Batch Distillation
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Batch Distillation
CONTENTS
SECTION
INTRODUCTION/PURPOSE
SCOPE
FIELD OF APPLICATION
DEFINITIONS
4.1
4.2
4.3
4.4
4.5
General
Choice of batch/continuous operation
Boiling point curve and cut policy
Method of design
Scope of calculations required for design
3
4
5
5
6
6.1
6.2
6.3
6.4
General
Approximate methods
Rigorous design - use of a computer model
Other factors influencing the design
7
7
7
8
6.4.1
6.4.2
6.4.3
6.4.4
6.4.5
6.4.6
6.4.7
8
8
8
9
9
9
10
Occupation
Choice of Batch Rectification or Stripping
Batch size
Initial estimate of cut policy
Liquid Holdup
Total reflux operation and heating-up time
Column operating pressure
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6.5
6.6
10
11
11
7.1
7.2
7.3
Kettle reboilers
Column Internals
Condensers and reflux split boxes
11
11
11
12
12
10
BIBLIOGRAPHY
15
APPENDICES
16
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FIGURES
1
13
18
19
20
21
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INTRODUCTION/PURPOSE
SCOPE
This Engineering Guide sets out the factors which can influence the design of a
batch still facility. However, no single document can fully reflect the known
diversity of experience and technique available.
It follows that this guide can provide, at best, a checklist by which an optimum
design can be evolved whilst avoiding some of the more common pitfalls.
For the reader who wishes only to be reminded of the traditional McCabe - Thiele
based methods applied to a batch still problem, a typical example is set out in
Appendix A.
FIELD OF APPLICATION
DEFINITIONS
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4.1
General
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4.2
(b)
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(c)
where the adjacent processing stages are batch operations and where
batch identity may be important,
(d)
(e)
where the contributory cost of energy is low (use of utilities such as hot oil
may favor continuous processing when interchange is possible).
Measurement and consideration of the boiling point curve of the feedstock can
give a useful indication of the distillation requirements to achieve separation,
particularly when the detailed vapor-liquid equilibria are known. For example, the
true boiling point test (see Bibliography, ref 4) in which the material is batch
distilled in a column with high plateage (up to 100) and high reflux (up to 100:1)
typically results in a plot of the overhead vapor temperature against percentage
distilled of the form indicated in Figure 2. The art of batch distillation lies in
deciding at what points in the distillation process the intermediate cuts should be
taken containing mixtures of components and how to subsequently reprocess
these mixtures to improve the overall recovery. For example, a cut fraction could
either be worked up separately or recharged with the next batch of feedstock. In
many multicomponent systems the shape of the curve can be enormously more
complex than that of Figure 2 and the range of cut point options is
correspondingly greater; in such cases the practice is to accumulate "fores" and
"tails" fractions about the major (or most valuable) component for subsequent
reworking.
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4.4
Method of design
Where reliable correlations for the vapor-liquid equilibria are available, the use of
an appropriate computer simulation is virtually mandatory in all but the simplest
of cases (ie binary systems of high relative volatility) particularly where tight
design and operation are critical. When insufficient time or material is available
for an empirical approach, the use of a computer program for solving the
unsteady state distillation problem permits a quantitative optimization
of still design and operation. Indeed it is possible, given the vapor-liquid
equilibria, for the engineer to evolve a sensible operational policy with regard to
splitting (and possibly reworking) a feedstock in order to guide laboratory scale
experimentation at a very early stage in product development. An increasingly
frequent problem involves separation of an aqueous feedstock
containing both organics and salts (substantial salting out effects may be
localized in the reboiler); the current range of software cannot handle this case.
4.5
All distillation column designs require solutions to the phase equilibria, the heatand-mass balances through the column (usually on a theoretical tray basis) and
then the hydraulics and mass-transfer characteristics of the tower internals.
Whilst these solutions specify the performance of a continuous still, batch
distillation calculations should additionally solve the unsteady state (compositions
throughout the unit changing as material is withdrawn) which in
turn depends on the holdup of liquid and throughput characteristics of the kettle,
column and auxiliaries. In many instances the liquid holdup pattern will determine
the achievable splits as well as having implications for control of the column. For
example, holdup and drainings from the column will determine the level of volatile
impurity for a product retained in the kettle; holdup in the reflux drum will
dominate distillate purity when a volatile product is a minor component in
the feedstock. Furthermore, a multicomponent distillation may be effected with
changes of reflux ratio, reboiler duty or operating pressure as specific cuts are
taken. The compositions of intermediate cuts may well also be parameters which
have to be optimized with regard to rework operation. Finally, the optimum
purities of products should be assessed in the context of the overall flowsheet
requirements since adjacent processing stages may be influenced by trace
contaminants or solvents.
It follows therefore that, in the case of a multicomponent feedstock, the number
of variables open to optimization can be extremely large. Design is therefore
inevitably an iterative process.
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The simplest case of binary batch distillation involves a reboiler and condenser
with no column fractionation. This was first considered by Rayleigh whose
solution to the equilibrium and mass balance equations assuming constant
relative volatility is as follows:
This type of distillation is generally restricted to duties where the relative volatility
is say above 5, and where neither high recoveries nor high purities are crucial. It
may also be used with an existing facility where the layout precludes the
installation of a column. In such a case it may be necessary to undertake
repeated Rayleigh-type distillations to improve recovery and purity in
products, but this carries penalties in terms of both energy and occupation.
6.1
General
Approximate methods
For the simulation of any multicomponent batch distillation, several computerbased methods are available which obviate many of the assumptions of manual
calculations. These are invariably theoretical plate methods which require an
adequate knowledge of the vapor-liquid equilibria of the system.
Some commercially available computer programs simulate batch distillation of a
multicomponent, non-ideal system and has the following facilities:
(a)
(b)
(c)
(d)
allows the user to change the reflux ratio, reboiler load, or column
pressure through the distillation and to add/remove a continuous feed from
the still.
(e)
interfaces to a reaction routine (to allow for reactions in the reboiler) and
also to FRI column internals routines are possible (but not generally
available).
Some programs requires the user to specify the number of theoretical plates,
reflux ratio and boilup rate, some initial estimate of these design variables is
required. Treating the system as pseudobinary (ie topping-off each component in
turn), variations on the Fenske equation for minimum number of stages and the
Underwood equation for minimum reflux ratio can be used to get suitable starting
values (see GBHE-PEG-MAS-603).
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The following typical plateage and reflux requirements have been cited in the
open literature for overhead product purities between 300 and 8000 ppm (see
Bibliography ref 5).
6.4.1 Occupation
The proportion of time for which the plant can be used for distillation activities
(i.e. charging, operation and discharging) has to be assessed at the start of the
design. For a dedicated still with a steady feedstock composition and with no
serious cross-contamination problems an assumed occupation of up to 70% can
be used for initial sizing purposes. Where a specific production rate is required
from a feedstock of variable quality the occupation should reflect the worse case
(particularly when reworked fractions are involved). For a multi-purpose still
where cleanouts between batches and reworking of various cuts are undertaken
it would be unwise to assume that the still can be used at more than 50%
occupation.
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(b)
(c)
(d)
(e)
The designer may have to evaluate several batch sizes in some detail before
coming to an suitable arrangement. Batch sizes are usually between 2 and 50
m3.
6.4.4 Initial estimate of cut policy
Where a simple solvent recovery is required, the cut policy to be adopted may be
almost self evident from the feedstock and product specifications. However, with
a greater number of products to be resolved the cut policy can become more
complex; particularly when substantial intermediate cuts are involved.
There are three possible ways of dealing with intermediate cuts, these being:
(a)
Distil the cuts separately; this may lead to extended overall cycle times or
large storage requirements. A typical practice would be to retain the heels
from several distillations before finally discharging the accumulated heel
for disposal.
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(b)
(c)
Recharge the cut back to the reboiler; this has been done in one instance
where the compositions matched up.
When using a simulation model for a new multicomponent problem with cut
policy and column design to be optimized, the user is advised to start off using
cut options based on total distillate taken before evolving strategies based on
stream compositions. This is because it is easy in initial calculations to make
incompatible demands on the cut patterns, e.g. when switching from one cut on
distillate composition to a cut based on kettle composition (which may already
have been exceeded). Once a feasible cut pattern has been evolved this can
then be translated into a policy which more clearly corresponds to likely practice viz: cuts determined by column top temperature, kettle temperature, etc.
6.4.5 Liquid Holdup
Holdup in the column will determine the residual level of volatile impurity of a
product drawn (with column drainings) from the still. Similarly, holdup in the reflux
drum will dominate distillate purity, especially when the volatile product is a minor
component in the feedstock. These effects can only be realistically predicted
using a simulation model.
Since holdup in the system can have drastic consequences for product quality
some initial guess at holdup is required even before a hydraulic design is
undertaken. For a column with 10 theoretical stages the total column holdup may
be initially taken as 2% of batch charge; for a greater number of theoretical plates
the column holdup should be scaled in direct proportion. The holdup in the
condenser/reflux system may initially be taken as 1% of the batch charge.
Once a feasible plateage/cut policy has been evolved a preliminary hydraulic
design (together with tray/packing efficiency) should be undertaken to re-assess
the holdup pattern. For a tray column the holdup is essentially the clear liquor
depth on the tray. For packed columns the various holdup correlations in the
literature (see GBHE-PEG-MAS-612) should be regarded as giving order-ofmagnitude estimates only. Similarly the holdup in the condenser/reflux systems
will
have to be re-estimated; this is usually done on the basis of holdup time in the
reflux drum (which may need to be substantial if the drum also serves to
separate two-liquid phases).
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6.5
Once the designer has set up an initial simulation, the subsequent evolution is an
iterative process in which several variables (reflux ratio, top pressure, cut points,
etc.) are manipulated. A cut point policy is usually evolved around the recovery
and purity of the major (most valuable) product stream.
In virtually all cases simplicity of the process sequence and its control will be
critical to both minimal capital and to successful operation. For instance, the total
number of cut fractions is usually kept to a minimum to minimize storage
requirements for intermediate fractions. Off-spec material may be accumulated
simply as "fores" and "tails" cuts for reworking. Obviously, simulation of the
overall cycle has to include the rework distillations together with correction for
any recovered material that is recharged with the main batch. There is a general
preference to adopt a cut policy (viz. changes of reflux ratio, etc.) that is as
simple as possible using essentially step changes in operation rather than
ramped changes. For example, a ramped reflux policy to maintain a fixed
distillate composition may only be feasible with direct on-line analysis and would
probably be too unreliable for most practical applications in multi-purpose plant.
Similarly, various cuts may be deliberately "overdone" in order to avoid a length
analysis. Deliberate cycling operation (ie. repeated intermittent take-off, possibly
including draining the reflux drum, after a period at total reflux) is not a generally
adopted first design practice on plant-scale units though some applications have
been reported in Petrochemicals Division (see Bibliography, ref 1).
As the design of the still and its auxiliaries evolves, an increasing number of
details should be reconsidered in case they influence the process requirements.
Examples include:
(a)
column hydrodynamics at all stages of the distillation (e.g. varying masstransfer efficiency and column pressure drop in vacuum duties),
(b)
suitable instruments and controls for all stages of the distillation (e.g. the
need for specialized instruments on nominated cuts; fast response valves
for small cut fractions),
(c)
(d)
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(e)
(f)
the area available in the still for disengagement of any foam. This is
almost impossible to characterize and may occur at any stage of the
distillation restricting the permissible boilup rate.
6.6
It is possible, using the facilities within CHEMCAD, for continuous feed addition
within the program to solve two quite common cases:
(a)
(b)
in azeotropic distillation where the distillate splits into two phases, one of
which is returned to the column as reflux.
Kettle reboilers
Kettle reboilers are almost invariably used on multi-purpose stills. The tube
bundle should be mounted low in the kettle to ensure good heat-transfer when
high boil-downs (e.g. up to 90% of charge) are required. This consideration
involves mechanical constraints as noted below and may force tight tube spacing
(thus limiting heat-transfer performance) to keep the coils submerged. In some
cases a dual-exchange bundle is installed so that the upper bundle can be
turned off part way through the boil-down. Finned tubes have been proposed in
some non fouling duties but have not been widely adopted in the industry.. The
designer should ensure sufficient disengagement area to avoid priming the still
contents into the column; this can be particularly difficult at the end of a
distillation if accumulated tars promote priming.
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Column Internals
Condensers and reflux split boxes used in batch distillation are usually of
conventional design and external to the column. As discussed previously, the
holdup in the reflux drum may limit the achievable separation of a column and
various low inventory reflux splitter arrangements are available (see Bibliography,
ref 2). If timed reflux splitting is adopted the pulse rate should reflect the
(notional) holdup on the top tray to avoid pulsing the column profile. Swinging
bucket reflux splitters have been used in columns up to 1 m diameter. Use of
pumped reflux is not common since it is frequently desirable to drain the
overheads by gravity to storage.
For small-scale columns or high vacuum duties (say below 20 mm Hg head
pressure) there may be considerable advantage in using an internal condenser;
however, reflux flow control (particularly at high reflux) may be more difficult. This
may be simplified by using an internal dephlegmator (to provide reflux) together
with an external condenser (the reflux rate being essentially fixed by the cooling
water supply to the dephlegmator). In small duties the reflux drum may be
combined with the condenser bonnet. The "Spotton" reflux divider is one
commercially available splitter which has proved satisfactory in a number of
applications since it provides reproducible splits over a wide range of flows with
only a small holdup (see Bibliography, ref.6).
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The main features of mechanical design which are particular to batch stills
include:
(a)
Kettle reboiler heads where the tube bundle may need to be located close
to the knuckle radius when a high boil down is required.
(b)
(c)
The risk of implosion when a cold feed is charged to a still which is full of
hot vapors. For normal materials of construction the entire still system
should be designed to withstand full vacuum since this is preferable to
providing a vacuum protection facility.
(d)
Where a column is to be mounted directly onto an agitated vessel the offcentre load may limit the size of column.
FIGURE 3
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FIGURE 3
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10
BIBLIOGRAPHY
REF.
1
D J Facey
Petrochemicals Division. Process Design Methods No 3/4
15 Jan 1973
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APPENDIX A
A.1
PROBLEM
Where
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Where
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A.4
SOLUTION
The equilibrium diagram (see Figure 4) shows that to produce distillate D from
feed F the reflux ratio has to exceed not only the line DF but also (because the
curve is inflected ) the tangent to the curve from D. This point of tangency is
located approximately at (0.600, 0.695) and the minimum L/V ratio is thus:
The operating (L/V) ratio is taken as being about 1.5 times the minimum; for
these calculations we will assume an (L/V) ratio of 0.75 which corresponds to a
reflux ratio of 3.
A series of McCabe-Thiele plots is then made for a number of distillate
compositions in the range of interest. An example of one of these for xD = 0.800
is given in Figure 5 using a reflux ratio of 3 with 7 theoretical plates which
correspond to a still composition (xW) of 9.06% ethanol. The results of these
diagrams are as follows:
A plot of 1/(xD > xW) against xW is then prepared (see Figure 6). A trial and error
procedure is then used to satisfy the equations 1 and 2 by integrating between
the initial liquid composition (0.18) and various lower limits until the equations are
satisfied and an average distillate composition of 0.8 is reached. The results are
as follows:
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The final still composition will then be about 4% ethanol and will correspond to a
distillate recovery of 520-424, i.e. 96 moles. From equation 3 the required time
for distillation will be:
Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown
Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass
Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance
Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts /
Process Technology Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology Petrochemicals
Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries
Web Site: www.GBHEnterprises.com
Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown
Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass
Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance
Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts /
Process Technology Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology Petrochemicals
Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries
Web Site: www.GBHEnterprises.com
Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown
Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass
Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance
Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts /
Process Technology Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology Petrochemicals
Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries
Web Site: www.GBHEnterprises.com
ENGINEERING GUIDES
GBHE-PEG-MAS-603
GBHE-PEG-MAS-611
GBHE-PEG-MAS-612
Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown
Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass
Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance
Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts /
Process Technology Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology Petrochemicals
Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries
Web Site: www.GBHEnterprises.com
Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown
Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass
Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance
Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts /
Process Technology Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology Petrochemicals
Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries
Web Site: www.GBHEnterprises.com