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    Column Pressure

    How do we choose the operating pressure

    of a column?

    Usually based on:

    (i) Temperature of overhead condenser

    (ii) Temperature at bottom of column

    Turton, 3rd edition

    Column Pressure

    1. If possible use cheapest coolant streamavailable cooling water (or air) in thecondenser

    2. If by following (1), the bottom temperature is

    too high then reduce pressure so that bottomtemperature is acceptable and choosewarmest coolant (refrigerant)

    Turton, 3rd edition

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    Column Pressure - example

    A column separates A (light) from B (heavy). At whatpressure would you operate this column?

    log P*(mmHg) =a -b/(c+T)

    A a = 6.80398 b = 803.810

    c = 246.990

    B a = 6.80896 b = 935.860

    c= 238.730

    Turton, 3rd edition

    Vapor pressure

    Turton, 3rd edition

    Distilllation ColumnOverhead Condenser

    Alog P*(mmHg) = 6.80398 - 803.810 /(246.990 + 49)

    = 4.0975

    P* = 12,516 mmHg = 242 psi

    What is pressure and temperature at bottom of the column?

    Q

    T

    32

    40-45

    49

    Top product is pure A

    Assume vapor condenses to 49 C (120 F)

    T-Q diagram

    Condensing media:For water inlet 32 C (90 F)Maximum outlet: 45 C (115 F)

    X

    water

    3240-45

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    What does DPtraydepend on?

    DPtray= rlg(hw+ hcr) + krgvo2

    Often this is the dominantterm

    DPtray is not a function of theoperating conditions.

    Turton, 3rd edition

    Weir height Contribution from gas flowthrough tray orifices

    DPtray

    Assume DPcol= 5 psi : Pressure drop per tray is on the order of 7.6cm (3 in) of water = 0.0007 bar (0.1 psi)

    Pbot= 242 + 5 = 247 psia = 12,770 mmHg

    For B bottom product:

    a - b/(c+T) = log(12,770)

    T=b/[a- log(12,770)]-C= 935.860/[6.80896 log(12,770)] - 238.730

    T = 107.5C

    Top product is pureA

    Bottom product is pure B

    DPcol= nDPtray Pbot= Ptop+ DPcol

    Turton, 3rd edition

    Distillation Column

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    R.Turton and J.A. Shaeiwitz -

    Copyright 2008

    7

    Number oftrays, n= 31

    Turton, 3rd edition

    Column PressureAcrylic Acid from Propylene

    68

    0.16

    0.07

    47

    Why is column operatingunder vacuum?

    Acrylic Acid production

    Why is column operating under vacuum?

    Polymerization of acrylic acid above 90C

    Must reduce pressure so that Pbot:P*(acrylic acid) =a-b/(c+ 89C)P=0.16 bar

    What about DPcol?DPcol= Pbot Ptop=0.16 - 0.07 = 0.09 bar

    Number of trays, n= 31DPtray= 0.09/31 = 0.003 bar (= 1.2 of acrylic acid)

    Turton, 3rd edition

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    McCabe-Thiele Analysis

    y

    x

    xD/(1+R)

    xD

    Feed line slope

    = -q/(1-q)

    xB xF

    Turton, 3rd edition, ch. 18

    1

    RR

    xyyx

    LDL

    VL

    FD

    FD

    xxy

    11

    FD

    FD

    xy

    yxR

    min

    R

    R

    V

    L

    achial

    1

    Column Pressure and

    TemperatureReboiler temp ~ boiling point of

    heavy component

    Condenser temp ~boiling pointof light component

    Increasing column pressure:

    increases both temp.decreases relative volatility and

    hence make separation more

    difficult

    Slope = L/V

    Slope = L/V V

    D

    B

    V

    F

    L = B + V

    L = V - D

    R = L/D

    R = L/B

    L

    L

    reflux

    Boil-up

    Distillation of Benzene from Toluene

    Flows in kmol/hComposition in benzene mole fractionReflux ratio=2.38Pressure = 2 bar

    Benzene recovery:G=DXD/(FxF) = 30(0.885)/(100(0.321))=0.827

    Diameter = 0.83 mContains 20 sieve plates with 0.61 m plate spacing

    Feed is introduced in plate 13

    Tower operates with a reflux ratio of 2.38

    = 70 (mass balance)XB=0.079

    1

    N

    Analyze this operation: Number of theoretical plates?

    where is the feed added? Column oversized/undersized? Effect ofchanging L/V?

    McCabe-Thiele construction:

    Speed of computation usingMcCabe-Thiele method is far

    slower than for process

    simulators.However, it remains an important

    analytical tool.

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    Distillation of Benzene from Toluene

    Flows in kmol/hComposition in benzene mole fractionReflux ratio=2.38Pressure = 2 bar

    Benzene recovery:

    G=DXD/(FxF) = 30(0.885)/( 100(0.321))=0.827

    Diameter = 0.83 mContains 20 sieve plates with 0.61 m plate spacingFeed is introduced in plate 13Tower operates with a reflux ratio of 2.38

    = 70 (mass balance)XB=0.079

    McCabe-Thiele construction:

    McCabe-Thiele construction yields 13 THEORETICAL stages (12 + reboiler).Average plate efficiency is 12/20=0.6 (60%)

    Feed is added in plate 13 (actual). Equivalent to theoretical plate number 8: 13x0.6=8

    R=L/D

    q=fraction of feed that is liquid

    Turton, 3rd edition, ch. 18

    1

    N

    XB=0.079

    XD=0.885

    ZF=0.321

    Some observations from previous process:

    -Feed is not being introduced at optimum location inthe column. The optimal location is plate 6(theoretical) or 10 (6/0.6) actual

    -Separation steps near the feed plate are small

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    Flows in kmol/hComposition in benzene mole fraction

    Reflux ratio=2.38Pressure = 2 bar

    G=DXD/(FxF) = 30(0.885)/ (100(0.321))=0.827

    Diameter = 0.83 mContains 20 sieve plates with 0.61 m plate spacingFeed is introduced in plate 13Tower operates with a reflux ratio of 2.38

    = 70 (mass balance)XB=0.079

    McCabe-Thiele construction:

    R=L/Dq=fraction of feed that is liquid

    Current situation (feed at plate 13 vs optimum atplate 10): The tower appears to

    be oversized for the

    present separation. Itcould process a

    lower quality of feedand improve

    benzene recovery

    Turton, 3rd edition, ch. 18

    There are more than the optimum # of stages in therectifying (top) section: This means that the tower

    was designed to process a lower concentration offeed or to produce a higher concentration distillatestream (benzene)

    Flows in kmol/hComposition in benzene mole fractionReflux ratio=2.38Pressure = 2 bar

    G=DXD/(FxF) = 30(0.885)/ (100(0.321))=0.827

    = 70 (mass balance)XB=00.79

    McCabe-Thiele construction:

    R=L/Dq=fraction of feed that is liquid

    Operating line moves away from equilibrium this increases separation ofeach stage (larger step size).

    Turton, 3rd edition, ch. 18

    Increasing L/V:

    The concentration of benzene in the bottom stream (xB) will be lowered

    If xDremains the same:

    Increasing L/V:

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    Scale-up/down of ColumnMcCabe-Thiele Analysis

    y

    x

    xD/(1+R)

    Feed line slope= -q/(1-q)

    xF xD

    xB

    What happenswhen refluxratio increasesbut number oftrays stays thesame?

    Turton, 3rd edition, ch. 18

    Flows in kmol/hComposition in benzene mole fraction

    Reflux ratio=2.38Pressure = 2 bar

    G=DXD/(FxF) = 30(0.885)/ (100(0.321))=0.827

    Diameter = 0.83 mContains 20 sieve plates with 0.61 m plate spacingFeed is introduced in plate 13Tower operates with a reflux ratio of 2.38

    = 70 (mass balance)XB=0.079

    McCabe-Thiele construction:

    R=L/Dq=fraction of feed that is liquid

    Computer simulation:Flowrate(kmol/h)

    Mole fraction Concentration

    Inputs

    F 100 zF 0.321

    Outputs from Simulation

    L0 71.5 X0 0.885

    VN+1 96.4 yN+1 0.079

    V1 101.5 Y1 0.885

    Ln 166.4 xN 0.079Turton, 3rd edition, ch. 18

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    Mill Situation

    (see working example)

    You are told that benzene in feed will varybetween 25 and 40%. However, you arerequired to keep Dand xDconstant.

    You are asked to asses the effect of suchchanges in feed concentration on theoperation of the distillation process

    Performance

    diagrams

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    Mill Situation:

    You are told that benzene in feed will vary between 25 and45%. However, you are required to keep Dand xDconstant.

    Reflux is chosen as dependentvariable (most common way to

    regulate the performance of adistillation column)

    Observations (after running anumber of simulations):

    For constant recovery G:

    As zFincreases, the reflux L0decreases.

    For a constant feed

    concentration zF:As Gincreases, the refluxincreases

    You can set up a number of other situations

    (estimate reflux rate to obtain desireddistillate conditions, etc.)

    Example: Find changes needed to get 90%

    recovery at same zF.

    Refluxrate

    Feed mole fraction, zF

    Constant recovery, G

    Benzenerecovery:

    Base Case

    Weeping gas velocity: 0.35 m/s

    Flooding gas velocity: 1.07 m/s

    Scale-up/down of ColumnOperation

    What other factors must we consider whencolumn operations change?

    Capacity of the column to process more or less

    material is limited (bounded) by:

    Flooding (scale-up)

    Weeping (scale-down)

    Turton, 3rd edition, ch. 18

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    Scale-up/down of ColumnOperation

    J.D. Seader and E.J. Henley, Separation Process Principles, John Wiley and Sons, NY 1998

    scaledown

    scaleup

    Benzene

    recovery:

    Base Case

    Weeping gas velocity: 0.35 m/s

    Flooding gas velocity: 1.07 m/s

    Example: Findchanges needed toget 90% recoveryat same zF (0.321)

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    Benzene

    recovery:

    Base Case

    Weeping gas velocity: 0.35 m/s

    Flooding gas velocity: 1.07 m/s

    Turton, 3rd edition, ch. 18

    Example: Findchanges needed toget 90% recoveryat same zF (0.321)

    New Feed rate:F=xDD/zFG= 91.9

    New reflux L0(from figure):

    L0=81 (point b)

    The distillation can be

    operated at a recoveryof 0.9; this reduces the

    feed that can be

    processed by 8.1%

    keep D and xDconstant

    Benzene

    recovery:

    Weeping gas velocity: 0.35 m/s

    Flooding gas velocity: 1.07 m/s

    Example: Find the

    maximum recoverypossible for thedistillation equipment for

    a feed concentrationzF=0.275

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    Scale-up/down of Column

    What if we want to change the feed rate to the

    column?

    If we want tokeep all the purities the samethen the reflux ratio must stay the same.

    Scale-down

    How do we adjust the condenser and reboilerso as to keep the reflux ratios the same? (tokeep all the product purities the same

    V

    D

    B

    V

    F

    L = B + V

    L = V - D

    R = L/D

    R = L/B

    L

    L

    reflux

    Boil-up

    Turton, 3rd edition, ch. 18

    Top of column

    QD= VlD=D(1+R)lD

    Bottom of column

    QB=VlB=B(R-1)lB

    Scale-up/down of Column

    What if we do not adjust any of the utilityflows while increasing/reducing the feed tothe column?

    Scale-down case

    F = B + D

    Fxf= BxB+ DxD

    Top of columnQD= VlD=D(1+R)lD

    Bottom of columnQB=VlB=B(R-1)lB

    V

    B

    V

    F

    L = B + V

    L = V - D

    R = L/D

    R = L/B

    L

    L

    reflux

    Boil-up

    Turton, 3rd edition, ch. 18

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    R.Turton and J.A. Shaeiwitz -

    Copyright 2008

    31

    47C and 0.07 bar

    Turton, 3rd edition

    Scale-up/down of Column

    What if we do not adjust any of the utility flowswhile increasing/reducing the feed to the column?

    Scale-down case

    F = B + D

    Fxf= BxB+ DxD

    Top of columnQD= VlD=D(1+R)lD

    Bottom of columnQB=VlB=B(R-1)lB

    Material balance control willadjust D+ Bto equal F

    Same cooling water flowand steam pressure causessame amount ofcondensation and reboil what happens to Rand R?

    Rand Rwill increase what happens to theseparation?

    V

    B

    V

    F

    L = B + V

    L = V - D

    R = L/D

    R = L/B

    L

    L

    Turton, 3rd edition, ch. 18

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    Scale-up/down of ColumnOperation

    For Scale-up must be aware of flooding limit normal design is between 75 85% of flooding, so

    scale-up window is small for vacuum operations changes in column pressure

    have a large effect on flooding

    For Scale-down

    weeping becomes an issue at 30-40% of flooding,

    depending on type of tray

    generally can avoid weeping problems by using higherthan necessary condenser and reboiler duties

    Turton, 3rd edition

    Number of Sequences of Ordinary Distillation Columns

    Benzene, Tb=80.1 CToluene, Tb 110.8 CBiphenyl, Tb=254.9 C

    Most volatile,taken asoverhead

    Toluene, Tb 110.8 CBiphenyl, Tb=254.9 C

    Least volatile

    Pure products produced (largedifferences in volatility)

    Other separation sequences arepossible!

    ethylenzenep-Xylenem-Xyleneo-Xylene

    p-Xylenem-Xylene

    o-Xylene

    Non-pure products produced(p- and m- xylene Tbs areseparated by only 0.8 C)

    Seider, Ch. 7

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    Synthesis of all possible ordinary distillation sequences for multicomponent feed that is to

    be separated into Pfinal products (nearly pure components or multicomponent mixtures)Lets order the feed components in decreasing volatilities and assume that this correlates with the normal

    boiling point (near ideal liquid solution).

    We come up with an equation for the number of different sequences of ordinarycolumns Nsto produce a number of products P:

    For example, for P=5 (A, B, C, D, E), the number of separation points is 5-1=4:A-B, B-C, C-D, D-E

    j= # of final products that must be developed from the distillate of 1st columnThus P-jis the # of final products that must be developed from the bottoms of the firstcolumn.

    Let Ni= the # of different sequences for I final products (thus, the number of sequences fora given separation point in the 1st column is NjNP-j. Note that in the first separator P-1different separation points are possible.

    Thus, the number of different sequences for Pproducts is:

    )!1(!

    )!1(21

    1

    PP

    PNNN

    P

    j

    jPjs

    Seider, Ch. 7

    )!1(!

    )!1(21

    1

    PP

    PNNN

    P

    j

    jPjs

    Number of different sequences for P products:

    Number ofProducts, P

    Number ofseparators in thesequence, (P-1)

    Number ofdifferentSequences, Ns

    2 1 1

    3 2 2

    4 3 5

    5 4 14

    6 5 42

    7 6 132

    8 7 429

    9 8 1430

    10 9 4862

    Seider, Ch. 7

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    Number ofProducts, P

    Number ofseparators inthe sequence,

    (P-1)

    Number ofdifferentSequences,

    Ns

    2 1 1

    3 2 2

    4 3 5

    5 4 14

    6 5 42

    7 6 132

    8 7 429

    9 8 1430

    10 9 4862 Direct sequence

    (commonly used in

    industry)

    pure" distillates (free of high-boiling compounds)

    If purity of D iscritical: addrerun(or

    finishing)column

    Sequence 2

    Sequence 3

    Sequence 4 Sequence 5: Indirect Sequence(least desirable due to difficulties in achieving

    purity for bottom products) Seider, Ch. 7

    Heuristics for Determining Favorable Sequences

    For P=3 or 4: designing and costing all sequences can be best to choose the mosteconomical one. However, in most case the direct sequence is often the choice.

    Otherwise, use following heuristics:

    1 Remove thermally unstable, corrosive, or chemically reactivecomponents early in the sequence

    2 Remove final products one by one as distillates (directsequence)

    3 Sequence separation points to remove, early in the

    sequence, those components of greatest molar % in the feed4 Sequence separation points in the order of decreasing

    relative volatility so that the most difficult splits are made inthe absence of the other components

    5 Sequence separation points to leave last those separationsthat give the highest-purity products

    6 Sequence separation points that favor near equimolaramounts of distillate and bottoms in each column

    When energy costs are high,this heuristics often leads tothe most economicalsequence.

    Note the marginal vapor Rate Method, Chapter 7 Seider

    Seider, Ch. 7

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    Example:

    Large variations in relative volatility andmolar % in process feed. Heuristics 4dominates over heuristic 3 and leads tothis sequence.

    H4: Sequence separation points in theorder of decreasing relative volatility sothat the most difficult splits are made inthe absence of the other components

    Seider, Ch. 7