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The set of feasibile composition profiles for ternary mixtures based on the existence
of a column section is bounded by the total and termini (beginning or end points) of
reflux and minimum reflux (reversible distillation boundaries and the stability of
operating) composition profiles singular points. This classification system
(Wahnschafft et al., 1992) i.e. the residue enables one to link candidate entrainers
curve and pinch point curve passing directly to flowsheets facilitating the desired
through the product composition. These separation between azeotrope-forming
regions form the basis of a feasibility test: If components a and b.
the bounds of the composition profiles do Singular points, which are pure
not intersect or overlap, the two proposed components and azeotropes, are labelled
products cannot be obtained in a according to the convention shown in Fig. 1.
single-feed column. This concept is an secondary
product 1. Primary product
extension of the one proposed by Levy et al. 1 2. Secondary product
3. Entrainer
(1985), who uses the intersection of liquid 0.8
2 4. Binary azeotrope to be
separated
Table 1. Key to standard distillation line map classification – ijk (l) – z Type p (q)
Classes*:
- 023 Classes*:
- 320 Classes*: - 323
- 104 - 323 - 114
- 014 - 114
Classes*:
Classes*: Classes*:
- 400-M
- 400-M - 124-m
- 200-m
- 200-m - 214-m
- 423-M
- 324-M
Classes*:
Classes*: - 214-m
- 214-m - 124-m
- 124-m - 423-M
- 423-M - 324-M
- 324-M
Fig. 2: Standard distillation line maps corresponding to feasible entrainers for which the
two pure products are located in the same distillation region. One of the products is a
saddle. (*: Existing classification of Stichlmair and Herguijuela, 1992)
Sutijan, Megan Jobson, and Robin Smith 27
Classes*: Classes*:
- 030 - 301
- 001 - 130
Classes*:
- 213
Classes*: - 312
- 031 - 132
- 130 - 431
- 134
- 314
Classes*:
- 123 Classes*:
- 321 - 040-M
- 231 - 002-m
- 341
- 143
- 413
Classes*:
Classes*: - 041-M
- 041-M - 401-M
- 401-M - 032-m
- 032-m - 230-m
- 230-m
Fig. 3: Standard distillation line maps for entrainers for which two pure
products are located within the same distillation region. Both products are
saddles. (*: Existing classification of Stichlmair and Herguijuela, 1992)
products are nodes and are connected by three-column flowsheets can be generated
distillation boundaries or so that all column specifications satisfy the
composition-space boundaries via a common saddle criterion, which indicates
saddle-type ternary or binary azeotrope. column feasibility (Rooks et al., 1998; Thong,
For these entrainers, two-column or 2000). An example of an entrainer of this
28 Synthesis of Ternary Homogeneous Azeotropic Distillation Sequences: Entrainer Selection
Classes*:
Classes*: - 120
- 020 - 201 Classes*:
- 004 - 430 - 102
- 304 - 012
- 043
- 340
Classes*:
Classes*:
Classes*: - 021
- 221
- 102 - 201
- 212
- 012 - 430
- 443
- 043 - 304
- 344
- 340
Classes*: Classes*:
- 221 - 122
- 122 - 212
- 434 - 221
- 344 - 443
- 434
- 344
Fig. 4: Standard distillation line maps for promising entrainers where the two node-type
desired products are located in different distillation regions. (*:Existing classification of
Stichlmair and Herguijuela, 1992)
type and a feasible flowsheet not previously in one or both desired products being
identified as suitable, is shown in Fig. 5. Fig. saddles in the distillation line map. Using a
6 represents standard distillation line maps combination of a double-feed column and
for feasible entrainers where the ternary boundary shifting, or recycling and mixing,
azeotrope is not of the same type as the entrainers which introduce a distillation
binary azeotrope of interest. boundary between the two components to
The criteria of Stichlmair and Herguijuela be separated, one of which is a saddle, can
(1992) always reject entrainers which result still facilitate the desired separation. Such
Sutijan, Megan Jobson, and Robin Smith 29
B
1
B2 Binary azeotrope : unstable node
distillation boundary (minimum boiling azeotrope)
0.8 at P 1
Ternary azeotrope : saddle
0.6 C-2
azeotrope (P1)
azeotrope (P2)
0.4 D1 feed
distillation boundary
0.2 C-1 at P 2
D2
B1
0
0 0.2 0.4 0.6 0.8 1
E A
Fig. 5: Example of a distillation line map XOX(12) type O for an entrainer that introduces a
ternary azeotrope of a different type to the binary azeotrope of interest. A two-column
flowsheet with boundary shifting can facilitate the separation.
Classes*:
Classes*: Classes*: - 011-S
- 003-S - 110-S - 101-S
- 010-S - 101-S - 330-S
- 330-S - 033-S
- 033-S
Classes*:
Classes*: - 112-S
- 121-S - 211-S
- 211-S - 433-S
- 343-S - 334-S
- 433-S
Fig. 6: Standard distillation line maps for promising entrainers in which the two node-type
desired products are located in different distillation regions. The entrainer introduces a
ternary azeotrope of a different type (i.e. maximum, intermediate or minimum boiling) to the
azeotrope of interest. (*: Existing classification of Stichlmair and Herguijuela, 1992)
Classes*: Classes*:
- 201 - 021
- 120 - 120
- 403 - 034
- 043 - 304
Table 2. Some physical properties, distillation line map characteristics and corresponding
feasible flowsheets of candidate entrainers for the separation of an acetone-chloroform
mixture.
(BS: boundary shifting, BC: boundary crossing, RM: recycling and mixing, DF: double feed
column)
once the ternary mixtures have been advantage of the new characterisation
classified (see Table 2). Of the candidate system is that suitable flowsheets can be
entrainers, only methanol is not suitable: in identified immediately. A new set of
this case the two products would be both entrainer selection criteria is defined; it
saddles separated by a distillation boundary. expands significantly the set of previously
For this class of distillation line maps, there published criteria by accepting many
is no feasible flowsheet that can be candidate entrainers that violate existing
generated. Detailed discussion on feasible entrainer screening criteria.
flowsheet identification will be presented in This new classification system allows
a further work. promising entrainers to be identified easily
and potentially feasible flowsheets to be
CONCLUSIONS derived directly. The methodology is
therefore valuable and powerful for the
A new classification system for synthesis of ternary homogeneous
homogeneous ternary azeotropic mixtures azeotropic distillation processes.
has been developed for the purposes of
screening candidate entrainers for ACKNOWLEDGMENTS
separating a binary azeotropic mixture into
its pure component products. The The authors thank the Engineering
‘standard distillation line map’ is classified Education Development Project of Indonesia
according to the presence and termini of for their financial support of Dr Sutijan.
distillation boundaries and the type
(stability) of binary azeotropes and products. References
Entrainers that induce liquid-phase splitting
are not addressed in this work. The key Bauer, M.H. and Stichlmair, J., (1995),
32 Synthesis of Ternary Homogeneous Azeotropic Distillation Sequences: Entrainer Selection
enhanced distillation, Chem. Eng. column, Ind. Eng. Chem. Fundam., 24,
Prog., 1989, 85 (1), pp. 63-69 pp. 454-463.
Stichlmair, J., Herguijuela, J.R, (1992), Wahnschafft, O.M.; Koehler, J.W., Blass, E.And
Separation regions and processes of Westerberg, A.W., (1992), The product
zeotropic and azeotropic ternary composition regions of single-feed
distillation, AIChE J., 38, pp. azeotropic distillation columns, Ind.
1523-1535. Eng. Chem. Res., 31, pp. 2345-2362.
Thong, D. Y-C., (2000a), Multicomponent Wahnschafft, O.M. And Westerberg, A.W.,
Azeotropic Distillation Design, PhD (1992), The product composition
Thesis, UMIST, Manchester. regions of azeotropic distillation
Thong, D. Y-C., (2000b), Research update on columns. 2. Separability in two-feed
two-feed distillation, unpublished columns and entrainer selection, Ind.
paper, UMIST, Manchester, UK. Eng. Chem. Res., 32, pp. 1108-1120.
Van Dongen, D.B. and Doherty, M.F., (1985), Widagdo, S. and Seider, W.D., (1996),
Design and synthesis of Azeotropic distillation, AIChE J., 42, pp.
homogeneous azeotropic distillations. 96-130.
1. Problem formulation for a single
column, Ind. Eng. Chem. Fundam., 24,
pp. 454-463.
Wahnschafft, O.M.; Koehler, J.W., Blass, E.