothesectionofthecolumn(S)bythe
relation:
∗= . (V.4)
V:thespeedofthevapors,generallyinpracticewehave:
1≤ ≤2( / )
2
S:thesectionofthecolumn: = 4
(V.5)
Aftercalculatingthevaporflowrateby(V.3),wecalculatethesectionofthe
columnby(V.4),thenwedeterminethevalueofthecolumndiameter
bytheequation(V.5).
4
= (V.6)
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Theheight(H)ofthecolumnisdirectlyrelatedtothenumberofplates.
[Link]
The trays in the columns are separated by a vertical distance.
constant and homogeneous throughout the column. This distance differs from a
columntoanother,anditdependsonthenatureoftheliquidtobeseparatedthe of
typesoftraysandoperatingconditions.
The height (h) of the plateau is the vertical distance between two plateaus.
successive.(Fig.V.2).
Wedistinguishtwocasesinthecalculationofthecolumnheight:
1- Thethebottomofthecolumnisconsideredasaplatform
In this case, the bottom of the column is considered as a floor.
since it contains the dense liquid where the drawing of the
residue. The number of trays hereisequaltothenumberofspacesandthe
theheightofthecolumnbecomes:
= h. é (V.7)
2-Thebottomofthecolumnisnotconsideredaplatform.
Inthiscase,thecolumnisconsideredasabuildingwhosebase
isagroundfloorandnotafloor.
Hereisthenumberthenumberoffloorsislessthanthenumberofspacesinaunit,
andtheheightofthecolumnisthereforecalculatedby:
= h.( é + 1) (V.8)
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Plateaus
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Exercises
Exercise-01
We prepare ideal mixtures from two completely liquid substances.
misciblewithdifferentmolarfractions.
We measure the boiling temperature for each mixture under the
atmosphericpressure
( P=1atm)basedonthemolefractionX1andvaporpressure
oftheconstituent(2)pure,wefindthefollowingvalues:
X1 1.00 0.95 0.90 0.85 0.80 0.75 0.70 0.65 0.60 0.50 0.40 0.25 0.15 0.00
X2
P°2 …. 3.5 3.25 2.66 2.50 2.20 2.08 1.93 1.81 1.60 1.41 1.26 1.15 1.00
P°1
Y2
1/Completethetable.
2/Drawthecurves: P° 2= f(T)andP°1=f(T)inthesamediagram.
Quelestlecomposéleplusvolatil?
3/Drawthecurvealpha=f(T), α beingthecoefficientofrelativevolatility.
4/Plottheboilingcurveandthedewpointcurveonthesamediagram.
5/We take a liquid mixture to50 °Cmole fractionX20.4and of
totalnumberofmolesN10
t molesitisheatedtothetemperatureof
80°Cunderatmosphericpressure.
- Findatthistemperaturetheratio:
N(vaporphase)/N(liquidphase)
- Deducethevaluesofthenumberofmolesoftheliquidphaseandofthe
vaporphase.
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Exercise-02
Wemustseparatebydistillationinarectifyingcolumn.2.10kg/hof
4 a
ideal binary liquid mixture of two products(A)and(B)totally
miscibleandwithoutazeotropeofmassfractions:XB=40%andXA=60%,
comes to its boiling point. We work with a reflux rate
1.5 min.
Therelativevolatilitycoefficientisequalto:4
The distillate leaves the reflux exchanger (K) in vapor form.
containingonly5%in moles of the heavy constituent and95%oftheconstituent
light, while the residue contains only5% in moles of the constituent
volatile.
Wegive:Cp(A)=100J/molKandΔHv(A)=15KJ/mol
Cp(B)=150J/molKandΔHv(B)=20KJ/mol
M(A)=60g/molandM(B)=90g/mol
1/Calculate: N N
, *
D
*
S
therefluxrate(V).
* * * *
2/Todeduce: N N
, N, N ,
LV GV LA GA
thedistiller.
Exercise-03
A column { rectifier is fed { from a tank containing a
ideal liquid mixture of two organic compounds(A)and(B)totally
misciblewithoutchemicalreaction
[Link]
followingcharacteristics:
- Thetemperatureis25°C
- Each15gtheliquidmixturecontains6gof(A)and9gof(B).
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Themelonthepreviousoneisheatedtoitsboilingtemperature
withafeedrate M *
F
768Kg/h .
Therelativevolatilitycoefficientisequalto3.
* *
1/CalculatethemolarflowrateofthedistilateN D,andthatoftheresidueN S .
2/Calculate:therefluxrate , deducethevaluesofthemolarflowrates:
* *
N N
, LV GV
.
3/DrawtheequilibriumcurveY=f(X)intheMcCabeThielediagram
aswellasthefollowinglines:Supply,rectification,exhaustion.
* *
Q ,Q ,Q
*
4/Calculatetheheatflows:
K B E
5/Determinethenumberofshelvesinthiscolumn.
Exercise-04
We must separate by distillation in a rectifying column.9. 10mol/h
4
of an ideal binary liquid mixture of two products (A) and (B) totally
miscible and without azeotrope of mole fractions:xB0.5andxA=0.5, the
charge enters at a temperatureTW
f e work with a reflux rate.
V=1.5Vmin .
A liquid distilate of purity is required.95%in moles and a residue not
containingonly5% inmolesofthevolatileconstituent.
In the McCabe-Thiele diagram, the equilibrium curve and the line
powersuppliespassthroughthesamepoint(0.5,0.75).
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Wegive: Cp (Average)=350J/molK
Hv(Average)=40KJ/mol
1/Calculate: N N
, *
D
*
S
,Vmin
*
2/Todeduce:V, N LV
, N *GV
3/Writetheequationsofthefollowinglines:Supply,rectification.
4/Plot the equilibrium curve Y=f(X) in the McCabe diagram
Theile.
5/Determinethenumberofshelvesinthiscolumn
* *
,Q ,Q
* * *
6/Calculate: N ,N N
, GA THE GA K B
Exercise-05
Wemustseparatebydistillationinarectificationcolumn.10mol/hof
6 a
ideal binary liquid mixture of two products(A)and(B)totally
miscibleandwithoutazeotropeofmolarfractions:XB=0.8andXA=0.2
Weworkwitharefluxrate 1.5 min.
The physicochemical analysis of the liquid phase and the vapor phase of
first(1e r) theplateauofthecolumnshowsthattheliquidphasedoesnotcontain
what5%inmolesof(A)whilethevaporphasecontains82.6%inmoles
of(B).
Following a defect in the reflux exchanger(K)only condense that60%of
*
vapors N GV
sothedistillateleavestherefluxexchanger(K)intheformof
vaporcontainingonly5% inmolesof(B).
Wegive:Cp(A)=100J/molKandΔHv(A)=15KJ/mol
Cp(B)=150J/molKandΔHv(B)=20KJ/mol
1/Calculate: N N
, *
D
*
S
,Vmin
* * * *
2/Todeduce: N N
, N, N,
LV GV THE GA
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Exercise-06
Wemustseparatebydistillationinarectifyingcolumn.10mol/hof
5 a
ideal equimolar liquid binary mixture of two products(A)and(B)
completely miscible and without azeotrope, the distilate leaves the exchanger of
reflux(K)intheformofaliquidcontaining95%inmolesoftheconstituent
lightwhiletheresiduecontainsonly5% ofthesameconstituent.
TheinlettemperatureofthepowersupplyTf =Tsf-25°C.
Tsf beingtheboilingpointofthefood.
IntheMcCabreandTheilediagram,thelineofcuttherectification
equilibriumcurveatthepoint(0.2,0.5)
Wegive:Cp(f)=125J/molKandΔHv(f)=12.5KJ/mol
Cp(D)=102.5J/molKandΔHv(D)=10.25KJ/mol
1/Calculate: N N
,*
D
*
S
therelationshipbetweenthem
* * * *
3/Todeduce: N N
, N, N,
LV GV THE GA
4/DrawtheequilibriumcurveY=f(X)intheMcCabeThielediagram.
5/Tracethepracticalplatesinthisdiagramiftheefficiency
theplateauisof0.5.
*
Q ,Q
*
6/Calculatetheheatflowsofthecondenserandtheboiler:
K B
7/Calculate: Cp(A),Cp(B),ΔHv(A),ΔHv(B)
Exercise-07
A storage tank contains an ideal liquid mixture of two compounds.
organic(A)and(B)completelymisciblewithoutchemicalreactionandwithout
azeotrope.
A25°Cthetotalpressureabovetheliquidmixtureis1atm,while
thatthepartialpressureof(A)east P A
=[Link],a
Weworkwitharefluxrate( ) thatwewildetermine.
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* *
1/CalculatethemolarflowrateofthedistilateN DandthatoftheresidueN S .
2/Yes60%themolarflowrateofcondensedvaporsatthetopofthecolumn N *
GV
*
are used as reflux liquid N LV
, inthen deduce: the rate of
* *
reflux , N LV
, N GV .
3/DrawtheequilibriumcurveY=f(X)intheMcCabeThielediagram
aswellasthefollowinglines:Nutrition,rectification,exhaustion.
4/Determinethenumberoftheoreticaltraysinthiscolumn.
Exercise-08
A column to be corrected is continuously fed by a liquid mixture.
ideal of two compounds(A)and(B)totally miscible without reaction
chemicalandnon-azeotropic.
Themolarcompositionofthemixtureis:60%of(A)and40%of(B).
Beforeenteringintoltothecolumntheload N *
F
heatedby8°topass
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Distillation&Rectification [Link]/GP/UKMO
Q
*
1/Calculate the heat flow rate (J/h) mis-at stake in the exchanger of
F
heat(E).
Q
*
2/Calculatetheheatflowrate (J/h)receivedbythecondenser(K).
K
Q
*
3/Calculatetheheatflowrate (J/h)cededbythereboiler(B).
B
4/Determinethenumberofshelvesinthiscolumn.
Exercise-09
4.10mol/hof
5 amixture idealbinaryliquidoftwoproducts(A)and(B)
completely miscible, must be separated by distillation in a column at
Rectifier. The distillate leaves the reflux exchanger.(K)in the form of a
purityliquidxD,whiletheresiduehasacontentof(A) xS0.1,
weworkwitharefluxrateV=1.5VminWegive:
Theequationofthecorrectionline: Y=0.6X+0.38
Theequationofthesupplyline: Y=3X-0.8
1/Calculate the reflux rate , éwrite the equation of the line of min then
findthecoordinatesofthepoints: P(xp, yp)andE(xE,yE)
2/Calculate: N ,N*
D
*
S
* * * *
3/Deduce: N N
, N, N,
LV GV THE GA
, what is the value of the coefficient of
volatilityα ?
4/Whatisthetheoreticalnumberoftrays?
Exercise-10
8.10mol/hof
5 an ideal binary liquid mixture of two products(A)and(B)
completelymiscibleandwithoutazeotropemustbeseparatedbydistillation
inacolumntocorrect
The food reaches its boiling temperature.(Tsf= T).
f We work
witharefluxrate =1.5
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Thedistillateleavestherefluxexchanger(K)intheformofsteamcontaining
90%in moles of(A)and10%in moles of(B)while the residue does not
containsonly10%inmolesofthevolatileconstituent.
During the distillation, it was noted that the specific heatsqKandqB
havethefollowingvalues:qK31.5KJ/molandqB44KJ/mol
Wearegiven:Teb(A)=160°C,Cp(A)=125J/molKandΔHv(A)=20KJ/mol
Teb(B)=200°C,Cp(B)=150J/molKandΔHv(B)=30KJ/mol
1/DrawthePonchon-Savaridiagram.h=f(x,y)weacceptthatthepace
thedewandboilingcurvesarelinearandwetake( h=0 kJ/mol
forT=0°C
* * * *
2/Calculate: , N, N ,N N,
N N *
D
*
S LV GV GA The
,
3/Findthefollowingtemperatures:Teb(s),Teb(D),Teb(F)
* *
4/Calculate: Q ,Q K B
bytwodifferentmethods,discusstheresults.
Exercise-11
Anidealbinaryliquidmixtureof2completelymiscibleconstituentsAand
B,ofmolefractions:40%inAand60%inB,thismixtureenterintothe
columntodistillatatemperatureof80°Cweworkwitharateof
reflux =1.5 min andXD=0.95,Xs=0.05
WearegivenforA:Cp=100J/molK,ΔHv=20kJ/mol,Teb=100°C,P°=2.4atm
ForB:Cp=150J/molK,ΔHv=30kJ/mol,Te b=120°C,P°=0.8atm
1-DrawthecurveofPonchoSavary:(h=f(x,y))
Weacceptthattheappearanceofthecurvedew and boiling watert litineraryand
wetakefor:T=0°C,h=0J/mol
2-Findtheboilingtemperatureofthemixture(Tsf).
3-Writetheequationofthesupplylineandthatoftherectification.
ofuW
r ritetheequationoftheequilibriumcurvey=f(x)forthismixture.
5-Whatisthenumberoftraystoseparatethismixture?
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Distillation&Rectification [Link]/GP/UKMO
Exercise-12
Duringtheproductionofanhydrideacetic(CHO),
4 6 3 thelatterislocated
distillationinarectifyingcolumn.
The mass charge is664.8 kg/hcontainer55%in moles of acid
acetic.Thischargeentersatatemperatureof106.5°C.
Weworkwitharefluxrate: =1.5 min.
Wegive:
- Thecoefficientofrelativevolatilitybetweenthetwoproductsis4
- The molar fractions of acetic acid in the distillate and in the
residuearerespectively:0.95and0.05
- Theboilingtemperatureofthefoodis127°C.
Composed Aceticanhydride Aceticacid
CHO
4 6 3 CHO
2 4 2
1/Calculate: N N
, *
D
*
S
2/Calculatetherefluxrate( ).
* * * *
3/Todeduce: N N
, N, N,
LV GV The GA
4/DrawtheequilibriumcurveY=f(X)intheMcCabeThielediagram.
5/Drawthetheoreticalplatesinthisdiagram.
*
Q ,Q
*
6/Calculatetheheatflowsofthecondenserandtheboiler:
K B
Exercise-13
Use the Mc Cabre and Theile method to determine the number
theoretical stages of the column to be rectified during theseparation of a
charge of50%in moles of Hexane and Octane with a purity of95%in
molesandaresiduenotcontainingwhat5%inmolesofthelightcomponent.
Thecoefficientofrelativevolatilitybetweenthetwoproductsbeingequalto6.5
57
Distillation&Rectification [Link]/GP/UKMO
Choosearefluxratewithintheoperatingrangeofthediagram.
fromGilly-land,comparethetwomethods.
Log x 1 *x
D S
1 x x D S
TheequationofFunks-Underwood:η ( thit)smin = 1
Log
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