Chapter 9

Batch Distillation

 Continuous distillation produces

large amounts of material of
constant composition
If small amounts of material or
varying product composition are
needed, one has to use batch
distillation
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Simple Batch Distillation

D, xD

W, xW

QR

still pot
3

Batch Distillation Uses

Relatively small amounts of product.
Non-continuous operation (batch).
Different distillations are to be done
using the same equipment.
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Batch Distillation
Unit may be a single pot or multi-staged.
There is no continuous feed the pot is
charged with liquid and then drained at the
end of the run.
Distillate (usually the desired product) may
be withdrawn continuously or collected in
an accumulator.
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Batch Distillation
One is more interested in the amounts of
bottoms and distillate collected rather than
the rates.
The amount and compositions in the pot
(bottoms) change as the more volatile
component(s) decrease(s) with time and the
less volatile component(s) increase(s) with
time.
Because the bottoms amount and
concentrations change with time, the
distillate amount, D, and concentration, xD, in
general, change with time.
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Batch Distillation Mass Balances

over Total Operation Time

Multistage Batch Distillation

Figure 9-2. Multistage batch distillation; (A) schematic, (B) photograph of

packaged batch distillation/solvent recovery system of approximately 400gallon capacity.

Multistage Batch vs. Continuous

Since there is no feed, there is only one
operating line.
The batch system can be operated with a
constant L/D, which means that xD will
change with time, or it can be operated
with a constant xD, which means that the
L/D must be continuously changed.
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Batch Trade-Off
For a constant L/D, the distillate concentration fed to the
accumulator decreases with time.
The composition of the desired component in the
distillate is at a maximum at the beginning of the batch
run and decreases with time as it is distilled from the
bottoms pot.
The concentration of the more volatile component in the
accumulator also decreases with time the trade off is a
lower concentration with more distillate accumulated.

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Multistage Batch Distillation

Operating Line
For a multistage batch column, if one can assume
CMO, then the operating line for the column is
essentially the same as that previously used for
continuous distillation:

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McCabe-Thiele -- Constant xD

Figure 9-7. McCabe-Thiele diagram for multistage batch distillation

with constant xD and variable reflux ratio

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McCabe-Thiele -- Constant L/D

Figure 9-5. McCabe-Thiele diagram for multistage batch distillation

with constant L/D, Example 9-2

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Constant L/D vs. xD

Operating at constant L/D is easy
one sets it and runs while the xD
continuously changes.
Operating at constant xD is more
difficult since one needs to
continuously monitor the distillate
concentrations and control the L/D.
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Multistage Batch Distillation

We have only one operating line since there is no feed.
We can plot this operating line on a McCabe-Thiele plot
along with our equilibrium curve.
We can step down the operating line from xD to xW to
determine the number of stages.
Note that the bottoms concentration, x W, keeps
changing with time as the liquid is boiled off.
Also note that xD changes with time for a constant
reflux ratio, L/V or L/D.
How do we determine the composition at the bottoms
in the pot?
We need to relate xD and xW with respect to time
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Differential Change

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Integrating

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Rayleigh Equation

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1. Plot or fit y-x equilibrium curve.

2. At a series of x values, find y-x.
3. Plot 1/(y-x) vs. x or fit it to an equation.
4. Graphically or numerically integrate from xF to xW,final

area

5. Find the final charge in the still

6. Compute average distillate composition

Solving Eqs. (9-1) and

(9-2)

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Figure 9-3. Graphical integration for simple batch

distillation, Example 9-1
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The Rayleigh equation can also be integrated

numerically. One convenient method for doing this
is to use Simpsons rule

Eq. 9-12

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If the equilibrium expression is given as a constant

relative volatility, , the Rayleigh equation can be
integrated analytically.

Final charge is given by:

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Rayleigh Equation Notes

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xD = f(xW) Relationship

Figure 9-6. Graphical integration, Example 9-2

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Algorithm
For a given L/D and number of column
stages, assume xDs, perform a McCabeThiele Analysis at each xD stepping down to
determine the corresponding x Ws.
Plot 1/(xD xW) vs. xW.
Graphically integrate or do a polynomial
curve fit between xW = xF and xW = xW,final
and integrate.
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Total Reflux
Note that a multistage batch still, operated
such that all of the distillate is returned to
the top of the column, is essentially the
same as a multi-stage distillation column
operated under total reflux.
For a binary separation, given a column
containing an N number of equilibrium
stages, one can measure xD at the top of
the column and xB at the bottom of the
column and perform a McCabe-Thiele
analysis to determine the theoretical N min.
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Column Overall Efficiency

For a column containing an Nactual number of
stages, the overall efficiency can be determined
from
Eo = Nequil /Nactual
where Nequil is the theoretical N obtained from
the McCabeThiele analysis.
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Constant-level batch distillation

Solvent switching
Boil off most of the original solvent and add a new
solvent continuously so that the second batch
distillation is such the amount of the second
solvent in the still pot is kept constant.
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Consider a mixture with a constant relative volatility

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Batch Steam Distillation

Fig. 9-4. Batch steam distillation

This technique is used for the systems
that are immiscible with water.

steam is sparged directly into the still pot

1.No need to heat above 100 degrees Celcius

2.No need for heat transfer equipment
3.Steam results in good mixing of the material in the pot

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Treat

wastes

that

contain

valuable

VOCs

(glycerine, lube oils, fatty acids, halogenated

hydrocarbons)
Only one stage is needed
Mass balance on a water free basis

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Total moles of water required

Above Equation can be integrated numerically in steps.

The total moles of water required is nw plus the moles of
water condensed to heat the feed and still pot, and to
vaporize the volatile organics.

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Multistage Batch Distillation

With a single stage one often cannot get the

desired distillate and residue compositions
Place a distillation column above the still
The Rayleigh equation is valid but one has to find a
relationship between xD and xW , which is obtained
from stage-by-stage calculation.
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Neglect accumulation everywhere

except the still pot

CMO (Constant Molal Overflow)

No need for energy balance & L and V will be constant

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Constant Reflux Ratio Operation

Use constant reflux ratio and allow xD to vary

Use McCabe & Thiele diagram for a series of xD
values to find their corresponding xW values.

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McCabe & Thiele diagram for multistage batch

distillation with constant reflux ratio
1.0
xD,1

xD,2

xW,2

xW,1

1.0

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Variable Reflux Ratio Operation

Vary the reflux ratio and keep xD constant

The slope of the operating line will now vary
Use McCabe & Thiele diagram to find xW values.

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McCabe & Thiele diagram for multistage batch

distillation with variable reflux ratio
1.0
xD

xW,2

xW,1

1.0

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Need to find the initial slope of the operating line so

that xW=xF
Need to increase the operating line slope until xW=xW,final
Use mass balance around the entire system for the
entire operation time to get Wfinal.

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Operating time
Usual batch duration including startup
shutdown is around eight-hour shift

and

Dumping the bottoms, cleanup, loading next batch

and heating until reflux starts to appear
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From Rayleigh equation

Total distillate amount in kmoles

uflood
Distillate flow rate
in kmoles/hr

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Energy requirement for the total

condenser

Energy balance around the entire system

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