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Designing a divided wall column

A refiner plans the application of divided wall column technology for greater
energy efficiency in the distillation of multi-component reformate

SAŠA POLOVINA, SREĆKO HERCEG and ANA GRANIĆ ŠARAC


INA

T
wo of the most important usually provides the heat to inevitable entropy losses, in
tasks facing refineries required for the separation particular due to remixing
today are to increase process. Condensation of over- within column sections and
conversion depth and to head vapour is used to take a interconnections and tempera-
increase energy efficiency. To certain amount of heat to gain ture differences in heat
achieve deep conversion, refin- the desired product. With exchangers.1
eries have started to invest in reboiling and condensation, a Energy efficiency in conven-
heavy residue processing. certain amount of energy is tional distillation (that is, classic
Increased energy efficiency is lost. distillation with one feed and
achieved by better utilisation of The minimum amount of two products) has been
all energy sources and by energy required for a reversible increased significantly in the
increasing heat recovery in distillation process (Qmin.) can last 20 years as a result of:
refinery processes. be described with Equation 1: • Better process control systems
Distillation is the most • Utilisation of high efficiency
common and important physi- Qmin. = ΔS Tc / (1-Tc/Th) internals
cal separation method. • Using side heat exchangers
Therefore it is not surprising where ΔS = change in entropy enabling use of cheaper utilities
that attention is dedicated to Tc = high temperature in the • Heat integration
increasing energy efficiency in reboiler • Heat pump assisted
this process. Distillation is also Th = low temperature in distillation.
a process that is responsible for condenser. However, the only way to
a large percentage of the According to the second law minimise energy losses that are
world’s energy consumption. of thermodynamics, change in caused by a remixing effect in
Due to its significant energy entropy can be defined as: the separation of multi-compo-
inefficiencies, some call it the nent mixtures is to apply the
‘energy dark horse’. It is known ΔS = -R Σ Xiln (Xi) principle devised by Petlyuk.2
that distillation represents According to this, in every
about 95% of all separations in where R = universal gas column in the sequence, only
the chemical industry and that, constant the easiest separation can be
in the US alone, about 40 000 Xi = molar fraction of compo- performed. This is the principle
distillation columns exist in all nent i. on which so-called divided wall
industries. The energy usage Q in columns (DWC) are based.
Distillation is a thermal sepa- conventional distillation Separation is achieved by using
ration process, where reboiling arrangements is typically more a vertical partition wall that
part of the bottom liquid than 50% higher than Qmin. due divides mainly the central part

www.eptq.com PTQ Q1 2016 1


A

A B A
AB

ABC BC
ABC

C C B

Figure 1 Direct and indirect sequence of distillation columns for the separation of a ternary mixture3

therefore there is a huge delay


in the application of this tech-
nology. Another reason for its
poor adoption is potential
A issues in process control. As the
divided wall column has
AB greater numbers of degrees of
freedom than a conventional
distillation column, for proper
B and safe operation of the
process it is necessary to
ABC
harmonise significantly larger
B number of variables.

Development and application


BC of divided wall columns
In conventional distillation
technology, separation of multi-
component mixtures of three
C products is carried out in at
least two consecutive columns
(the number of distillation
Figure 2 The so-called prefractionator sequence for separation of three columns required in series is
products3 equal to the number of prod-
ucts, minus one). Figure 1
of the column into a prefrac- non-welded wall technology it shows an example of two possi-
tionator and main column is possible to use this principle ble sequences for separating
sections. In each section, two for separation of multi-compo- three products: the so-called
components with the greatest nent mixtures consisting of four direct and indirect sequences.
difference in volatility are sepa- or more products. Figure 2 shows another possi-
rated, while others are allowed The main obstacle to greater bility: a sequence of three
to distribute.3 The biggest expansion of this technology columns. The first column in
application for divided wall lies in the fact that there is no the series is a prefractionator or
columns was separation of reliable method for calculation column that has no products,
mixtures of three products. of distillation and dimension- but is used for sharp separation
Now, after the introduction of ing of the column, and of components with the great-

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est difference in the relative
A
volatility (of components A and
Brugma’s sequence
C), while the middle-boiling
component B is distributed in
the top and bottom products of A
the prefractionator. The final AB

separation is performed in two


distillation columns. In one ABC

column, separation of compo- B


nents A and B is carried out,
and in the other components C BC
and B are to be separated. In
this way, the middle-boiling
component B is removed from
the bottom of one column and
C
from the top of the second
column. This configuration, B
although it requires more Petlyuk’s sequence
equipment (one column and
two heat exchangers) compared
A
to the direct/indirect AB
sequences, can lead to signifi-
cant reduction in the amount of ABC
energy required to perform the
B
same separation task, due to
avoidance of energy losses
related to remixing of compo-
BC
nent B.
If the reboiler of the top
column and condenser of the
bottom column are thermally C
coupled (see Figure 2), capital
cost savings can be achieved. Figure 3 Brugma’s sequence (a) and Petlyuk’s sequence (b) of distillation
The first example of the columns for separation of three products2,4
described distillation sequence
enabled reduction of energy shows two sequences of distil- vapour flow in direct and indi-
and investment costs, by use of lation columns for separation of rect conventional distillation
an additional evaporator three products.2,4 series and for Petlyuk’s pseudo
(reboiler) and condenser A study in 1972 confirmed and normal design showed
located in the prefractionator.4 substantial energy savings, significant savings for the
Petlyuk described the design of which can be achieved by latter.7 Underwood’s equations
fully thermally coupled distilla- usage of a thermal connection were used for the calculation of
tion columns.2 The reboiler and for the separation of compo- minimum required vapour. A
condenser in this configuration nents with close boiling points.5 further study indicated that
are located at the main column A later study of the separation Petlyuk’s design has five
and the reboiler and condenser of ternary mixtures6 recom- degrees of freedom, which was
of the prefractionator are mended operation of Petlyuk’s the basis for the further devel-
replaced with thermal coupling pseudo-column if the concen- opment of distillation
to the main column. In this tration of component B (middle technology.8
way, the heat required for sepa- component) in a mixture is The first proposed applica-
ration is provided with a single between 40% and 80%. A tion of the divided wall for
reboiler and condenser. Figure 3 comparison of the optimal separation of ternary mixtures

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head of the column and sepa-
rated by a divided wall. Such a
column is called a fully ther-
A mally coupled column. When
Reflux liquid from column 2
the system is properly oper-
SEC-3 ated, the potential energy
Vapour feed to column 2 Column 2 savings can be 20-40%,
Reflux liquid from column 1 Descent drops to column 2 compared to conventional
SEC-1 SEC-4 distillation systems. The first
B
Column 1
divided wall column was
designed at BASF SE in
Feed Reflux liquid from column 3
Ludwigshafen, Germany.
SEC-2 SEC-5
Column 3
Liquid feed to column 3
Design basis
Design of divided wall columns
SEC-6
is carried out in several steps:
• Shortcut calculation (Vmin
diagram)
C
Liquid • Rigorous calculation and
Vapour
optimisation
• Column sizing – hydraulic
Figure 4 SPE divided wall column for the separation of a ternary mixture11 design.

Shortcut calculation (Vmin


diagram)
PBC
PAB B The purpose of a shortcut calcu-
lation is to provide data that
PAC will be the basis for rigorous
calculation. One such method is
VT/F

A AB BC C the so-called Vmin diagram,


which is a graphical representa-
ABC tion of vapour and liquid flow
rates required to perform all
splits within a given distillation
1−q sequence. It is based on
Underwood’s equations, imply-
0 1
ing the following simplifications
D/F and conditions: infinite number
of theoretical stages, constant
Figure 5 Vmin diagram for separation of ternary mixtures into three products relative volatilities and constant
(q indicates quality of feed; q = 0 – saturated vapour; q = 1 – saturated molar flow rates in a column.
liquid)12 The required data for a Vmin
consisted of the main column component mixtures of three diagram are: composition of the
in a single shell with three side products in two distillation feed, relative volatilities,
products, where the feed input columns would be replaced by required key component splits,
and three side products were separation in a single divided and thermal condition of the
separated by a dividing wall.9 wall distillation column (see feed. Figure 5 shows a Vmin
Later work enabled application Figure 4).11 diagram for the separation of
of the dividing wall for separa- In a divided wall column, the ternary mixtures into three
tion in Petlyuk’s series.10 Using prefractionator as a separate products. The diagram illus-
new technologies, conventional unit has been abandoned. It is trates how the components of
distillation separation of multi- integrated into the shell of the the ternary mixture in a conven-

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tional distillation column, with through the dividing partition for fractionation of reformate
an infinite number of equilib- can be neglected. with a capacity of 80 t/h was
rium stages, are distributed The number of stages is set to simulated as the basis of the
between the top and bottom of 2.5Nmin (where Nmin is the design. The process was
the column depending on two number of equilibrium stages at modelled with ChemCAD
defined degrees of freedom total reflux) as calculated by the process simulator software. For
(D/F – net flow of product to Fenske equation in shortcut the modelling of vapour-liquid
the top per unit of feed; V/F – simulation. The flow rates of all equilibrium, the Soave-Redlich-
vapour flow rate above the streams are set to match the Kwong (SRK) equation was
feed). values obtained from the Vmin selected as one of the most
For a ternary mixture (to diagram. frequently used models for
obtain three products from hydrocarbon mixtures.
multi-component mixtures), Sizing – hydraulic design
three points need to be formu- After simulation, the process Simulation of the base case
lated: the point of sharp split parameters obtained are used Given the increasingly stringent
between components A and B, for sizing. A divided wall requirements for the content of
PAB; the point of sharp separa- column can be equipped as a benzene in motor gasoline,
tion of components A and C, conventional distillation reformate fractionation plant
PAC; and the point of sharp column, with various types of has become a strategically
separation of components B trays or packings. The differ- important process in refining.
and C, PBC. Initial values of ence compared to sizing a Reducing the benzene content
liquid and vapour molar flow conventional column is in the of heavy reformate enables the
rates in a divided wall column regulation of vapour split use of larger quantities of
can then be determined across the partition. The liquid heavy reformate for gasoline
through relations between split is easily regulated in oper- blending.
those peaks. ation, while the vapour flow on By separating the C5-C6 frac-
To calculate the minimal both sides of the wall depends tions of the products from
number of theoretical stages of primarily on resistance to flow, catalytic reforming (reformate),
the distillation process, which is provided by internal the concentration of aromatic
Fenske’s method is used, while elements of the column, inclina- components in heavy reformate
the Gilliand correlation tion of the wall, and by the is higher, which leads to an
provides the relationship wall itself. By proper sizing, increase in RON. Therefore, the
between reflux and number of equal pressure drop on both requirement for RON from the
required theoretical stages. sides of the wall is achieved, catalytic reformer (a semi-re-
Feed stage location is deter- meaning that vapour flow rates generative reformer) is smaller,
mined by the Kirkbride in operation will be the same as which means less severe work-
equation. in design. ing conditions, thereby
For the assessment of the significantly extending the
Rigorous calculation pressure drop in structured length of the catalytic cycle of
To obtain a basis for hydraulic packings, the Delft model is the plant.
design and sizing – that is, to used. Its biggest advantage As the feed for reformate
obtain the final values of the over other models is that it fractionation is composed of
design parameters, a rigorous does not require any special, many different types of mole-
simulation using commercial experimentally determined cules, for the purposes of
process simulators is needed. parameters for packings, only calculation, the number was
Such simulators do not incor- their geometric characteristics. reduced to 15 main compo-
porate a DWC model, so it is nents. Table 1 shows the
necessary to build up a thermo- Design of reformate chemical composition of such a
dynamically equivalent fractionation for a divided wall mixture. The first numeric data
sequence of conventional column row in Table 1 shows the chem-
columns. These models are Operation of INA Rijeka refin- ical composition of reformate
applicable if heat transfer ery’s existing plant (a splitter) for simulation.

www.eptq.com PTQ Q1 2016 5


Main parameters, composition of feed, quantity and compositions of benzene fraction must be 50-75
products obtained by simulation in base case (BRC – benzene rich cut) wt%
• The maximum benzene
Stream name Reformate Light reformate BRC Heavy reformate content of heavy reformate is
Temperature, °C 115.1569 40 40 143.2143 1.5 wt% and the process is opti-
Pressure, bar 2.8 2.7 1.7 1.7
Enthalpy, MW -13.472 -13.69 -0.18206 -0.13731 mal if the benzene content is
Total flow, kmol/hour 852.8956 269.9423 72.3152 510.8459 between 0.5-1 wt% by weight.
Total flow, kg/hour 80000.0367 21498.9317 5993.9609 52524.0687
Mass percentage, %
Operating modes used in the
i-pentane 6.300794 23.445995 0 0 daily operation of the existing
n-pentane 4.770194 17.750454 0 0 reformate fractionation plant
2-methylpentane 5.572594 20.736268 0 0
3-methylpentane 4.346296 16.173041 0.000001 0 (splitter) were utilised for defin-
n-hexane 5.371594 19.980904 0.000204 0 ing operating conditions. Also,
benzene 6.970397 1.904563 73.879582 1.434139
2,4-dimethylpentane 0.41 0.008776 5.426328 0.004345
the total number of trays (equi-
2-methylhexane 2.241398 0.000002 19.839668 1.154297 librium stages) and feeding
n-heptane 2.049998 0 0.850597 3.025316 points (tray ordinal number)
toluene 23.890366 0 0.003621 36.387306
ethylbenzene 4.264195 0 0 6.494849 were fixed according to the
p-xylene 5.507694 0 0 8.388839 existing plant operation. These
m-xylene 12.395789 0 0 18.88018
o-xylene 6.341793 0 0 9.65927 data were also taken as
1,2,4,5-tetramethylbenzene 9.566893 0 0 14.571458 unchangeable (constant)
throughout calculation. Thus,
Table 1 the calculation of a column for
separation of light reformate
Inlet parameters and results of rigorous calculation for the reformate and heavy reformate (322-C-
fractionation plant (capacity of 80 t/h) 001) was carried out with 77
trays and with feed entering the
Inlet parameters Results
30th tray, while the calculation
Inlet column temperature, °C Evaporator heat duty, MW of a column for separation of
322-C-001 115 322-H-001 13.6 benzene reach cut and heavy
322-C-002 154 322-H-002 3.7 reformate (322-C-002) was
Total 17.1
carried out with 52 trays and
Top column temperature, °C Condenser heat duty, MW with feed entering the 22nd
322-C-001 84 322-C-001 -13.4 tray.
322-C-002 97 322-C-002 -3.4 The composition of the feed,
Total -16.8
quantity and composition of
Bottom column temperature, °C Benzene content, % m/m the products obtained by simu-
322-C-001 154 Light reformate 1.9 lation in the base case at the
322-C-002 143 Benzene rich cut 73.8 capacity of 80 t/h are shown in
Heavy reformate 1.4
Table 1. The data obtained by
Top column pressure, bar strict calculation are in accord-
322-C-001 2.7 ance with actual process data
322-C-002 1.7 and the concentrations of

Reflux ratio
benzene in the products are
322-C-001 4.3 below standard limits. (Due to
322-C-002 4.5 the large number of compounds
in the products of reformate
Table 2 fractionation, daily analysis and
quality control is carried out
The distillation products have than 2 wt% only for controlling the benzene
to meet the following • n-hexane must end up in content of products.) Main
requirements: light reformate as much as values and process parameters
• Benzene content in light possible used for the calculation, as well
reformate must not be higher • The benzene content of the as the number of trays and feed

6 PTQ Q1 2016 www.eptq.com


point, are in accordance with Chemical composition of the feed, distribution coefficient at the feed
real process conditions. supply tray and the desired column distribution by components
In Table 2, inlet process
parameters and the results of Component Mole fraction Distribution coef. at a feed supply tray Product
rigorous calculation at a plant i-pentane 0.081913 3.289 D
n-pentane 0.062015 2.75 D
capacity of 80t/h are shown. 2-methylpentane 0.060654 1.578 D
3-methylpentane 0.047307 1.424 D
DWC design n-hexane 0.058466 1.283 D
benzene 0.083699 0.914 S
For calculation purposes, the 2,4-dimethylpentane 0.003838 0.986 S
feed composition was reduced 2-methylhexane 0.020981 0.762 S
n-heptane 0.019189 0.600 B
to 15 components, which were toluene 0.2432 0.402 B
arranged in order of increasing ethylbenzene 0.037674 0.196 B
p-xylene 0.04866 0.182 B
boiling point. Table 3 shows: the m-xylene 0.109516 0.178 B
composition as mole fractions o-xylene 0.05603 0.158 B
of the mixture that was used for 1,2,4,5-tetramethylbenzene 0.066857 0.03 B

the calculation of the divided ‘Key components’ shown in bold


wall column at 80 t/h; distribu-
tion coefficients at the feed Table 3
supply tray; and the desired
column products (D – distillate, Characteristic points of a Vmin diagram
B – bottom, S – average prod-
uct). The grouping of Specified in the calculation
components by resulting prod- Section Point Required separation
C1 PAC r(C,D)=0.005 r(A/B)=0.01
ucts corresponds to the C2,1 PAB r(B,D)=0.05 r(A/B)=0.4
situation in the base case. C2,2 PBC r(C,D)=0.08 r(B/B)=0.1
In the first phase of calcula- Results
VT/F D/F N Nf Nmin
tion, a shortcut calculation is 0.62 0.35 64 34 15
performed. In this step, each 1.03 0.29 64 47 16
0.78 0.4 67 45 17
section is observed as a sepa-
rate conventional distillation (C1 – prefractionator; C2,1 – main column above side product; C2,2 – main column below side product; F – feed;
VT – vapour molar flow through column; D – distillate molar flow through column)
column, where separation takes
place. For each product, a key
distillation component has to Table 4
be selected. These ‘key compo-
nents’ are for light reformate tion takes place between the feed and a bottom product with
n-hexane, benzene for the key component of light refor- 99.2% n-heptane in the feed to
benzene fraction, and n-hep- mate, n-hexane, and the key the column.
tane for heavy reformate. component of the middle prod- In this calculation, basic
In the first column, separa- uct, benzene. Distillate should parameters for the second
tion of components with the contain 60% n-hexane in the phase of the calculation (rigor-
greatest difference in relative feed to this column, and 95% ous calculation) were
volatility (n-hexane and n-hep- benzene in the feed should generated. For the purpose of
tane) takes place. For the remain in the bottom product rigorous calculation, a divided
calculation, distillate product of the column. wall column is regarded as
should contain 99% n-hexane in For the third column shortcut three conventional distillation
the feed, and 99.5% n-heptane distillation, a calculation for columns. The result of rigorous
in the feed should be recovered benzene, the key component of calculation is the minimum
at the bottom of this column. the middle product, and n-hep- vapour flow required for the
The minimum number of equi- tane, the key component of the separation. This minimum
librium stages required for the heavy reformate, is performed. vapour flow is then needed for
separation is also fixed. We require a top product the creation of a Vmin diagram,
In the second column separa- containing 90% benzene in the the third phase of calculation.

www.eptq.com PTQ Q1 2016 7


relationship between these two
1.2 variables, other variables can be
1.1 determined.
PAB
10 The highest point in the Vmin
0.9 diagram (PAB) represents the
PBC
0.8
minimum amount of vapour
0.7
required for the separation of
VT/F

0.6
PAC n-hexane and benzene. The
0.5
minimum amount of vapour is
0.4
0.3
related to the minimum
0.2 amount of energy required for
0.1 separation in thermally
0 connected columns.
0 0.1 0.2 0.3 0.4 0.5 0.6 0.7 0.8 0.9 1.0 Point PAC represents a
D/F preferred point and shows the
amount of vapour required for
Figure 6 Vmin diagram for the separation of three key products of reformate the separation of n-hexane and
in a divided wall column n-heptane in a prefractionator,
for the given amount and
purity of distillate product. The
Liquid L/D = 2.55 247 D
preferred point represents the
Vapour optimal means of operating the
distillation process for the
required purity of the product.
631 878
25
After the Vmin diagram is
RL = 0.330
constructed, material balance
calculations for the three distil-
212 21 531 419 13 347 lation columns should be
performed. The balance must
F 853 103 S
include liquid and vapour
1139 19 605 316 11 347 flows for each column (section).
These flows will be the basis
RV = 0.636
for sizing the divided wall
1455 28 952 column.
Figure 7 shows a vapour and
liquid material balance, with
V/B = 1.89 503 B distillate, middle product and
bottom product yields in ther-
Figure 7 Vapour and liquid material balance, and distillate, middle product and mally connected columns with
bottom product yields in thermally connected columns (F, D, S, B – molar flows a capacity of 80 t/h.
of feed, distillate, side product and bottom product; RL – Liquid splitting over A material balance was
dividing wall; RV – vapour splitting over dividing wall; L/D – reflux ratio; V/B – calculated from the balance
reboiling ratio)
equations, where one can start
from an initial value of the
Table 4 shows characteristic idea of the minimum energy required vapour flow rate from
points of a Vmin diagram needed for the required the evaporator, or from the top
generated by rigorous separation. of section 2.1, and the amount
calculation. By creating this diagram, the of distillate produced. In both
After determining the charac- required amount of vapour for cases, the amount of vapour
teristic points, a Vmin diagram the separation and the amount flow through the prefractiona-
can be constructed (see Figure of product distillate can be tor was determined based on
6). This diagram gives a clear determined. By defining the the Vmin diagram, so that

8 PTQ Q1 2016 www.eptq.com


operation of the prefractionator Feed and product parameters and composition determined by simulation
was in the area of the preferred of a reformate splitter as one thermally completely connected column
point. The rest of the vapour is
sent to the top of the main Reformate Light reformate BRC Heavy reformate
column, bypassing the prefrac- Temperature, °C 100 76.5658 108.5178 163.0543
Pressure, bar 2.7 2.7 2.7 2.7
tionation section. Total flow, kmol/hour 852.8957 236.2961 103.0002 513.6421
In the fourth phase of calcu- Total flow, kg/hour 80000.0509 18606.8835 8528.6865 52868.0441
Mass percentage, %
lation, data from the Vmin i-pentane 6.300794 27.0899 0.000009 0
diagram as well as data from a n-pentane 4.770194 20.509313 0.000142 0
rigorous calculation for each 2-methylpentane 5.572594 22.758687 2.608568 0
3-methylpentan 4.346294 15.619758 6.675395 0.000001
column served as initial points n-hexane 5.371594 12.220876 23.712844 0.000019
of calculation for the reformate benzene 6.970394 1.799891 55.30771 1.000001
2,4-dimethylpentane 0.41 0.00157 3.824329 0.002657
splitter. The capacity of the 2-methylhexane 2.241398 0.000001 7.388397 2.202627
reformate splitter is 80 t/h and n-heptane 2.049998 0 0.43665 3.032277
is a thermally completely toluene
ethylbenzene
23.89037
4.264196
0
0
0.045967
0.000002
36.144784
6.452656
connected column. The initial p-xylene 5.507695 0 0.000001 8.334335
number of equilibrium stages m-xylene 12.395791 0 0.000002 18.757503
o-xylene 6.341793 0 0 9.596482
was fixed at N ≥ 4Nmin. Feed 1,2,4,5-tetramethylbenzene 9.566893 0 0 14.476661
flow rates were fixed at a value
determined from the Vmin
diagram and material balance. Table 5
After convergence of simula-
tion in the process simulator Required number of equilibrium stages and the equivalent height of a
ChemCad, optimisation of the structured filler at 80 t/h capacity
distributed liquid and vapour
in the sections above or below
the wall was performed. Section Theoretical number of equilibrium stages Height of a packing bed, m
C1,1 21 8.4
The number of equilibrium C1,2 19 7.6
stages, N, was set at N ≥ C2,1 25 10
C2,2 13 5.2
2.5Nmin. Stages that do not take C2,3 11 4.4
part in separation were elimi- C2,4 28 11.2
nated. In this way, for the
prefractionator section, 40 equi-
librium stages were Table 6
determined, and for the main
column 80 equilibrium stages of 2.3 m at the widest point. To reduce pressure drop
were obtained. The interior of the column through section C1,2 and C2,4,
Table 5 shows the composi- consists of structured fillers. the height of a packing bed
tion of feed and products The Delft model was used to was decreased (compared with
determined by simulation of estimate the pressure drop height of a packing bed shown
the reformate splitter as one through the column.12 For all in Table 5), and the height of a
thermally completely connected sections, a height equivalent to packing bed was increased in
column. a theoretical plate (HETP) section C2,1. Feed enters the
value of 0.4 m was used. prefractionator part of the
Divided wall column sizing Table 6 shows the required DWC above tray 19; there are
For the reformate splitter at number of equilibrium stages 21 stages in the upper rectifi-
INA Rijeka refinery, column and the equivalent height of a cation section and 19 in the
C-001 was presumed to be of structured filler at the capacity lower stripping section. As a
sufficient size and was selected of 80 t/h, and Table 7 indicates result of prefractionation, we
for simulation of a divided the basic dimensions and esti- obtain a mix of light reformate
wall column. Column C-001 is mated pressure drop across the and BRC at the top of the
36 m high and has a diameter layers of the filler. rectification section and a mix

www.eptq.com PTQ Q1 2016 9


Heat duty of conventional separation sequence and DWC
Light reformate

Parameters 322-C-001 322-C-002 DWC


Evaporators heat duty, MW 13.6 3.7 8.52
Annual cost of consumed refinery fuel gas, Euro 3 259 363 1 805 359 Reflux

2.0
2.1.A
Table 8

n-hexsane
5.2

Top of main column


Condenser heat duty and related savings

2.0
Parameters 322-C-001 322-C-002 DWC
2.1.B
Condenser heat duty, MW -13.4 -3.4 -6.79
Annual cost of spent electrical energy, Euro 65 280 43 520

5.2
Table 9

2.0
of heavy reformate and BRC at dividers and seven liquid 1.1. 2.2.

Rectification section

Benzene
the bottom of the stripping collectors must be installed in

5.2
section. the column. Figure 8 shows the

8.4

n-heptane
In the top section 2.1 of the dimensions of the divided wall

Central part of column


main column, which has 26 column for separation of refor-

Refractionator
theoretical stages, light refor- mate at a capacity of 80 t/h.
BRC
mate is received. Part of it The result of sizing is a Feed

2.0
returns to the top as reflux. divided wall column with a 1.2. 2.3.

Striping section
The main column central height of 56 m, which fully

n-heptane

4.4
Benzene
section above the BRC product meets the required product
7.2
outlet 2.2 has 13 theoretical quality.
stages, and the section below
BRC outlet 2.3 has 11 theoreti- Energy savings of a divided
2.0

cal stages wall column


The bottom section 2.4 of the Energy savings are based on 2.4.A
main column consists of 28 better utilisation of heat in the
5.4

Bottom part of column


theoretical stages, and it has heat integrated column as well
the largest liquid load in the as on the elimination of a
column. Because separation in second column and accompa-
2.0

n-heptane
sections 2.1 and 2.4 requires a nying equipment. 2.4.B
large number of theoretical Table 8 shows heat duties of
5.4

equilibrium stages, the height condensers and evaporators for


of the structural filler has to be the existing columns and for
more than 10 m; these sections new DWC.
must be divided into two sepa- When we compare heat
5.0

rate layers. The upper part of duties for evaporators in a Heavy


the main column consists of conventional separation reformate

sections 2.1A and 2.1B contain- sequence with a DWC, we see


ing structured fillers with a that a DWC, for the same sepa-
height of 5.2 m, while the ration and the same product Figure 8 Sized divided wall column for
lower part of the main column quality requires 8.78 MW less reformate fractionation
consists of sections 2.4A and energy than the conventional
2.4B, containing structured fill- sequence. The reason lies in a evaporator. Table 8 also shows
ers with a height of 5.4 m. For completely thermally linked that by using a DWC, a refinery
better distribution of liquid on distillation column and in can save an annual €1 454 004
the surface of the filler, eight complete elimination of one in fuel gas.

10 PTQ Q1 2016 www.eptq.com


Annual cost estimation is nying equipment. All of the mode at which a greater
based on processing of 268 991 existing equipment (evapora- percentage of n-hexane would
t/y of feed. For processing tors and coolers) can also be finish in light reformate, whilst
1000 kg of feed in a conven- utilised for the DWC. The keeping the content of benzene
tional separation sequence, resulting reduction energy in light reformate below 2 wt%,
28.85 kg of refinery fuel gas is consumption of more than 50% was sought.
needed, while for the same would make investment in and Design of this type of column
quantity of processed feed in a operation of a DWC solution enables operation of the refor-
DWC, 15.98 kg of refinery fuel economically viable. mate splitter as one column
gas is needed. (The price of with three products, thus elimi-
refinery fuel gas is €0.42/kg of Conclusions nating the work of the second
feed.) Using a calculation method column, one furnace for reboil-
For calculation of a DWC, air with a Vmin diagram, a refor- ing column bottoms, and a
coolers were used as the most mate splitter in INA Rijeka system for condensing top
economical heat exchangers. refinery was redesigned as a product.
(Electrical energy costs €120/ divided wall column. After Sizing of a DWC was based
MWh.)1 Table 9 shows the simulation of the base case, a on the existing 322-C-001
condensers’ heat duty as well good match with actual process column. A column height of 56
as their electrical energy cost. conditions was observed. Then m (including internal architec-
The refinery can save an a complete calculation method- ture) would be sufficient to
annual €21 760 by using a ology for a divided wall obtain product quality.
DWC instead of a conventional column was performed. DWC would be about 20 m
separation sequence, based on Calculations include a basic higher than the existing 322-C-
268 991 t/y of feed processing. shortcut calculation, thorough 001 column, but this does not
For estimation of investment rigorous calculation, construc- exclude the possible redevelop-
costs, Dejanovic’s method was tion of Vmin diagram, thermal ment of an existing column to
used.13 Estimated investment connection of columns and DWC. The position of the
costs include the costs of sizing of the unit as a divided dividing wall, as well as flows
installing a new DWC shell, wall column. through the column sections
the internal architecture of the The Vmin method seems to and the corresponding pres-
column, and installation of an provide fast and relatively easy sure drop through the column,
evaporator and condenser. An estimates of operational flows, were calculated for 322-C-001
existing plant for reformate based on possible operational column’s diameter of 2.3 m,
fractionation was used as the or investment savings. and the calculation showed
basis for design. Investment Rigorous simulation of the that the diameter of the column
cost estimates for a conven- base state of the unit, at a is not a limiting factor for its
tional separation sequence and capacity of 80 t/h, showed a use as a DWC. The required
a DWC were made. good match with actual process height of the column can be
Initial calculations indicate parameters, and the quantity obtained by separating and
that, regardless of the much and quality (for instance redesigning with new parts a
higher investment costs of benzene content) of the result- section of the existing shell.
DWC equipment with struc- ing products correspond to the Preliminary economic calcu-
tured fillers, the cost of a new quantity and quality of the lations indicate that more than
DWC is no higher than the cost products produced by the 50% reduction in energy
of the present columns (taking actual reformate splitter unit. consumption would make
into account the accompanying In a process simulation using investment and operation of a
evaporators and condens- ChemCAD, separation of DWC economically viable.
er-coolers in both cases). This is benzene and n-hexane proved
logical because reformate frac- to be the hardest task, which Acknowledgement
tionation using DWC corresponds to engineering We would like to thank Dr Igor Dejanović
eliminates the investment costs experience in the operation of for his help and support in preparing
of one column with accompa- the actual unit. An optimal this article, and University FKIT, Zagreb,

www.eptq.com PTQ Q1 2016 11


for the use of ChemCAD simulation 1. Design comparisons, AICHE Journal, Saša Polovina is a Project Expert
software. 1978, vol 24, no 2, 303-315. with INA’s Belarus Naftan team. He
7 Fidkowski Z, Królikowski L, Thermally was previously Area Manager at INA’s
coupled system of distillation columns: Rijeka refinery and is now responsible
Optimization procedure, AICHE Journal, for making detailed engineering
References 1986, vol 32, no 4, 537-546. project plans, as well as supervision,
1 Halvorsen I J, Skogestad S, Energy 8 Chavez C R, Seader J D, Wayburn T commissioning and start-up of process
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Gas Science and Engineering, 2011, vol 3, interlinked separation systems, Industrial chemical engineering and technology
no 4, 571-580. & Engineering Chemistry Fundamentals, from the University of Zagreb, Croatia.
2 Petlyuk F B, Platonov V M, Slavinskii D 1986, vol 25, no 4, 566-576. Srećko Herceg is with INA’s Belarus-
M, Thermodynamically optimal method 9 Wright R O, Fractionation apparatus, Naftan team at JSC Naftan, Novopolotsk,
for separating multicomponent mixtures, US Patent 2471134, 1949. Belarus. Projects he has been working
International Chemical Engineering, 10 Kaibel G, Distillation columns with on include construction of a low
1965, vol 5, no 3, 555-561. vertical partitions, Chemical Engineering temperature isomerisation unit, revamp
3 Dejanović I, Razvoj metode & Technology, 1987, vol 10, no 1, 92-98. of a HDT diesel and naphtha unit, and
dimenzioniranja kolona s razdjelnom 11 Sumiju Plant Engineering Co. 2013, construction of a sulphur recovery unit
stjenkom (Developing of a model viewed 1 Nov 2012, www.spe.shi.co.jp/ with a sour water stripping unit. He has
for divided-wall columns’ design), en/distill1.html. been undertaking postgraduate study at
Doktorska disertacija, Sveućilište u 12 Rix A, Olujić, Ž, Pressure drop of the Faculty of Chemical Engineering and
Zagrebu, Fakultet kemijskog inženjerstva internals for packed columns, Chemical Technology at the University of Zagreb.
i tehnologije, Zagreb (in Croatian), 2010. Engineering and Processing: Process
4 Brugma A J, Process and device for intensification, 2008, vol 47, no 9-10, Ana Granić Šarac is a Process Engineer
fractional distillation of liquid mixtures 1520-1529. at INA’s Rijeka refinery, providing
more particularly petroleum, US Patent 13 Dejanović I, Matijašević L, Olujić technical support for processing
2295256, 1942. Z, Divided wall column application for plants including catalytic reforming,
5 Stupin W J, Lockhart F J, Thermally platformate splitter – a case study, hydrogen management and purification,
coupled distillation - a case history, Pierucci S, Buzzi Ferraris G (editors), isomerisation, LPG/gasoline Merox, and
Chemical Engineering Progress, 1972, vol 20th European Symposium on Computer gasoline hydrotreating. She graduated as
68, no 10, 71-72. Aided Process Engineering – ESCAPE20, a chemical engineer from the University
6 Tedder D W, Rudd D F, Parametric Elsevier B.V., Ischia, Naples, Italy, 6-9 of Zagreb’s Faculty of Chemical
studies in industrial distillation. Part June 2010. Engineering and Technology.

12 PTQ Q1 2016 www.eptq.com

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