Batch distillation

Batch distillation[1] refers to the use of distillation in batches, meaning that a mixture is distilled
to separate it into its component fractions before the distillation still is again charged with more
mixture and the process is repeated. This is in contrast with continuous distillation where the
feedstock is added and the distillate drawn off without interruption. Batch distillation has always
been an important part of the production of seasonal, or low capacity and high-purity chemicals.
It is a very frequent separation process in the pharmaceutical industry.

Batch rectifier
Diagram of a Batch Rectifier

The simplest and most frequently used batch distillation configuration is the batch rectifier,
including the alembic and pot still. The batch rectifier consists of a pot (or reboiler), rectifying
column, a condenser, some means of splitting off a portion of the condensed vapour (distillate)
as reflux, and one or more receivers.

The pot is filled with liquid mixture and heated. Vapour flows upwards in the rectifying column
and condenses at the top. Usually, the entire condensate is initially returned to the column as
reflux. This contacting of vapour and liquid considerably improves the separation. Generally, this
step is named start-up. The first condensate is the head, and it contains undesirable
components. The last condensate is the feints and it is also undesirable, although it adds flavor.
In between is the heart and this forms the desired product.

The head and feints may be thrown out, refluxed, or added to the next batch of mash/juice,
according to the practice of the distiller. After some time, a part of the overhead condensate is
withdrawn continuously as distillate and it is accumulated in the receivers, and the other part is
recycled into the column as reflux.
Owing to the differing vapour pressures of the distillate, there will be a change in the overhead
distillation with time, as early on in the batch distillation, the distillate will contain a high
concentration of the component with the higher relative volatility. As the supply of the material is
limited and lighter components are removed, the relative fraction of heavier components will
increase as the distillation progresses.

Batch stripper

Diagram of a Batch Stripper

The other simple batch distillation configuration is the batch stripper. The batch stripper
consists of the same parts as the batch rectifier. However, in this case, the charge pot is located
above the stripping column.
During operation (after charging the pot and starting up the system) the high boiling
constituents are primarily separated from the charge mixture. The liquid in the pot is depleted in
the high boiling constituents, and enriched in low boiling ones. The high boiling product is routed
into the bottom product receivers. The residual low boiling product is withdrawn from the charge
pot. This mode of batch distillation is very seldom applied in industrial processes.

Diagram of a Middle Vessel Column

Middle vessel column

A third feasible batch column configuration is the middle vessel column. The middle vessel
column consists of both a rectifying and a stripping section and the charge pot is located at the
middle of the column.

Feasibility studies

Generally, the feasibility studies of batch distillation are based on analyses of the following
maps:

Residue curve map

still path map

distillate path map

different column profile maps

During the feasibility studies, the following basic simplifying assumptions are made:

infinite number of equilibrium stages

infinite reflux ratio

negligible tray hold-up in the two column sections

quasi-steady state in the column

constant molar overflow

Bernot et al.[2] used the batch distillation regions to determine the sequence of the fractions.
According to Ewell and Welch,[3] a batch distillation region gives the same fractions upon
rectification of any mixture lying within it. Bernot et al.[2] examined the still and distillate paths
for the determination of the region boundaries under high number of stages and high reflux ratio,
named maximal separation. Pham and Doherty in pioneering work[4] described the structure and
properties of residue curve maps for ternary heterogeneous azeotropic mixtures. In their model,
the possibility of the phase separation of the vapour condensed is not taken into consideration
yet. The singular points of the residue curve maps determined by this method were used to
assign batch distillation regions by Rodriguez-Donis et al.[5][6] and Skouras et al.[7][8] Modla et
al.[9] pointed out that this method may give misleading results for the minimal amount of
entrainer. Lang and Modla[10] extended the method of Pham and Doherty and suggested a new,
general method for the calculation of residue curves and for the determination of batch
distillation regions of heteroazeotropic distillation.

Lelkes et al.[11] published a feasibility method for the separation of minimum boiling point
azeotropes by continuously entrainer feeding batch distillation. This method has been applied
for the use of a light entrainer in the batch rectifier and stripper by Lang et al. (1999)[12] and it
applied for maximum azeotropes by Lang et al.[13] Modla et al.[9] extended this method for batch
heteroazeotropic distillation under continuous entrainer feeding.

See also

Azeotropic distillation

Extractive distillation

Fractional distillation

Heteroazeotrope

Steam distillation

Vacuum distillation

Theoretical plate

References

1. Kister, Henry Z. (1992). Distillation Design (1st ed.). McGraw-Hill. ISBN 978-0-07-034909-4.

2. Bernon, Christine; Doherty, Michael F.; Malone, Michael F. (1990). "Patterns of composition change in
multicomponent batch distillation". Chemical Engineering Science. Elsevier BV. 45 (5): 1207–1221.
doi:10.1016/0009-2509(90)87114-8 (https://doi.org/10.1016%2F0009-2509%2890%2987114-8) .
ISSN 0009-2509 (https://www.worldcat.org/issn/0009-2509) .

3. Ewell, R. H.; Welch, L. M. (1945). "Rectification in Ternary Systems Containing Binary Azeotropes".
Industrial & Engineering Chemistry. American Chemical Society (ACS). 37 (12): 1224–1231.
doi:10.1021/ie50432a027 (https://doi.org/10.1021%2Fie50432a027) . ISSN 0019-7866 (https://www.w
orldcat.org/issn/0019-7866) .
 4. Pham, Hoanh N.; Doherty, Michael F. (1990). "Design and synthesis of heterogeneous azeotropic
distillations—II. Residue curve maps". Chemical Engineering Science. Elsevier BV. 45 (7): 1837–1843.
doi:10.1016/0009-2509(90)87059-2 (https://doi.org/10.1016%2F0009-2509%2890%2987059-2) .
ISSN 0009-2509 (https://www.worldcat.org/issn/0009-2509) .

5. Rodríguez Donis, Ivonne; Gerbaud, Vincent; Joulia, Xavier (2002). "Feasibility of heterogeneous batch
distillation processes". AIChE Journal. Wiley. 48 (6): 1168–1178. doi:10.1002/aic.690480605 (https://doi.
org/10.1002%2Faic.690480605) . ISSN 0001-1541 (https://www.worldcat.org/issn/0001-1541) .

. Donis, Ivonne Rodríguez; Esquijarosa, Jhoany Acosta; Gerbaud, Vincent; Joulia, Xavier (2003).
"Heterogeneous batch-extractive distillation of minimum boiling azeotropic mixtures". AIChE Journal.
Wiley. 49 (12): 3074–3083. doi:10.1002/aic.690491209 (https://doi.org/10.1002%2Faic.690491209) .
ISSN 0001-1541 (https://www.worldcat.org/issn/0001-1541) .

7. Skouras, S.; Kiva, V.; Skogestad, S. (2005). "Feasible separations and entrainer selection rules for
heteroazeotropic batch distillation". Chemical Engineering Science. Elsevier BV. 60 (11): 2895–2909.
doi:10.1016/j.ces.2004.11.056 (https://doi.org/10.1016%2Fj.ces.2004.11.056) . ISSN 0009-2509 (http
s://www.worldcat.org/issn/0009-2509) .

. Skouras, S.; Skogestad, S.; Kiva, V. (2005). "Analysis and control of heteroazeotropic batch distillation".
AIChE Journal. Wiley. 51 (4): 1144–1157. doi:10.1002/aic.10376 (https://doi.org/10.1002%2Faic.1037
6) . ISSN 0001-1541 (https://www.worldcat.org/issn/0001-1541) .

9. Modla, G.; Lang, P.; Kotai, B.; Molnar, K. (2003). "Batch heteroazeotropic rectification of a low α mixture
under continuous entrainer feeding". AIChE Journal. Wiley. 49 (10): 2533–2552.
doi:10.1002/aic.690491009 (https://doi.org/10.1002%2Faic.690491009) . ISSN 0001-1541 (https://ww
w.worldcat.org/issn/0001-1541) .

10. Lang, P.; Modla, G. (2006). "Generalised method for the determination of heterogeneous batch distillation
regions". Chemical Engineering Science. Elsevier BV. 61 (13): 4262–4270. doi:10.1016/j.ces.2006.02.004
(https://doi.org/10.1016%2Fj.ces.2006.02.004) . ISSN 0009-2509 (https://www.worldcat.org/issn/0009-
2509) .

11. Lelkes, Z.; Lang, P.; Moszkowicz, P.; Benadda, B.; Otterbein, M. (1998). "Batch extractive distillation: the
process and the operational policies". Chemical Engineering Science. Elsevier BV. 53 (7): 1331–1348.
doi:10.1016/s0009-2509(97)00420-x (https://doi.org/10.1016%2Fs0009-2509%2897%2900420-x) .
ISSN 0009-2509 (https://www.worldcat.org/issn/0009-2509) .
12. Lang, P.; Lelkes, Z.; Otterbein, M.; Benadda, B.; Modla, G. (1999). "Feasibility studies for batch extractive
distillation with a light entrainer". Computers & Chemical Engineering. Elsevier BV. 23: S93–S96.
doi:10.1016/s0098-1354(99)80024-6 (https://doi.org/10.1016%2Fs0098-1354%2899%2980024-6) .
ISSN 0098-1354 (https://www.worldcat.org/issn/0098-1354) .

13. Lang, P.; Modla, G.; Benadda, B.; Lelkes, Z. (2000). "Homoazeotropic distillation of maximum azeotropes
in a batch rectifier with continuous entrainer feeding I. Feasibility studies". Computers & Chemical
Engineering. Elsevier BV. 24 (2–7): 1665–1671. doi:10.1016/s0098-1354(00)00448-8 (https://doi.org/10.
1016%2Fs0098-1354%2800%2900448-8) . ISSN 0098-1354 (https://www.worldcat.org/issn/0098-135
4) .

Further reading

Perry, Robert H. & Green, Don W. (1984). Perry's Chemical Engineers' Handbook (7th ed.).
McGraw-Hill. ISBN 978-0-07-049841-9.

Johann G. Stichlmair; James R. Fair (1998). Distillation: principles and practice. Wiley-VCH.
ISBN 978-0-471-25241-2.

I.M. Mujtaba (2004). Batch Distillation:Design and Operation. Imperial College Press. ISBN 978-
1-86094-437-6.

Hilmen Eva-Katrine, Separation of Azeotropic Mixtures:Tools for Analysis and Studies on Batch
Distillation Operation, Thesis, Norwegian University of Science and Technology Department of
Chemical Engineering, (2000).

Beychok, Milton (May 1951). "Algebraic Solution of McCabe-Thiele Diagram". Chemical

Engineering Progress.

External links

Batch distillation program online (http://petrochemical.gronerth.com/linkus.php?link=22)

Batch distillation of the hydrocarbon compounds.
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