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    Tutorial Topic 7

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    Tutorial Topic 7

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    Tutorial Topic 7

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    of 4

    UNIT OPERATION A – DISTILLATION TUTORIALS 1

    Tutorial 4 – Distillation of Difficult Mixtures: Azeotropes


    1. On distillation of difficult mixtures, we considered the separation (using 2 columns
    operating at pressures P1 and P2) of a binary mixture, 100 kmol/hr, 50% B. The mixture
    exhibited boiling azeotrpic behaviour as follows:

    Pressure Azeotropic Composition


    P1 80% A
    P2 90% A

    A flowsheet and a preliminary material balance were developed.


    a) How would the flow sheet be modified if these were maximum boiling (rather than
    minimum boiling) azeotropic compositions?
    b) For minimum boiling azeotropic behaviour, develop a 2-column flowsheet for the
    complete separation of a mixture of composition 95% A, 5% B.
    c) For minimum boiling azeotropic behaviour, and a complete separation of
    composition 85% A, 15% B, show that there are two possible 2-column separation
    schemes. Complete preliminary material balances assuming perfect splits, for each
    of these alternatives. Can you suggest the more promising scheme for further
    investigation?

    2. On distillation of difficult mixtures, we considered the separation (using 2 columns and a


    decanter) of a mixture containing 25 mole% n-butanol and 75 mole% water. Develop
    potential separation schemes based on the same general principles, for mixtures of
    composition:
    a) 40 mole% n-butanol, 60 mole% water
    b) 70 mole% n-butanol, 30 mole% water
    (As in the original problem take the azeotropic composition as 35 mole% n-butanol and
    the ‘left hand’ and ‘right hand’ limits of the L/L region to be at 5 mole% and 50 mole% n-
    butanol, respectively)

    ©Heriot-Watt University B40EA April 2016 v1


    UNIT OPERATION A – DISTILLATION TUTORIALS 2

    3. The following data show the vapour and liquid compositions obtained when three
    mixtures (A, B, and C) are flashed at 1.2 bar.

    Composition (mole fractions)


    Vapour Liquid
    A n-heptane 0.5419 0.4581
    Toluene 0.4581 0.5419
    B n-heptane 0.4486 0.0514
    Toluene 0.3699 0.1301
    Phenol 0.1815 0.8185
    C Toluene 0.7678 0.2322
    Phenol 0.2322 0.7678

    By evaluating appropriate relative volatilities show that:

    i) Toluene and n-heptane would be difficult to separate by conventional distillation.


    ii) Phenol could be a suitable solvent for separating toluene and n-heptane by
    extractive distillation.
    iii) Provide and explain a flowsheet for the separation of toluene and n-heptane
    using phenol as extractive distillation solvent, showing in particular the relative
    positions of the two feeds within the extractive column.

    4. The following data show the vapour and liquid compositions obtained when two mixtures
    (A, B) of acetone and chloroform are flashed at 1 bar.

    Composition (mole fractions)


    Mixture Vapour Liquid
    A Acetone 0.01 0.0079 0.0121
    Chloroform 0.99 0.9921 0.9879
    B Acetone 0.99 0.9908 0.9892
    Chloroform 0.01 0.0092 0.0108

    By comparing relative volatilities in the two cases demonstrate that this system will show
    azeotropic behaviour.

    Would you expect this to be a minimum boiling azeotrope or a maximum boiling


    azeotrope? (the normal boiling points of acetone and chloroform are 55.7 oC and 60.8°C.
    (this is not essential information but will help you a sketch a reasonably realistic Txy
    diagrams for this system).

    ©Heriot-Watt University B40EA April 2016 v1


    UNIT OPERATION A – DISTILLATION TUTORIALS 3

    Answers to selected questions


    Q1 Maximum boiling point Azeotrope, and the scheme to treat this looks like

    c)

    d)
    Basis (1) (2) (3) (4) (5)
    100 kmol
    A 85 108 85 108 -
    B 15 27 - 12 15
    Total 100 135 85 120 15

    Basis (1) (2) (3) (4) (5)


    100 kmol
    A 85 153 - 68 85
    B 15 17 15 17 -
    Total 100 170 15 85 85

    Q2. a)

    ©Heriot-Watt University B40EA April 2016 v1


    UNIT OPERATION A – DISTILLATION TUTORIALS 4

    b)

    Q3 i) Relative volatilities are close to 1 – alpha (n-heptne/toluene)=1.4, ii) Relative volatility n-


    c7/toluene 3.07, iii)

    Q4

    i) Low acetone concentration, alpha (rel volatility)=0.65, high acetone concentration alpha
    =1 (ie an azeotrope).
    ii) Mixture has a maximum boiling point azeotrope.

    ©Heriot-Watt University B40EA April 2016 v1

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