Introduction to Distillation[1]

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    Introduction to Distillation

    1Binous - Introd. to Distillation

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    Exploits differences in boiling point, or volatility

    Requires the input of energy

    Handles a wide range of feed flow rates

    Separates a wide range of feed concentrations

    Produce high product purity

    2Binous - Introd. to Distillation

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    vapor becomes richer in the more volatile components

    3Binous - Introd. to Distillation

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    thermodynamic vapor-liquid equilibrium considerations

    4Binous - Introd. to Distillation

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    K-values

    Wilson model for iEOS for fugacity coefficients

    Relative volatility

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    6Binous - Introd. to Distillation

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    a single equilibrium stage can only achieve

    a limited amount of separation 7Binous - Introd. to Distillation

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    CMO assumption

    When CMO is true?

    (1) sensible heat effects are small

    (2) molar latent heats of vaporization are equal

    (3) heat of mixing is negligible

    (4) there are no heat losses or gains.

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    Cascade of Separation Stages

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    Assume CMO:

    Mass balance:

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    We need vapor and liquid to

    feed the bottom and top of

    the cascade.

    The feed to the process is

    introduced at an intermediate

    stage.

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    12Binous - Introd. to Distillation

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    Liquid is prevented from weeping through the holes

    in the plate by the upflowing vapor. In this way the

    vapor and liquid are contacted.

    The liquid from the first tray flows over a weir and

    down a downcomer, to the next stage and so on.

    13Binous - Introd. to Distillation

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    Sieve trays

    Valve trays

    Bubble-cap trays

    In practice, the column will need more trays than the

    number of equilibrium stages as mass transfer limitations

    prevent equilibrium being achieved on a tray.

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    packed columns:

    Here the column is filled with a solid material which has a high

    voidage (random packing material such as Pall rings, Ceramic

    Intalox saddles... or structured packing such as Glitsch grid) .

    Liquid trickles across the surfaces of the packing and vapor

    flows upward through the voids in the packing, contacting the

    liquid on its way up the column.

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    design of a distillation column involves:

    1. Set the product specifications.

    2. Set the operating pressure.

    3. Determine the number of theoretical stages required and the energy

    requirements.

    4. Determine the actual number of trays or height of packing needed and the

    column diameter.

    5. Design the column internals, which involves determining the specificdimensions of the trays, packing, liquid and vapor distribution systems, etc.

    6. Carry out the mechanical design to determine wall thicknesses, internal

    fittings, etc.

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    Binary Distillation

    17Binous - Introd. to Distillation

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    Reflux ratio

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    19Binous - Introd. to Distillation

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    20Binous - Introd. to Distillation

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    21Binous - Introd. to Distillation

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    The construction is started by plotting the operating lines for the

    rectifying and stripping sections. The q-line intersects the

    operating lines at their intersection.

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    The intersection of the operating lines is the correct feed

    stage, i.e. the feed stage necessary to minimize the overallnumber of theoretical stages.

    The construction steps off between the operating lines and

    the equilibrium lines.

    The construction can be started either from the overhead

    composition working down or from the bottom composition

    working up.

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    Choice of Operating Parameters

    The operating parameters to be selected by the designer include:

    1. operating pressure

    2. reflux ratio

    3. feed condition

    4. feed stage location

    5. type of condenser

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    operating pressure

    Pressure has an important effect on all aspects of thedistillation column design.

    25Binous - Introd. to Distillation

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    As pressure increases, the relative volatility decreases,

    making separation more difficult.

    Minimum reflux ratio also increases with increasing

    pressure, as does the minimum number of stages.

    All of these trends point to operating the distillation

    columns at a pressure as low as possible.

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    Latent heat decreases with increasing pressure; this would have

    the effect of decreasing the reboiler duty as pressure increases.

    Finally, both the condenser and the reboiler temperature

    increase as pressure increases.

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    28Binous - Introd. to Distillation

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    Reflux Ratio

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    30Binous - Introd. to Distillation

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    Feed Condition

    The feed condition affects vapor and liquid flow rates in the

    column, and in turn:

    1. reflux ratio, heating and cooling duties

    2. column diameter

    3. most appropriate location of the feed stage

    Heating or cooling the feed can reduce energy cost

    by reduction of utility consumption.

    31Binous - Introd. to Distillation

    C li h f d

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    Cooling the feed:

    1. decreases the number of stages in the rectifying section but

    increases the number of stages in the stripping section.

    2. requires more heat in the reboiler but decreases the cooling

    duty of the condenser.

    Heating the feed:

    1. increases the number of stages in the rectifying section but

    decreases the number of stages in the stripping section.

    2. decreases the heat requirement of the reboiler but increases

    the cooling duty of the condenser.

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    Feed Stage Location

    When choosing the feed stage location, our objective is to find a

    stage in the column for which the composition matches as closely

    as possible that of the feed.

    Mismatches between the composition on the feed stage and that

    of the feed create inefficiencies in the distillation. This leads to an

    increase in the number of stages required for the same

    separation, or more reflux, which means increased energy

    requirements, or a combination of both.

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    Distillation Equipment

    Sieve tray, is the most common arrangement used. It is

    cheap, simple, and well understood in terms of its

    performance.

    Valve arrangement offer more flexibility to cope with wider

    range of liquid and vapor flow rates.

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    35Binous - Introd. to Distillation

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    The difference between the performance of an ideal stage and

    a real tray results from the fact that equilibrium is not

    achieved on a real tray because of mass transfer limitations.

    We therefore define an efficiency to convert from the

    theoretical stages to real trays.

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    Three different efficiencies can be defined:

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    38Binous - Introd. to Distillation

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    1. flooding: liquid cannot flow down the column

    2. entrainment: liquid drops are carried up the column by the

    vapor flow

    3. downcomer backup: liquid backs up in the downcomers

    4. weeping: vapor flow is too low to maintain liquid on the tray

    5. coning: poor vapor-liquid contact occurs due to the vapor

    forming jets

    39Binous - Introd. to Distillation

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    Packing

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    Column Diameter Calculation

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    42Binous - Introd. to Distillation

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    Column Sequences

    If a feed mixture needs to be separated into more than two

    products, then more than one distillation column will be required.

    43Binous - Introd. to Distillation

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