PP311 Distillation

Embed Size (px)

Citation preview

  • 8/8/2019 PP311 Distillation

    1/173

    Distillation

    Distillation is a kind of seperation technique of two or more volatile liquid compunds byusing the difference in boiling points and

    relative volatility. The process takes place in a column, and two

    heat exchangers. In the column two phases, liquid and gas, are

    distributed to enrich the vapor in morevolatile compounds and enrich the liquidphase on less volatile compounds.

    Mass transfer is the key to a successfuldistillation.

  • 8/8/2019 PP311 Distillation

    2/173

    imple or batch or differential dist i l lation

  • 8/8/2019 PP311 Distillation

    3/173

    he Rayleigh Equation

    :for the still see the Figure below les of liquid originally in still

    s of liquid remained in still( )uid composition in still mole fraction of A

    ( )id composition in still mole fraction A,he amount of liquid in the still is L with mole fraction of A in the liquid bei

    ( + ) , ,fferential time t dt a small amount of vapour dL is produced and the( ).in the vapour is y mole fraction The vapour I

    n equi librium .with the residue liquid The amount of liquid in the still is

    ( - ), ( - ).m L to L dL while the liquid composition changed from x to x dx

    :Performing a material balance on A= +Initial amount in still Amount left in still Amount vaporized

    , We have= ( - ) ( - ) +L x dx L dL y dL= - - + +L xL x dL L dx dx dL y dL

    , :Neglecting the term dx dL the equation reduces to= -dx y dL x dL

    - :Re arranging gives the following Integrating from L 1 to L 2, and from x 1 to x 2, we obtainthe :a yle ig h E qu at io n

    http://www.separationprocesses.com/Distillation/Fig013c.htmhttp://www.separationprocesses.com/Distillation/Fig013c.htmhttp://upload.wikimedia.org/wikipedia/en/3/35/Steam_Distillation.JPG
  • 8/8/2019 PP311 Distillation

    4/173

    t ea m di st il la ti on

    ( )he boiling point of pure water 100 C and for( ).henylamine 184 Ct 98 C , he saturated vapour pressures of the two pure:iquids are

    : .enylamine 7 07 kPa: .ater 94 3kPa .ormal atmospheric pressure is 101 325 k

    http://upload.wikimedia.org/wikipedia/en/3/35/Steam_Distillation.JPGhttp://upload.wikimedia.org/wikipedia/en/3/35/Steam_Distillation.JPGhttp://upload.wikimedia.org/wikipedia/en/3/35/Steam_Distillation.JPG
  • 8/8/2019 PP311 Distillation

    5/173

    t ea m d is ti ll at io n

    acuum dis ti ll at ion

    team dist illation with vacuum

  • 8/8/2019 PP311 Distillation

    6/173

    If you boil a liquid mixture C 1, you will get a vapour with composition C 2, which you( ).can condense to give a liquid of that same composition the pale blue lines

    If you reboil that liquid C 2, it will give a vapour with composition C 3. Again you( ).can condense that to give a liquid of the same new composition the red lines

    Reboiling the liquid C 3 will give a vapour still richer in the more volatile( ).component B the green lines You can see that if you were to do this once or twice

    , .more you would be able to collect a liquid which was virtually pure B The secret of getting the more volatile component from a mixture of liquids is

    - - .obviously to do a succession of boiling condensing reboiling operations

    -int composition diagram for a mixture of two liquids at atmospheri)gram for a mixture of two liquids

  • 8/8/2019 PP311 Distillation

    7/173

    Fractional Distillation

    Packed tower

    http://www.energybulletin.net/image/uploads/40234/Fractional_distillation.gifhttp://www.energybulletin.net/image/uploads/40234/Fractional_distillation.gifhttp://www.energybulletin.net/image/uploads/40234/Fractional_distillation.gif
  • 8/8/2019 PP311 Distillation

    8/173

    Packed tower

    ( )Stacked rashig ring top view

  • 8/8/2019 PP311 Distillation

    9/173

    Equipment Designs

    Plate Columns (TrayColumns) Packed Beds

  • 8/8/2019 PP311 Distillation

    10/173

    Plate Columns (Tray

    Columns) It is the most widely used kind of

    distillation column.

    Trays are shaped to maximize theliquid-vapor contact andincrease the mass transfer area.

    Tray types include sieve, bubblecap and valve.

  • 8/8/2019 PP311 Distillation

    11/173

    li id

  • 8/8/2019 PP311 Distillation

    12/173

    vapor

    liquid

  • 8/8/2019 PP311 Distillation

    13/173

  • 8/8/2019 PP311 Distillation

    14/173

  • 8/8/2019 PP311 Distillation

    15/173

  • 8/8/2019 PP311 Distillation

    16/173

  • 8/8/2019 PP311 Distillation

    17/173

  • 8/8/2019 PP311 Distillation

    18/173

    Advantages &

    DisadvantagesAdvantages Least expensive colum

    for diameters greaterthan 0.6m

    The liquid-vapor contactin the plate columns ismore effective than inpacked columns.

    Cooling coils can be

    easily added to theplate column Can handle high liquid

    flow rates.

    Disadvantages Higher pressure drops

    than packed columns

    Foaming can occurbecause the liquid isagitated by the vaporflowing up through it.

  • 8/8/2019 PP311 Distillation

    19/173

    Packed Beds Packings can be provided into 3 types:

    1. random/dumped , 2. regular/stacked and 3.structured/ordered.

    Random/Dumped packing constitutes of bulk inert materials.Random packings are simply dumped into the tower duringinstallation and allowed to fall at random.

    Stacked packing: stacked by hand

    Structured packing: ordered geometry. Generally made of

    perforated corrugated metal, with adjacent sheets arranged sothat liquid liquids spread over their surfaces while vaporflowsthrough channels formed by corrugations.

    Important criteria for packing required are : large interfacial

  • 8/8/2019 PP311 Distillation

    20/173

  • 8/8/2019 PP311 Distillation

    21/173

    S ta cke d ra sh ig rin g( )top view

  • 8/8/2019 PP311 Distillation

    22/173

  • 8/8/2019 PP311 Distillation

    23/173

  • 8/8/2019 PP311 Distillation

    24/173

    Advantages &

    Disadvantages When the

    diameter is lessthan 0.6m it is

    less expensivethan the platecolumn.

    Packing is able tohandlecorrosivematerials.

    Lower pressuredrop than inplate columns.

    Good for

    Can break duringinstallation or dueto thermalexpansion.

    Not cost efficient forhigh liquid flowrates.

    Contact efficiencies

    are decreasedwhen the liquidflow rate is toolow.

    http://www.energybulletin.net/image/uploads/40234/Fractional_distillation.gif
  • 8/8/2019 PP311 Distillation

    25/173

    Fractional DistillationPacked tower

    http://www.energybulletin.net/image/uploads/40234/Fractional_distillation.gifhttp://www.energybulletin.net/image/uploads/40234/Fractional_distillation.gifhttp://www.energybulletin.net/image/uploads/40234/Fractional_distillation.gif
  • 8/8/2019 PP311 Distillation

    26/173

    Packed tower

    ( )Stacked rashig ring top view

    S ?12 Y21 tage

  • 8/8/2019 PP311 Distillation

    27/173

    Stage ?12 Y21 tage

    device where-- 2 phases are brought into intimate contact

    .mass transfer takes place between 2 phases leading to bring them to eqm the phases are separated after mass transfer takes place

    .Sufficient time eqm

    . = =Eqm Stage theoretical stage ideal stage

    :fficiency .fractional approach to eqm which a real stage produces1

    *2

    12

    y y y y

    =

  • 8/8/2019 PP311 Distillation

    28/173

    Bof pressurevapor Aof pressurevapor

    /PPyvolatilitrelative BA ==== B

    B

    A A

    x y

    x y

    AB

    :For binary mixtures x

    = 1 - x A; y

    =

    1 - y A

    relationmequilibriu/

    )1(1

    ==+

    = B A P P x

    x y

    apor liquid equil ibrium

    Numerical measure of the ease with which the components may be separated AB = ,1 separation is not possible

    is t i l lat ion is a kind of separation technique of two or more volatile liquid compounds by using the difference in boiling

    .points and relative volatility

  • 8/8/2019 PP311 Distillation

    29/173

    L X V Y

  • 8/8/2019 PP311 Distillation

    30/173

    L -1 , X -1

    Ln, Xn V +1 , Y +1

    Vn , Yn

    tage n2

    1

    1

    2

    D L

    Dx

    x D L

    L

    y n D

    nn

    n

    n +++=+1

    111

    ++

    +=+

    D

    Dn

    D

    Dn

    R

    x x

    R

    R y

    off ken product tatopof flow

    refluxasreturnedflow

    == D L

    R D

    CONSTANT MOLAL OVERFLOW

    D B F Dx Bx Fx

    D B F

    +=+=

    B L Bx

    x B L

    L y

    m

    Bm

    m

    mm

    =+1 B L

    Bx x

    B L L

    y Bmm =+1

  • 8/8/2019 PP311 Distillation

    31/173

    Operating Lines

    From steady statematerial balances:

    Rectifying section:

    Stripping section:

    Written in terms of theReflux Ratio:

    Rectifying section:

    Stripping section: D L

    Dx x D L

    L y

    n

    Dnn

    nn +++=+1

    B L

    Bx x

    B L

    L y

    m

    B

    mm

    m

    m

    =

    +1

    D L

    R D =

    111 +++=+ D Dn

    D

    Dn R x

    x R R

    y

    B L

    Bx x

    B L

    L y B

    mm

    =

    +1

  • 8/8/2019 PP311 Distillation

    32/173

    2

    1

    1

    2

    1

    L -1 , X -1

    Ln , Xn V +1 , Y +1

    Vn , Yn

    tage n

    1

  • 8/8/2019 PP311 Distillation

    33/173

    =ion of feed moles of l iquid flow in the strippi

  • 8/8/2019 PP311 Distillation

    34/173

    F qV V )1( +=

    qF L L +=

    Dnnn Dx x LVy +=+1 3 F qV V )1(

    = 2

    Bmm Bx x L yV =+1 4

    qF L L = 1 3 4

    +

    = q

    x x

    q

    q y F

    11

    x x x

    y y y

    nm

    nm

    ==

    ==++ 11:t intersect ion

    -l ine equat ion or

    quation for feed line

    =ion of feed moles of l iquid flow in the strippilts rom introduction of each moles of feed

    L V

    Feed plate

    V L

  • 8/8/2019 PP311 Distillation

    35/173

    )(

    1 F b pLT T c

    q +=

    )( d F pV T T cq=

    -he value of q for cold liquid feed is found from the equation

    :he value of q when the feed is superheated vapor

  • 8/8/2019 PP311 Distillation

    36/173

    q = 0 (saturated vapour)q = 1 (saturated liquid)0 < q < 1 (mix of liquid and vapour)q > 1 (subcooled liquid)q < 0 (superheated vapour)

    +

    = q

    x x

    q

    q y F

    11

    ons ruc on nes or c a e

  • 8/8/2019 PP311 Distillation

    37/173

    Lecture 13: McCabe-Theile 37

    ons ruc on nes or c a e-Thiele Method

    Equilibriumcurve

    45 line

    X=x FxB

    y

    yB

    yN

    Stripping Section:Operating line

    xD

    Rectifying Section:Operating line

    q-line

    q=1 q>1

    0

  • 8/8/2019 PP311 Distillation

    38/173

    Bof pressurevapor Aof pressurevapor

    /PPyvolatilitrelative BA ==== B

    B

    A A

    x y

    x y

    AB

    :For binary mixtures x = 1 - x A; y =1 - y A

    relationmequilibriu/)1(1

    ==+

    = B A P P x x

    y

    apor liquid equil ibrium

    Numerical measure of the ease with which the components may be separated AB = ,1 separation is not possible

    is t i l lat ion is a kind of separation technique of two or more volatile liquid compounds by using the difference in boiling

    .points and relative volatility

    n mum e ux or

  • 8/8/2019 PP311 Distillation

    39/173

    39

    n mum e ux orMcCabe-Thiele

    Equilibriumcurve

    xFxB

    y

    yN

    xD

    By returning no exiting vapor as refluxand no exiting liquid as boilup theoperating line intersection is as far tothe left as equilibrium allows.

    Although this is the minimum amountof reflux, it takes infinite stages (notethe pinch point between the operatinglines and equilibrium).

    1min

    min

    +=

    R

    R

    x x

    y x

    q D

    q D

    ),( D D x x),( qq y x

    :n actual practice

    .2 R

    m > 1),phase splitting may occur and a minimum-

    boiling heterogeneous azeotrope forms,having a vaporphase inequilibrium with

    two liquid phases.

    n-butanol/water T-xy

  • 8/8/2019 PP311 Distillation

    106/173

    New Mexico State University

    diagram see animation on course

    website

  • 8/8/2019 PP311 Distillation

    107/173

    New Mexico State University

    created in Aspen Plus

    analyze stripping column 1

  • 8/8/2019 PP311 Distillation

    108/173

    New Mexico State University

    21 BBF +=2bot,B21bot,B1B xBxBFz +=

    ( )( )2bot,B1bot,B

    2bot,BB1 xx

    xzFB

    = ( )( )1bot,B2bot,B1bot,BB

    2 xxxzFB

    =

    rearrange as

    1bot,B1

    B1

    B x1VL

    xVL

    y

    =

  • 8/8/2019 PP311 Distillation

    109/173

    x ,bot1

    x

    1bot,B1

    B1

    B x1VLx

    VLy

    =

    analyze column 2

  • 8/8/2019 PP311 Distillation

    110/173

    New Mexico State University

    2bot,B2

    B2

    B x1VLxVLy =

    1bot,B2B2Bx

    V

    L1x

    V

    Ly

    =

    bottom operating line

    top operating line

    2bot,B2

    B2

    B x1VLx

    VLy

    =

  • 8/8/2019 PP311 Distillation

    111/173

    x ,bot1

    x

    1bot,B1

    B1

    B x1VL

    xVL

    y

    =

    x ,bot2

    x

    1bot,B2

    B2

    B xVL1x

    VLy

    =

    x ,bot2

    Partial water miscibility

  • 8/8/2019 PP311 Distillation

    112/173

    New Mexico State University

    Partial water miscibility Partially miscible

    system of organicand water form asingle phase only

    at very high, orvery low waterconcentrations.

    Water is the morevolatilecomponent insuch systems.

    dry organic

    organic phase

    wate

    rphase

    feed

    Partial water miscibility

  • 8/8/2019 PP311 Distillation

    113/173

    New Mexico State University

    Partial water miscibility

    dry organic

    organic phase

    wate

    rphase

    feed

    iquid phase mole fraction water

    vapor

    phase

    mole

    fraction

    water

    Partial water miscibility

  • 8/8/2019 PP311 Distillation

    114/173

    New Mexico State University

    Partial water miscibility In each phase,

    Raoult's can beapplied tomiscible

    materials, whileHenry's can beapplied to thenonmiscible.

    aqueous phase

    organic phase

    dry organic

    organic phase

    wate

    rphase

    feed

    ( ) -aaaa xVPp = a-ooo xHp =

    ( ) oooo xVPp = oaaa xHp =

    Partial water miscibility

  • 8/8/2019 PP311 Distillation

    115/173

    New Mexico State University

    Partial water miscibility Equate partial

    pressures of thesame phase, solvefor Henry's

    constant: H calculated from known

    solubilities d ry org an ic

    org an ic p h ase

    w aterp h a se

    feed( )

    oa

    -aaaa

    x

    xVPH

    = ( )ao

    -oooo

    x

    xVPH

    =

    ( ) -aaaa xVPp = a-ooo xHp =( ) oooo xVPp = oaaa xHp =

    Partial water miscibility

  • 8/8/2019 PP311 Distillation

    116/173

    New Mexico State University

    Partial water miscibility Estimations of of

    water in organicphase:

    d ry org an ic

    org an ic p h ase

    w aterp h a se

    feed

    ( )( )( ) oao

    aaa

    o

    aoo,a xVP

    xVPVPH

    ==

    ( )( )

    ( )( )ooo

    aaa

    oato

    aata

    ooo

    oaaoo,a

    xp

    xp

    xpp

    xppxyxy

    ==

    =

    ( ) oooo xVPp = oaaa xHp =( ) -aaaa xVPp = a-ooo xHp =

    Steam Distillation

  • 8/8/2019 PP311 Distillation

    117/173

    New Mexico State University

    Steam Distillation Steam added directly to distilling

    organic mixture to reduce therequired temperature and to keepsuspended any solids that may bepresent.

    Separation of volatiles fromnonvolatiles.

    Process results in a pseudo-binary

    distillation with the water and volatileorganics forming a heterogeneousazeotrope.

    Common in purification of essential oils ,coal or anics waste solvent

    Batch Steam Distillation

  • 8/8/2019 PP311 Distillation

    118/173

    New Mexico State University

    Batch Steam Distillation

    Continuous Steamll

  • 8/8/2019 PP311 Distillation

    119/173

    New Mexico State University

    Distillation

    w ater

    feed

    vo la tile o rg an ic

    steam

    w ater

    o rg an ics

    Steam Distillation

  • 8/8/2019 PP311 Distillation

    120/173

    New Mexico State University

    Steam Distillation With two liquid phases present and in

    equilibrium, compositions of the liquidphases are fixed by their mutualsolubilities.

    As the amount of aqueous or organicphase is increased, phaseconcentrations do not change.

    Since each phase exerts its own vapor

    pressure, the vapor composition willbe constant regardless of the averageliquid composition.

    A heterogeneous azeotrope results.

    Steam Distillation

  • 8/8/2019 PP311 Distillation

    121/173

    New Mexico State University

    Steam Distillation

    Water and organic phases exertseparate vapor pressures on thetotal pressure:

    Consider the case where 1 of theorganics in the mixture is a volatile species:

    Liquid phase compositions set byequilibrium. When total pressure isfixed, temperature is set (i.e.,bubble point calculation), and

    toa ppp =+

    ( ) ( ) taaaovo pxVPxVP =+

    tii ppy =

    Steam Distillation

  • 8/8/2019 PP311 Distillation

    122/173

    New Mexico State University

    Steam Distillation

    Ratio of volatile organic to water in thevapor is

    If several volatile organics exist in theorganic phase, y v,o and p v,o are the

    sums of the respective values for allthe organics. The total moles of steam required is n w

    plus the amount condensed to heat

    ( )( ) o,vot

    o,vo

    o,vt

    o,v

    a

    o,v

    a

    o,v

    a

    o,v

    xVPpxVP

    ppp

    pp

    yy

    nn

    ==== tii ppy =

    Complex ternary distillation

  • 8/8/2019 PP311 Distillation

    123/173

    New Mexico State University

    systems A distillation curve is a plot of mole

    fractions on every tray fordistillation at total reflux.

    Consider column numbered from topdown Bubble point calc

    at every stage Total reflux operating line

    Solution at every stage

    ( ) 1xx,p, TK yc

    1i

    j,i j,ii

    c

    1i

    j,i ====

    1 j,i j,i xy =

    ( )=

    = c

    1i j,iref i

    j,iref i1 j,i

    x

    xx

    Residue Curves

  • 8/8/2019 PP311 Distillation

    124/173

    New Mexico State University

    Residue Curves

    A residue curve is a triangulardiagram that displaysconcentrations for a 1-stagebatch distillation operated todryness f(Nstage ).

    Residue curves follow the liquidresidue composition in the still.

    Different residue lines result fromdifferent starting compositions. Acollection of these curves for agiven ternary system is called a

    Residue Curves

  • 8/8/2019 PP311 Distillation

    125/173

    New Mexico State University

    Residue Curves

    During distillation, molar liquid holdup Hdrops.

    Unsteady state mass and component

    balances: where V is molar rate

    at which vapor leaves Rearrange

    System of i ODEs must be solvesimultaneously

    For constant , recursion relations can

    VdtdH = ( ) ii Vydt

    Hxd =

    ( )( )iii yxHtV

    dtdx =

    ( )

    +=

    =+

    c

    1ik,iref ik,iref ik,ik,i1k,i xxxhxx

  • 8/8/2019 PP311 Distillation

    126/173

    New Mexico State University

    A ternary residue map of a heterogeneous system

    viewed as three binary

    Txy diagrams

  • 8/8/2019 PP311 Distillation

    127/173

    New Mexico State University

    eatures of a esidue curve map

    Residue Map Characteristics

  • 8/8/2019 PP311 Distillation

    128/173

    New Mexico State University

    p

    If we assign direction of the residuecurves as from the startingcomposition to the ending

    composition, then the arrow oneach curve points from a lowerboiling component or azeotropeto a higher boiling component orazeotrope .

    Residue Map Characteristics

  • 8/8/2019 PP311 Distillation

    129/173

    New Mexico State University

    p

    The presence of azeotropes cancreate distillation boundaries which cannot be crossed by a residuecurve.Distillation boundaries represent theresidue curve on which the light orstarting residue composition is a

    lower boiling pure component orazeotrope and the heavy or endingcomposition residue is a higher purecomponent or azeotrope.

    Residue Map Characteristics

  • 8/8/2019 PP311 Distillation

    130/173

    New Mexico State University

    p

    Any given pure component point orazeotrope will be connected to somebut not all other pure component

    points and azeotropes on the graph. Those that are connected formdistillation boundaries. Theseboundaries are thermodynamic innature.

    Residue Map terminologyN d R id b i d d

  • 8/8/2019 PP311 Distillation

    131/173

    New Mexico State University

    p gy Node : Residue curves begin and end at

    nodes. Stable node : The component or azeotrope

    with the highest boiling point in the region.All the residue curves in the region point to

    (terminate) at this point. Unstable node : The component or

    azeotrope with the lowest boiling point inthe region.

    Saddle : Residue curves move toward andthen away from saddles. Pure componentsand azeotropes which have a boiling pointbetween the stable and unstable nodes are

    Residue curvesT f t ti i t f

  • 8/8/2019 PP311 Distillation

    132/173

    New Mexico State University

    Types of stationary points of three-component mixtures: (a) 1 component stablenode, (b) 1 component unstable

    node, (c) 1 component saddle, (d) 2-component stable

    node, (e) 2-component unstable

    node, (f) 2-component saddle, (g) 3-component stable

    node, (h) 3-component unstable

    node

    Residue curvesR id b d

  • 8/8/2019 PP311 Distillation

    133/173

    New Mexico State University

    Residue-curve maps can be used to

    make preliminary estimates of regions of feasible productcompositions for distillation of non-ideal ternary mixtures.

    Residue curvesP d t i d t i d b

  • 8/8/2019 PP311 Distillation

    134/173

    New Mexico State University

    Product regions are determined bysuperimposing a column material balanceon the curve map diagram.

    If a straight line is drawn that connectsdistillate and bottoms compositions, that

    line must pass through the feedcomposition at some intermediate point tosatisfy overall and component materialbalances.

    For such a material balance line, thedistillate and bottoms compositions mustlie on the same residue curve.

    S

    ever Rule

    = /F 100 kmol hr

  • 8/8/2019 PP311 Distillation

    135/173

    New Mexico State University

    F

    /F 100 kmol hr= /S 52 kmol hr

    M

    152100

    15252

    D

    B

    feasible product regions, zeotropicsystems:

  • 8/8/2019 PP311 Distillation

    136/173

    New Mexico State University

    H

    L I

    systems:i. Find the limiting distillate

    composition point for theregion. Draw a linefrom this point through thefeed composition, to theopposite sideof the map. This pointrepresentsthe bottoms composition withthe lowest amount of low boiler possible forthe limiting distillatecomposition(material balance line M 1).

    F

    M1

    feasible product regions, zeotropicsystems:

  • 8/8/2019 PP311 Distillation

    137/173

    New Mexico State University

    H

    L I

    systems:ii. Find the limiting bottoms

    composition point for theregion. Draw a linefrom this point, through thefeed composition, to theopposite sideof the map. This pointrepresentsthe distillate composition withthe lowest amount of highboilerpossible for the limitingbottoms composition(material balance line M 2).

    F

    M1

    M2

  • 8/8/2019 PP311 Distillation

    138/173

    feasible product regions,azeotropic systems

  • 8/8/2019 PP311 Distillation

    139/173

    New Mexico State University

    azeotropic systemsFor azeotropic systems with distillation

    boundaries, a feasible product region can befound for each region.

  • 8/8/2019 PP311 Distillation

    140/173

    New Mexico State University

    ernary

    e t e r o g e n e o u sA ze o tro p e

    / ,Ethanol Water using Tolueneentrainer

  • 8/8/2019 PP311 Distillation

    141/173

    New Mexico State University

    Ethanol/Water withToluene entrainer

  • 8/8/2019 PP311 Distillation

    142/173

    New Mexico State University

    Extractive Distillation

  • 8/8/2019 PP311 Distillation

    143/173

    New Mexico State University

    used for theseparationof azeotropesand close-boiling

    mixtures. solvent is

    added tothe

    column, forwhich oneof thecomponents (B) isselectivel

    1recycleso lvent

    AProduct

    2

    m ake upsolven t

    fe ed

    BProduct

    Azeotropic Distillation w/ addedSolventh azeotrope

  • 8/8/2019 PP311 Distillation

    144/173

    New Mexico State University

    Solvent When ahomogeneousazeotrope isformed, addedsolvent orentrainer canbe used to

    produce abinary orternaryazeotrope whichcan be used toseparate themixture.

    The exact natureof the flowsheetdepends on theequilibrium

    behavior of the

    azeot opic

    column

    stripper

    B

    feed

    A

    azeotropephase

    separation

    makeupentrainer

    Reactive DistillationWh i i l h

  • 8/8/2019 PP311 Distillation

    145/173

    New Mexico State University

    When reactions occur in a column, the

    mass and energy balances must bemodified to include reaction terms. Often used to separate products

    simultaneously during chemicalreaction to drive an equilibriumreaction in the direction of theproducts.

    Reactive DistillationCA DA DCBA ++

  • 8/8/2019 PP311 Distillation

    146/173

    New Mexico State University

    volat i l

    product

    feed

    CAC

    b le ed

    -onvolat i l

    product

    feed

    DAb le ed

    D

    & D-on

    volat i le

    B

    DCBA ++C

    D

    A

    Reactive DistillationA l b l f t j i

  • 8/8/2019 PP311 Distillation

    147/173

    New Mexico State University

    A general mass balance for stage j is

    where the reaction term r j is positive

    for product components of thereaction. A rate law must be substituted into this

    equation.

    j j j1 j1 j1 j1 j j j j j rzFxLyVxLyV +=+

  • 8/8/2019 PP311 Distillation

    148/173

    1

    m

    2

    1

    nD

    +m 1

    B

    .e cti fy ing s ec

    .tr ipping sec eed plate

  • 8/8/2019 PP311 Distillation

    149/173

  • 8/8/2019 PP311 Distillation

    150/173

  • 8/8/2019 PP311 Distillation

    151/173

  • 8/8/2019 PP311 Distillation

    152/173

  • 8/8/2019 PP311 Distillation

    153/173

  • 8/8/2019 PP311 Distillation

    154/173

  • 8/8/2019 PP311 Distillation

    155/173

  • 8/8/2019 PP311 Distillation

    156/173

  • 8/8/2019 PP311 Distillation

    157/173

  • 8/8/2019 PP311 Distillation

    158/173

  • 8/8/2019 PP311 Distillation

    159/173

  • 8/8/2019 PP311 Distillation

    160/173

  • 8/8/2019 PP311 Distillation

    161/173

  • 8/8/2019 PP311 Distillation

    162/173

  • 8/8/2019 PP311 Distillation

    163/173

  • 8/8/2019 PP311 Distillation

    164/173

  • 8/8/2019 PP311 Distillation

    165/173

  • 8/8/2019 PP311 Distillation

    166/173

  • 8/8/2019 PP311 Distillation

    167/173

  • 8/8/2019 PP311 Distillation

    168/173

    d ll l d h f f l l f

    http://en.wikipedia.org/wiki/Essential_oilhttp://en.wikipedia.org/wiki/Essential_oilhttp://en.wikipedia.org/wiki/Essential_oil
  • 8/8/2019 PP311 Distillation

    169/173

    Steam distillation is employed in the manufacture of essential oils , for,instance perfumes . ,In this method steam is passed through the plant material

    .containing the desired oils It is also employed in the synthetic procedures.of complex organic compounds Eucalyptus oil and orange oil are obtained by.this method on the industrial scale

    Steam distillation is also widely used in petroleum refineries andpetrochemical " ".plants where it is commonly referred to as steam stripping

    Other industrial uses of steam distillation include the production of consumer food products such as sprayable or aerosolized condiments such as sprayable mayonnaise

    thestrtedpofthtliid v a p o u r p r e s s u r e o f a n a g i t a t e d m i x t u r e w o u l d j u s t b e t h e s u m o f t h e s e - i n o t h e r w o r d s , 1 0 1 . 3 7 k P a

    o i n t o f t h e m i x t u r e o i l w h e n t h e i r v a p o u r p r e s s u r e b e c o m e s e q u a l t o t h e e x t e r n a l p r e s s u r e . N o r m a l a t m o s p h e r i c p r e s s u r e i s 1 0 1 . 3 2 5 k P a . t h a t w i t h t h e f i g u r e w e h a v e j u s t g o t f o r t h e t o t a l v a p o u r p r e s s u r e o f a m i x t u r e o f w a t e r a n d p h e n y l a m i n e a t 9 8 C . I t s t o t a l v a p o u r

    i s f r a c t i o n a l l y h i g h e r t h a n t h e n o r m a l e x t e r n a l p r e s s u r e . n s t h a t s u c h a m i x t u r e w o u l d b o i l a t a t e m p e r a t u r e j u s t a s h a d e l e s s t h a n 9 8 C - i n o t h e r w o r d s l o w e r t h a n t h e b o i l i n g p o i n t o f p u r e 0 C ) a n d m u c h l o w e r t h a n t h e p h e n y l a m i n e ( 1 8 4 C ) .

    http://en.wikipedia.org/wiki/Essential_oilhttp://en.wikipedia.org/wiki/Essential_oilhttp://en.wikipedia.org/wiki/Perfumeshttp://en.wikipedia.org/wiki/Perfumeshttp://en.wikipedia.org/wiki/Eucalyptus_oilhttp://en.wikipedia.org/wiki/Orange_oilhttp://en.wikipedia.org/wiki/Oil_refineryhttp://en.wikipedia.org/wiki/Petrochemicalhttp://en.wikipedia.org/wiki/Petrochemicalhttp://en.wikipedia.org/wiki/Oil_refineryhttp://en.wikipedia.org/wiki/Orange_oilhttp://en.wikipedia.org/wiki/Eucalyptus_oilhttp://en.wikipedia.org/wiki/Perfumeshttp://en.wikipedia.org/wiki/Essential_oil
  • 8/8/2019 PP311 Distillation

    170/173

    phenylamine 7.07 kPawater 94.30 kPa

    o u r p r e s s u r e o f t h e m i x t u r e t h a t t h e m i x t u r e i s b e i n g a g i t a t e d , t h e n b o t h o f t h e l i q u i d s w i l l b e i n e q u i l i b r i u m w i t h t h e i r v a p o u r s . T h e t o t a l v a p o u r p r e s s u r e i s t h e n

    e s u m o f t h e i n d i v i d u a l v a p o u r p r e s s u r e s :

    p o r e f e r s t o t h e s a t u r a t e d v a p o u r p r e s s u r e o f t h e p u r e l i q u i d . a t t h i s i s i n d e p e n d e n t o f t h e a m o u n t o f e a c h s o r t o f l i q u i d p r e s e n t . A l l y o u n e e d i s e n o u g h o f e a c h s o t h a t b o t h c a n e x i s t i n e q u i l i b r i u m

    v a p o u r . p l e , p h e n y l a m i n e a n d w a t e r c a n b e t r e a t e d a s i f t h e y w e r e c o m p l e t e l y i m m i s c i b l e . ( T h a t i s n ' t a c t u a l l y t r u e , b u t t h e y a r e n e a r e n o u g h e t o b e u s a b l e a s a n e x a m p l e . ) t h e s a t u r a t e d v a p o u r p r e s s u r e s o f t h e t w o p u r e l i q u i d s a r e :

    t ea m d is ti ll at io n is a special type of distillation (aseparation process ) for temperature sensitive materials like naturalaromatic .compoundsMany organic compounds tend to decompose .at high sustained temperaturesSeparation by normal distillation would then not be an option so water

    http://www.tutorgig.com/ed/Distillationhttp://www.tutorgig.com/ed/Separation_processeshttp://www.tutorgig.com/ed/Separation_processeshttp://www.tutorgig.com/ed/Aromaticityhttp://www.tutorgig.com/ed/Aromaticityhttp://www.tutorgig.com/ed/Organic_compoundhttp://www.tutorgig.com/ed/Chemical_decompositionhttp://www.tutorgig.com/ed/Chemical_decompositionhttp://www.tutorgig.com/ed/Organic_compoundhttp://www.tutorgig.com/ed/Aromaticityhttp://www.tutorgig.com/ed/Separation_processeshttp://www.tutorgig.com/ed/Distillation
  • 8/8/2019 PP311 Distillation

    171/173

    ,Separation by normal distillation would then not be an option so wateror steam .is introduced into the distillation apparatus By adding water

    ,or steam the boiling points ,of the compounds are depressed allowing them,to evaporate at lower temperatures preferably below the temperatures at.which the deterioration of the material becomes appreciable If the

    ,substances to be distilled are very sensitive to heat steam distillation can also be combined with vacuum distillation . After distillation the

    , -vapors are condensed as usual usually yielding a two phase system of, .water and the organic compounds allowing for simple separation

    Principle When a mixture of two practically immiscible liquids is heated while being

    ,agitated to expose the surfaces of both the liquids to the vapor phase each constituent independently exerts its own vapor pressure as a function of

    . ,temperature as if the other constituent were not present Consequently thef h h l i B ili b i h h f

    http://www.tutorgig.com/ed/Steamhttp://www.tutorgig.com/ed/Boiling_pointhttp://www.tutorgig.com/ed/Vacuum_distillationhttp://www.tutorgig.com/ed/Vacuum_distillationhttp://www.tutorgig.com/ed/Phase_(matter)http://www.tutorgig.com/ed/Phase_(matter)http://www.tutorgig.com/ed/Phase_(matter)http://www.tutorgig.com/ed/Vacuum_distillationhttp://www.tutorgig.com/ed/Boiling_pointhttp://www.tutorgig.com/ed/Steamhttp://www.tutorgig.com/ed/Miscibilityhttp://www.tutorgig.com/ed/Vapor_pressurehttp://www.tutorgig.com/ed/Vapor_pressurehttp://www.tutorgig.com/ed/Vapor_pressurehttp://www.tutorgig.com/ed/Vapor_pressurehttp://www.tutorgig.com/ed/Miscibility
  • 8/8/2019 PP311 Distillation

    172/173

    .vapor pressure of the whole system increases Boiling begins when the sum ofthe partial pressures of the two immiscible liquids just exceeds theatmospheric pressure ( ). ,approximately 101 kPa at sea level In this way many organic compounds insoluble in water can be purified at a temperature well

    . ,below the point at which decomposition occurs For example the boiling point of bromobenzene ,is 156 C and the boiling point of water is 100 C

    . ,but a mixture of the two boils at 95 C Thus bromobenzene can be easily.distilled at a temperature 61 C below its normal boiling point

    Applications Steam distillation is employed in the manufacture of essential oils , for,instance perfumes . ,In this method steam is passed through the plant

    .material containing the desired oils It is also employed in the synthetic.procedures of complex organic compounds Eucalyptus oil and orange oil are

    .obtained by this method on the industrial scale Steam distillation is also widely used in petroleum refineries and

    petrochemical " ".plants where it is commonly referred to as steam stripping Other industrial uses of steam distillation include the production of consumer food products such as sprayable or aerosolized condiments such as

    .sprayable mayonnaise

    h V l til A id Still i l t ifi t th i i d t f

    http://www.tutorgig.com/ed/Partial_pressurehttp://www.tutorgig.com/ed/Atmospheric_pressurehttp://www.tutorgig.com/ed/Bromobenzenehttp://www.tutorgig.com/ed/Essential_oilhttp://www.tutorgig.com/ed/Essential_oilhttp://www.tutorgig.com/ed/Perfumeshttp://www.tutorgig.com/ed/Perfumeshttp://www.tutorgig.com/ed/Eucalyptus_oilhttp://www.tutorgig.com/ed/Eucalyptus_oilhttp://www.tutorgig.com/ed/Eucalyptus_oilhttp://www.tutorgig.com/ed/Orange_oilhttp://www.tutorgig.com/ed/Oil_refineryhttp://www.tutorgig.com/ed/Petrochemicalhttp://www.tutorgig.com/ed/Petrochemicalhttp://www.tutorgig.com/ed/Oil_refineryhttp://www.tutorgig.com/ed/Orange_oilhttp://www.tutorgig.com/ed/Eucalyptus_oilhttp://www.tutorgig.com/ed/Eucalyptus_oilhttp://www.tutorgig.com/ed/Perfumeshttp://www.tutorgig.com/ed/Essential_oilhttp://www.tutorgig.com/ed/Bromobenzenehttp://www.tutorgig.com/ed/Atmospheric_pressurehttp://www.tutorgig.com/ed/Partial_pressure
  • 8/8/2019 PP311 Distillation

    173/173

    ,he Volatile Acid Still is a glass apparatus specific to the wine industry forthe etermination of volatile acids .in wine by steam distillation Our

    standard glass VA still includes an aspirator pump to suck the sample out, .after completion of the analysis allowing for rapid cycling of samples Its precursor was the glass Cash Still and many people refer to these stills

    " " " ". ,generically as Cash still or RD80 For historical interest see our notes on the istory of the VA Still . &Adams Chittenden Scientific Glass

    ,manufactures both the VA Still and Cash Still offering an exceptionally high, ,quality product with a new m pr ov ed c or ds et nd connector , and a large

    , .capacity condenser at competitive prices We have been making VA Stills and. ;Cash Stills our entire glassblowing careers We are proud of our stills they" " .have a high Wow factor and demonstrate our skills and quality For

    ,instructions on setup and operation see the Instructions ." " We were entertained to hear a SoundClip on NPR's Talk of the Nation on

    earing a Wine's Acidity .featuring the sound of the VA Still Thanks to.Patrick Taylor of Cuneo Cellars for permission to use his words and sounds

    http://www.adamschittenden.com/213Why.phphttp://www.adamschittenden.com/214History.phphttp://www.adamschittenden.com/212Improvements.phphttp://www.adamschittenden.com/212Improvements.phphttp://www.adamschittenden.com/215AdamsChittendenVAInstructions.phphttp://www.adamschittenden.com/215AdamsChittendenVAInstructions.phphttp://www.npr.org/templates/story/story.php?storyId=5581768http://www.npr.org/templates/story/story.php?storyId=5581768http://www.adamschittenden.com/215AdamsChittendenVAInstructions.phphttp://www.adamschittenden.com/212Improvements.phphttp://www.adamschittenden.com/212Improvements.phphttp://www.adamschittenden.com/212Improvements.phphttp://www.adamschittenden.com/214History.phphttp://www.adamschittenden.com/213Why.php