tugas#3 - liquid-liquid extraction (tayangan#)

Upload: nabila-agnasia-desmara

Post on 02-Jun-2018

225 views

Category:

Documents


0 download

TRANSCRIPT

  • 8/10/2019 TUGAS#3 - Liquid-Liquid Extraction (Tayangan#)

    1/10

    TUGAS KELOMPOK:

    MEMBUAT TAYANGAN

    (PPT)

    Kalian diminta untuk membuat TAYANGAN yang berbasis dari contoh tayangan berikut ini.

    Untuk keperluan kalian, diharapkan kalian dapat menambahkan bahan-bahan lain yang

    terdapat pada referensi-referensi lainnya, termasuk yang dimiliki oleh kelompok-kelompok

    lainnya (PAGI atau pun SIANG).

  • 8/10/2019 TUGAS#3 - Liquid-Liquid Extraction (Tayangan#)

    2/10

    1

    11 Liquid-liquid Extraction

    A liquid mixture (e. g. A+B) is treated

    with a solvent S (extractant) in which

    one or more of the desired components is

    preferentially soluble.

    The separation of compounds is based on

    differences in solubilities

    [distribution of components between

    (partially) immiscible liquid phases].

    11.1 Introduction

    11.1.1 Extraction processes

    physical operation

    depends on the solubilities

    in two (partially) immiscible liquids

    chemical operation

    chemical reaction occurs,

    with higher selectivity

    Requirement for the solvent in physical

    extractions:

    (1) the solvent S and liquid-mixture are at

    least partially if not completely

    immiscible;

    (2) its solubilities for components aredifferent.

    A+B S

    A

    A single stage batch extraction:

    Subsequent separation process:

    distillation, crystallization, reextraction,

    solvent S extract E

    (S+A+B)

    yA, yB

    feed F

    (solute A +

    diluent B )

    raffinate R

    (B+A+S)xA, xB

    B

    A

    B

    A

    x

    x

    y

    y>

    Extraction is preferable in the following

    cases:

    (1) when the relative volatility is near unity,

    or when the azeotrope is formed;

    (2) when the concentration of less volatile

    components is low;

    (3) when heating must be avoided; and

    (4) when the components to be separated

    are quite different in nature.

    Factors to be considered for selecting

    solvent:

    (1) solubility

    (2) selectivity

    (3) subsequent separations

  • 8/10/2019 TUGAS#3 - Liquid-Liquid Extraction (Tayangan#)

    3/10

    2

    11.1.2 Contact between two phases

    differential contacting equipment

    e. g., packed columns, pulsed columns,

    spray towers.

    stagewise equipment

    e. g., mixer-settler units

    11.2 Equilibrium of Ternary Systems and

    Principle of Extraction

    xS = 0.3

    xA+xB +xS = 1

    x mass fraction S0.2 0.4 0.6 0.8

    xS

    xA

    xB

    M

    A

    0.8

    0.6

    0.4

    0.2

    B

    11.2.1 Triangular diagram

    1. Triangular diagram

    0.2

    0.4

    0.8

    0.6

    xA = 0.4

    xB = 0.3

    2. Lever rule

    Two liquid mixtures

    R kg (xA

    ,xB

    ,xS

    ) and

    E kg (yA

    ,yB

    ,yS

    ) are

    mixed to form a

    mixture

    Mkg (zA

    ,zB

    ,zS

    ). S

    A

    B xS

    RxA

    yA E

    yS

    M

    zS

    zA

    Lever rule:

    (1) M, E, and R are along the same line;

    (2) the mass ratio of mixtures equals to the

    length ratio of

    line segments.

    ME

    MR

    R

    E

    =

    ,RE

    MR

    M

    E=

    RE

    ME

    M

    R=

    S

    A

    B xS

    RxA

    yA E

    yS

    M

    zS

    zA

    When the solvent S is mixed with the

    binary mixture F (A+B) , point M must be

    on line SF, and its position is determined by

    the lever rule.

    S

    A

    B

    MS

    MF

    F

    S=

    (11-26)

    On the line SF, the mass

    ratio of A and B is the same.

    FM

    11.2.2 Equilibrium of partially misciblesystems

    Liquid mixture: solute A + solvent B

    New solvent S

    Types of ternary mixture:

    (1) S may be completely immiscible with

    the original solvent B.

    (2) S may be partially miscible with B.

    (3) S and B, S and A form two partially

    miscible liquids.

    I

    II

  • 8/10/2019 TUGAS#3 - Liquid-Liquid Extraction (Tayangan#)

    4/10

    3

    1. Solubility curve, tie line, and plait point

    plait point P

    conjugate phasesE and R areconnected by thetie line.

    P

    A

    SB

    solubility curve

    homogeneous

    phase

    tie line

    R0 E0

    R1E1

    M1

    two-phase region

    Solubility curve:

    Extract on the RHS of pint P

    ys = (yA ) (11-9)

    Raffinate on the LHS of pint P

    xs = (xA ) (11-10)

    P

    A

    SB R0 E0

    2. Distribution coefficient and

    distribution curve

    Distribution curve

    yA =f (xA ) (11-8)

    Distribution coefficient

    A

    A

    x

    y=

    (11-6)

    kA =mass fraction of A in extract .

    mass fraction of A in raffinate

    yA

    xA0

    y = x

    P

    11.2.3 Phase equilibrium and extraction

    operation

    1. Single-stage extraction process

    solventrecovery

    purified extract

    E,yA

    purified raffinate

    R,xA

    feed F

    solvent S

    SB

    A

    ERR

    E

    F

    extract E

    raffinate R

    M

    2. Selectivity ratio of solvent

    Binary systems:

    B

    A

    BA

    BA

    k

    k

    xx

    yy=

    /

    /

    (11-11)

    oo

    oo

    BA

    BA

    xx

    yy

    /

    /=

    or (11-12)

    o

    o

    o

    A

    AA

    x

    xy

    )1(1 (11-13)

    , = 1, separation by

    extraction is impossible.

    Note:

    distribution coefficientk

    phase equilibrium

    selectivity ratio

    separability by extraction

    o

    o

    o

    A

    AA

    x

    xy

    )1(1

    (11-13)

    SB

    A

    R

    E

    FM

    oo

    AA xy=When

    E

    R

  • 8/10/2019 TUGAS#3 - Liquid-Liquid Extraction (Tayangan#)

    5/10

    4

    3. Effect of miscibility of original solvent Band extractant S

    small miscibility

    larger two-phase region

    , better result of separation

    lower temperature

    miscibility

    , surface tension .

    11.3 Calculation for an Extraction Process

    11.3.1 Mathematical description

    1. Material balance

    Stage m:

    Rm1,xm1, A,xm1, S Rm ,xm, A,xm, S

    mEm ,ym, A,ym, S Em+1,ym+1, A,ym+1, S

    Total material balance:

    Rm1 +Em+1 =Rm +Em

    Material balance for solute A:

    Rm1xm1, A +Em+1ym+1, A =Rmxm, A +Emym, A

    Material balance for solvent S:

    Rm1xm1, S +Em+1ym+1, S =Rmxm, S +Emym, S

    Rm1,xm1, A,xm1, S Rm ,xm, A,xm, S

    mEm ,ym, A,ym, S Em+1,ym+1, A,ym+1, S

    2. Equilibrium stage and stage efficiency

    Equilibrium stage:

    The compositions of the two streams

    leaving the stage are in equilibrium,

    no mater what composition they have

    when they enter the stage.Rm1,xm1, A,xm1, S Rm ,xm, A,xm, S

    mEm ,ym, A,ym, S Em+1,ym+1, A,ym+1, S

    A problem of extraction may beconsidered from two aspects:

    equilibrium stage

    it is independent of equipment and

    may be calculated first.

    stage efficiency

    it depends on the equipment, determined

    experimentally.

    actual number of stages

    = equilibrium stage/efficiency

    11.3.2 Single-stage extraction

    For design:

    given:F,xFA

    specify:xA

    select:zA,zS

    calculate: S,E,yA,yS,

    R,xS.

    For operation:

    given:F,xFA

    S,zA,zS

    calculate:E,yA,yS,

    R,xA,xS.

    F, xFA

    S, zA, zS

    R, xA, xS

    E, yA, yS

  • 8/10/2019 TUGAS#3 - Liquid-Liquid Extraction (Tayangan#)

    6/10

    5

    1. Analytical method

    Six unknowns are solved from 6

    equations.

    Phase equilibrium relationship:

    yA =f (xA ) (11-8)

    ys = (yA ) (11-9)

    xs = (xA ) (11-10)

    Total material balance:

    F + S =R +E =M (11-20)

    Material balance for solute A:

    xFA+SzA =RxA+EyA =MxMA (11-21)

    Material balance for solvent S:

    SzS =RxS+EyS (11-22)

    2. Graphical method

    (1) Draw the solubility

    curve.

    (2) Locate points F and

    S, and the mixture

    M is on the line FS.(3) Locate point R byxA,

    find the tie line RE by interpolation,

    M is the intersection of lines RE and FS.

    R

    A

    SB

    E

    M

    F

    xA

    ?

    A

    P E3R3

    R2R1

    SB

    E2

    E1

    Find the tie line RE:

    (a) By estimation;

    (b) By auxiliary

    curve.

    E

    R

    ?

    (4) Determine the flowrates of streamsby material balance and lever rule

    Total material balance:

    M=F + S

    R

    A

    SB

    E

    M

    F

    xA

    MS

    MF

    F

    S=

    R =ME

    RE

    MRME

    =

    (5) Find the composition in the extractyAandyS , and the concentration of solvent

    in the raffinatexS.

    R =F E

    are the amount of

    purified extract and

    raffinate, respectively. xS

    E

    R

    yS

    yA

    =

    ER

    FRFE

    R

    A

    SB

    E

    M

    F

    xA

  • 8/10/2019 TUGAS#3 - Liquid-Liquid Extraction (Tayangan#)

    7/10

    6

    Or: the flowrates of streams may be

    obtained by material balance only,

    in whichxFA is given,xA is specified,zA is

    selected, andxMA andyA are found from the

    phase diagram.

    AMA

    MAFA

    zx

    xxFS

    =

    AA

    AMA

    xy

    xxME

    =

    3. Range of separation in a single-stage

    extraction and the limit in the amount of

    extractant

    Point c:

    the maximum amount

    of solvent Smax .

    Correspondingly,

    in raffinate:xA, min

    in purified raffinate:xA,min

    A

    SB

    E

    M

    FxF,A

    R co

    min,Axo

    min,Ax

    Point d:

    the minimum amount of solvent Smin .

    The amount of

    solvent used for

    operation:

    Smin < S < Smax

    In general,

    S = (1.1 2.0)Smin xA,min

    A

    SB

    E

    M

    FxF,A

    R co

    min,Ax

    d

    Draw a line tangent

    to the solubility curve

    through point S, we

    obtain the maximum

    concentration in the

    purified extract,o

    max,Ay

    o

    max,Ay

    xA,min

    A

    SB

    E

    M

    FxF,A

    R co

    min,Ax

    d

    11.3.3 Multi-stage crosscurrent extraction

    for single-stage extraction,

    but the amount of liquid

    mixture in each stage is

    usually different.

    Features:

    the concentration of solute

    is low in the raffinate, and

    the amount of solvent is

    large.

    1

    2

    3

    S E1

    S E3

    S E2

    F

    R1

    R3

    R2

    The calculation is the repeat of that 11.3.4 Multistage countercurrent extraction

    Higher extract rate may be obtained with

    less extractant.

    Calculation:

    amount of solvent, number of equilibrium

    stages, amount and concentration of

    streams leaving each stage.

    Method of stage-to-stage:

    analytical or graphical

  • 8/10/2019 TUGAS#3 - Liquid-Liquid Extraction (Tayangan#)

    8/10

    7

    11.3.5 Calculation for extraction with

    completely immiscible solvents

    1. Representation of composition and phase

    equilibrium

    X mass ratio in raffinate

    (kg solute/kg diluent )

    Y mass ratio in extract

    (kg solute/kg solvent )

    Equilibrium relationship:

    Y=KX (11-35)

    K distribution coefficient, generally

    dependent upon concentration.

    2. Single-stage extraction

    B amount of original solvent

    S amount of pure solvent

    Z

    mass ratio of A in extractant

    Material balance for solute A:

    S(YZ) =B(XF X) (11-36)

    feed B, XF

    solvent S, Z

    extract S, Y

    raffinate B, X

    Equilibrium relationship:

    Y=KX (11-35)

    Material balance for solute A:

    S(YZ) =B(XF X) (11-36)

    For givenB,XF andZ, specify one variable

    among S, YandX, other two may be

    calculated.

    3. Multistage crosscurrent extraction and

    countercurrent extraction

    11.3.6 Extraction with reflux

    High purity may be achieved.

    11.3.7 Differential contacting

    countercurrent extraction

    The diameter of column depends on the

    flowrates and velocities of two phases.

    The height of column may be obtained by

    calculating the number of transfer unit or

    HETS.

    Exercises: 11 1, 3, 5

  • 8/10/2019 TUGAS#3 - Liquid-Liquid Extraction (Tayangan#)

    9/10

    8

    11.4 Extraction Equipment

    Requirement:

    bringing the feed mixture and the solvent

    into intimate contact

    separation of the resulting two phases

    11.4.1 Types of extraction equipment

    stagewise contactors

    differential contactors

    Both may be with or without the addition

    of external energy.

    Stagewise contactors:

    mixer-settler unit

    sieve-plate column

    Differential contactors:

    1. spray tower

    2. packed column

    3. pulsed packed column

    pulsed sieve column

    4. vibrational sieve plate column

    5. rotary disc column

    6. centrifugal extractor

    11.4.2 Flooding in extraction equipment

    and limit of velocity

    The performance of equipment is mainly

    determined by:

    allowable flowrates of two phases (D)

    rate of mass transfer (H)

    The superficial velocities of two phases at

    which the flooding occurs are the limit for

    the velocities.

    11.4.3 Rate of mass transfer in extraction

    equipment

    Factors affecting mass transfer:

    (1) drop size and size distribution of

    dispersed phase

    (2) circulation inside drops and interfacial

    disturbance

    (3) axial mixing in the equipment

    11.4.4 Selection of extraction equipment

    Following factors are to be considered:

    the number of stages required

    production capacity

    properties of the materials

    residence time

  • 8/10/2019 TUGAS#3 - Liquid-Liquid Extraction (Tayangan#)

    10/10

    9

    11.5 Supercritical Fluid Extraction and

    Liquid Membrane Extraction

    11.5.1 Supercritical fluid extraction

    1. Principle

    It is an extraction process in which a

    supercritical fluid is used as the solvent.

    Supercritical fluid:

    viscosity that of gas

    density and solubility

    those of liquid

    diffusivity >> that in liquid

    S

    criticalpoint

    t

    pSFL

    G

    2. A process of supercritical extraction

    CO2 is compressed as a supercritical

    fluid, and used as an extractant.

    reducing valveextractfeed

    extraction

    productraffinate SF

    compressor

    11.5.2 Liquid membrane extraction

    (

    separation )

    The extraction and reverse extraction

    are carried out simultaneously.

    (a) make an emulsion by dispersingaqueous drops (in m) into an organic

    phase (W/O);

    (b) disperse the

    emulsion into the

    aqueous phase

    (in 0.11 mm)

    (W/O/W).

    liquid

    membrane

    external

    phase

    internal

    phase

    A

    B

    Or: with O/W/O system.

    Extraction with supported membrane:

    The liquid

    membrane phase

    is retained in a

    porous medium.liquid

    membrane

    lyophilic

    porous

    membrane

    recovery

    phase

    original

    liquid

    A