Chemical Engineering and Processing 73 (2013) 151–157

Contents lists available at ScienceDirect

Chemical Engineering and Processing:

Process Intensification
journal homepage: www.elsevier.com/locate/cep

From laboratory experiments to simulation studies of methanol

dehydration to produce dimethyl ether reaction—Part II: Simulation
and cost estimation
Yadollah Tavan a,∗ , Seyyed Hossein Hosseini b
a
National Iranian Gas Company, Tehran, Iran
b
Chemical Engineering Department, Faculty of Engineering, Ilam University, 69315-516 Ilam, Iran

a r t i c l e i n f o a b s t r a c t

Article history: The vapor phase dimethyl ether (DME) synthesis is simulated by Hysys process simulation software
Received 25 April 2013 and relevant cost analysis is also conducted. Based on cost estimation results, it is found that capital
Received in revised form 3 August 2013 investment of the classic DME process is greatly influenced by the distillation towers and operating
Accepted 5 August 2013
costs. Accordingly, to solve these problems an innovative DME process based on a top-wall dividing-wall
Available online 12 September 2013
column (DWC) in vapor phase is proposed, in this work. It is shown that the novel proposed DWC process
leads to 44.53% reduction in operating costs compared to the conventional one, while both schemes
Keywords:
predict almost the same output specifications.
Simulation
DME © 2013 Elsevier B.V. All rights reserved.
Cost estimation
DWC
Hysys

1. Introduction 400 ◦ C and pressure up to 18 bar [2]. Among these catalysts, ␥-

alumina and HZSM-5 are extensively studied and attracted a great
Dimethyl ether (DME) is a clean, colorless gas that is easy to liq- deal of attention as potential catalysts due to their high activity and
uefy and transport. It has remarkable potential for increased use as proper stability [3–5].
an automotive fuel, for electric power generation, and in domes- Importance of DME has motivated numerous researches to focus
tic applications such as heating and cooking. It is produced from on investigation of various catalysts, while purification of DME
the variety of feed-stocks such as natural gas, crude oil, residual process has received much less attention. In the later part of this
oil, coal, waste products and bio-mass [1]. DME can be manufac- paper (part I), the proper kinetic models of DME production over
tured directly from synthesis gas produced by the gasification of the HZSM-5 and ␥-alumina catalysts in fixed bed reactor were
coal and biomass or through natural gas reforming and indirectly investigated [6]. In the present part (part II), separation of DME
via methanol dehydration reaction. In the direct path, methanol is through distillation technology is conceptually discussed and stud-
produced in the middle of the reaction and consumed in the dehy- ied.
dration reaction. Although direct DME production seems to be a A conventional process of DME synthesis typically includes two
more economical route but at the present, this process has not been serial distillation columns (direct sequence system) in which the
commercialized completely and almost all produced DME comes main disadvantage is its rather high investment costs and signif-
from the indirect process plants (Eq. (1)). icant energy requirements. The required energy is provided by
steam that its cost substantially makes a high contribution on the
2CH3 OH ↔ CH3 OCH3 + H2 O, Hrxn = −21.225 kJ/mol (1)
total annual cost of a distillation column. In the in-direct DME
The dehydration reaction takes place on solid–acid catalysts production process to overcome the drawback of energy-intensive
such as ␥-alumina, alumina modified with silica, phosphorus, related to distillation columns, using the advanced process inten-
Al2 O3 –B2 O3 and zeolites materials such as chabazite, mordenite, sification and integration techniques such as thermally coupled
SAPOs, HZSM-5 and H-Y in the temperature ranging from 250 to distillation columns, dividing-wall columns (DWC), and heat-
integrated distillation columns can be proposed [7]. A DWC is an
integration of two simple thermally coupled distillation columns
∗ Corresponding author. Tel.: +98 21 88912525; fax: +98 21 88912525. into one column by providing a vertical wall, dividing the core in
E-mail address: [email protected] (Y. Tavan). two parts, which work as the pre- or post-fractionator and the main

0255-2701/$ – see front matter © 2013 Elsevier B.V. All rights reserved.
http://dx.doi.org/10.1016/j.cep.2013.08.006
152 Y. Tavan, S.H. Hosseini / Chemical Engineering and Processing 73 (2013) 151–157

column. By process integration, the feed components can be dis- Table 1

The NRTL-RK binary interaction parameters of the system (Aij (cal/mol)).
tilled and separated with a small amount of utilities consumption
[7,8]. The main advantage of a DWC is its possibility in saving both Component Water Methanol DME
energy and capital costs [7–23]. The theoretical studies have shown Water – −357.83 74.56
that DWCs save at least 30% of energy costs compared to the con- Methanol 572.74 – 743.99
ventional schemes [7–9]. Notably, the capital cost savings result DME 86.95 −268.06 –
from reduction in quantity of equipments (i.e. number of columns,
reboilers, condensers, etc.).
To improve energy efficiency and reduce capital cost of the 2. Simulation of conventional DME production unit
DME purification process, some efforts have been carried out by
using DWC technology [8,24]. For example, Kiss and Suszwalak [8] In order to perform conceptual design of separation process in
showed that a reactive DWC leads to the significant energy sav- the DME production unit, the residue curve and ternary diagram of
ings for liquid phase DME production unit. In addition, Minh et al. water/methanol/DME are useful to elucidate the distillation part.
[24] used a DWC for a direct method DME synthesis and confirmed Fig. 1 shows the residue curve map and ternary diagram of the
the advantage of using DWC in terms of energy saving. It should DME–methanol–water mixture at the pressure of 10 bar using the
be noted that DME is traditionally produced by the vapor phase binary interaction parameters presented in Table 1. From Fig. 1, it
methanol dehydration reaction at industrial scale. Hence, indus- is clear that azeotrope point does not exist in the present system
trial aspect of DME process has been overlooked in the mentioned and distillation process is a kind of normal process. In this study
works [8,24]. More recently, Kiss and Ignat [25] studied vapor phase based on the previous results [6], a combination of fixed-bed reac-
DME production and observed 28% reduction in operating costs of tor and HZSM-5 as the proper catalyst is considered for simulation
the process using DWC with the partition wall located in the middle of conventional vapor phase DME production unit. A system con-
of the column at 10 bar pressure. taining two heat exchangers, a fixed-bed reactor, and two serial
In our previous work [6], a comparison between performance of distillation columns is simulated by Hysys. In order to represent
␥-alumina (Engelhard Company) and HZSM-5 (SiO2 /Al2 O3 = 67.6, the phase equilibrium of the system accurately, the selection of an
Zeochem AG Company) catalysts which characterized by NH3 - appropriate thermodynamic model is essential. As can be seen in
TPD and BET surface area tests, was carried out and a proper Fig. 1, a small liquid phase split envelope is observed for the system
rate equation for industrial conditions of methanol dehydration at 10 bar pressure, thus, vapor–liquid–liquid equilibrium (VLLE) is
process over the best catalyst (HZSM-5) was proposed. In the chosen for the current system. The NRTL-RK property model, which
current contribution, the derived rate equation of HZSM-5 is imple- uses the RK equation as the vapor phase model and NRTL (non-
mented into Hysys process software and subsequently simulation random-two-liquid) activity coefficient model for the liquid phase
of vapor phase methanol dehydration unit is carried out. Based is implemented into Hysys. The flowchart of conventional process
on the authors’ knowledge a few researches are available in the of the system is depicted in Fig. 2.
literature on the cost analysis and economic model development The reaction takes place in the reactor and the derived rate equa-
for DME production. Accordingly, in the present study an eco- tion of HZSM-5 is used for prediction of reaction behavior [6]. DME
nomic model is developed for conventional vapor phase DME is separated from the other components as distillate in the first
production unit. In order to reduce the energy requirements and tower, which operates at 10 bar pressure due to the low boiling
number of columns in the sequence distillation columns of DME point of DME. The bottom product, stream w, is then throttled to
synthesis unit (conventional process), the possibility of utiliz- 1 bar and sent to the second tower, where the methanol and water
ing the top-wall DWC is examined by Hysys and the interesting are separated. Two serial columns include 10 and 19 stages, respec-
results are compared to that of the conventional scheme. There- tively. The run specifications for the first column in terms of DME
fore, the main advantages of the present study can be listed as purity and condenser temperature in the top stream are 99.9% and
follows 45 ◦ C, respectively. Furthermore, the run specifications for the sec-
ond column in terms of reflux ratio and methanol purity in the top
stream are 1.2 reflux minimum and more than 99%, respectively. It
(1) In this study, the DWC process is designed and optimized by is worthwhile to mention that that the base process is optimized by
incorporating our previous kinetic model related to HZSM-5 the sequential quadratic programming (SQP) method and the input
catalyst into the fixed bed reactor, which locates before the data and simulation results are illustrated in Table 2 and Fig. 3.
DWC [6]. It is noteworthy that the DME process is a known chemical sys-
(2) A new configuration of DWC for vapor phase DME produc- tem to exhibit the non-linear behavior since the recycling of the
tion is proposed. The top-wall DWC that usually called a split recovered methanol is included. Therefore, special consideration
shell column with divided overhead and common bottom sec- should be given to design of this situation and more details about
tions is used in the simulation. The new scheme consists of two this behavior can be found in the literature [26].
condensers, only a reboiler and a main column which divided
into two parts. Although, this novel process has an additional
condenser compared to the mid-wall DWC [25], higher energy 2.1. Cost estimation of vapor phase methanol dehydration
saving is achieved for this novel process.
(3) Though, most of the previous works used a single operating To make a fair evaluation, the equipment costs of the system are
pressure for the DWCs, the present work considers pressure estimated using the procedures proposed by Douglas and the other
drop for the DWC system using the tray rating method of Hysys researchers [27–31].
process software.
(4) All equipments are conceptually designed in details. After 2.1.1. Equipment cost
short-cut simulation of the columns, the rigorous simulation For the conventional distillation column the diameter (D) and
of distillation columns is also carried out with the aid of opti- the height (Ht ) are calculated as follows
mization method to ensure reliability of the results and detailed
 T
0.25
design of the system. Consequently, maximum energy saving is 0.5
D = 0.01735 × MW × VNT (2)
obtained in this study. P
 Y. Tavan, S.H. Hosseini / Chemical Engineering and Processing 73 (2013) 151–157 153

Fig. 1. Residue curve map and ternary diagram of the mixture DME–methanol–water at 10 bar pressure.

where MW is molecular weight of a mixture (g/mol), T is tempera- where Qreb (W) is the reboiler duty, Ureb is the overall heat-transfer
ture (K), P is pressure (kPa) and VNT is maximum vapor flow rate in coefficient and the temperature driving force T (K) in the reboiler
distillation column (mol/s). depends on the operating condition of steam. The heat transfer area
for the condensers is calculated by
Nt × 2 × 1.2
Ht = (3)
3.281
Qcon
where Nt stands for the total number of stages. The heat transfer Scon (m2 ) = (5)
(Ucon × Tcon )
area for the reboilers is calculated by
Qreb where Qcon (W) is the condenser duty, Ucon is the overall heat-
Sreb (m2 ) = (4)
Ureb × Treb transfer coefficient and the log-mean temperature driving force

Fig. 2. Flowsheet of the conventional DME production process.

154 Y. Tavan, S.H. Hosseini / Chemical Engineering and Processing 73 (2013) 151–157

Table 2
The results of conventional vapor phase DME production and equipments costs.

Property Stream

Feed DME Methanol Water Return W

Temperature (◦ C) 140 45 64.15 106 64 156

Pressure (kPa) 1000 1000 120 120 1000 1050
Flow rate (mol/s) 2.50 1.25 0.49 1.25 0.49 1.74
Composition (mol%)
Methanol 99 0 99.15 0.45 99.15 28.22
Water 1 0.02 0.85 99.55 0.85 71.78
DME 0 99.98 0 0 0 0

Property Equipment

DME recovery Water/methanol separator Reactor

Diameter (m) 1.53 2.59 –

Length (m) 7.3 13 –
Total trays 10 19 –
Condenser duty (kJ/h) 2,143,683 184,006 –
Reboiler duty (kJ/h) 1,799,337 145,132 –
Reflux ratio 3 1.96 –
Minimum volume (m3 ) – – 9
Feed inlet temperature (◦ C) 150 80 220
Feed inlet stage 3 17 –
Solving method Modified Hysim inside-out –
Equipment type Ordinary column Gibbs
Operating pressure (kPa) 1000 120 1000

Tcond (K) depends on the dew and bubble points for a total con- where FC = Fm × Fp = 3.67 × 1
denser.
M&S
Tray cost ($) = (4.7D1.55 Ht FC ) (7)
M&S 280
Column cost ($) = (101.9D1.066 Ht 0.802 (2.18 + FC )) (6) where FC = Fs + Ft + Fm = 1 + 1.8 + 1.7
280
M & S 0.65
Heat exchanger cost ($) = (S (2.29 + FC )) (8)
280
where FC = (Fd + Fp ) × Fm = (1.35 + 0) × 3.75 for the reboiler,
FC = (Fd + Fp ) × Fm = (1 + 0) × 3.75 for the condenser and M & S
which is 1609.
The minimum volume of the reactor (9 m3 ) is determined based
on the optimum temperature progression chart [32]. Due to corro-
sivity of methanol, stainless steel material is chosen and the cost of
reactor is found to be 38,400$ using the online site [33].
Capital investment = column cost + tray cost

+ total heat exchanger cost + reactor cost (9)

2.1.2. Operating cost

From the reboiler duties and the heat of steam vaporiza-
tion (2148 kJ/kg) and by considering the price of low pressure
steam of 9 $/tone, the annual steam consumption costs is equal
to $157,436.49. Furthermore, the condensers are considered as
air-cooler and the price of electricity as well as the annual elec-
tricity consumption costs are accounted for by 6 cents/kWh and
$126,963.9, respectively.

2.1.3. Catalyst cost

Catalyst cost = Catalyst loading [kg] × 25 $/kg (10)
By considering a year for the catalyst life, the catalyst cost of
$50,000 is used for the total cost calculations. The results of cost
estimation are presented in Fig. 4a. It is revealed that the cost of
distillations, reactor and heat exchangers are 61.2, 29.5, and 9.3%
of the total investment cost, respectively. It can be found that capital
investment of methanol dehydration for producing DME is greatly
influenced by the distillation costs. In addition, Fig. 4b provides a
Fig. 3. Component composition profile in the conventional DME production unit for head-to-head comparison of the key performance economic indi-
(a) the first column and (b) the second column. cators. It is seen that besides the equipments, operating cost has a
 Y. Tavan, S.H. Hosseini / Chemical Engineering and Processing 73 (2013) 151–157 155

DWC and reactive DWC. More recently, the reactive DWC and CD
techniques for the DME synthesis are studied by Kiss and Suszwalak
[8] and Lei et al. [34], respectively. Hence, in the current research,
top-wall DWC utilization is evaluated by Hysys process simula-
tion software to reduce the energy requirements and number of
equipments in a novel DME process.

3. Simulation of the DWC–DME unit

A flow diagram of DWC, shown in Fig. 5, comprises two con-

densers, a reboiler and a main column, which is divided into two
parts including sieve trays. Such configuration for a DWC has
been described previously by the researchers [7,9]. It should be
noted that the dividing wall is frequently constructed entirely of
a metallic material or with the corrosion-resistant metallic mate-
rials (chromium-nickel-containing stainless steels). On the other
hand, the dividing wall can be constructed entirely of plastic (for
example poly-tetrafluoroethylene) [35].
In the DWC system, the water is separated as a single bot-
tom product, while two distillate products (DME and methanol)
are collected from each side of the main column. Since there
is no off-the-shelf DWC unit in the current commercial process
simulators, two coupled columns are used in Hysys, as the ther-
modynamically equivalent of the DWC. The stages number of 6 and
16 are accounted for the first and second columns, namely, the pre-
fractionator (PF) and the main column (MC), based on decomposing
of DWC into shortcut columns, respectively. Also, tray rating fea-
Fig. 4. Cost distribution of vapor phase methanol dehydration in terms of (a) equip-
ture of Hysys is used to calculate pressure drop in the column while
ments costs and (b) total annual costs. both the PF and MC columns operate at 10 bar pressure. Since the
PF has two degrees of freedom, therefore, for easier convergence of
the solution, the condenser temperature of 45 ◦ C and DME purity
major impact on the total investment cost for the vapor phase DME of 99.99% in the distillate stream are used as the input param-
production unit. Consequently, finding a solution to overcome the eters. High purities of methanol and water (about 99.9%) in the
drawback of distillation costs and extensive operating costs via the product streams are also used to run the MC. Notice that the steps
process intensification tools seems to be necessary. The available involved in the design and implementation of a DWC is similar to a
alternatives to reduce these costs can be catalytic distillation (CD), conventional column and more details about DWC simulation can

Fig. 5. Configuration of the DME production process via the DWC technique.
156 Y. Tavan, S.H. Hosseini / Chemical Engineering and Processing 73 (2013) 151–157

Fig. 6. The convergence of the SQP method for the DWC–DME unit.
Fig. 7. Component composition profile of the DWC–DME unit.

be found in Premkumar et al. work [10]. In order to optimize the duty of the DWC–DME system is significantly lower than the cor-
DWC system, it is assumed that energy optimization of a DWC with responding term in the conventional DME process. It is calculated
fixed number of trays is equivalent to the energy minimization of that the DWC–DME process leads to 44.53% reduction in operat-
the whole DWC process due to this fact that the energy require- ing costs, compared to the classic DME production unit. This saving
ment strongly depends on the interconnecting liquid and vapor is in a fair agreement with the researchers findings for the DWCs
flows [11]; therefore, it is very important to find the optimal val- schemes [9–15,25]. Fig. 7 shows the composition profiles in both
ues for thus flows to minimize the energy requirements and make sides of the wall. As can be seen in the figure, high purity products
a fair comparison. Moreover, it should be stated that location of are obtained in the DWC configuration. In the MC column, it is seen
side streams and number of stages have only a minor effect on the that the concentrations of methanol and water oppositely increase
system and these effects are then neglected [7–19]. Hence, design along the column that the same trend was observed in the sequence
results after optimization of the interconnecting liquid and vapor columns as shown in Fig. 3. It has been reported that the Petlyuk
flows leads to an optimal design. column is generally more efficient than the other thermally cou-
In this regards, for the search of the minimum energy pled schemes [17–19]. It is noteworthy that a DWC is practically
requirements of the whole DWC–DME unit, the method of SQP identical to a Petlyuk column, if the heat transfer across the col-
implemented as a part of Hysys is used. The target is minimization umn wall is neglected or the wall is insulated. In this study, Fig. 8
of energy demand using the interconnecting flows as search vari- shows the temperature difference between both sides of the wall
ables and by assuming the pure DME at the top of the column as and indicates that this difference is less than 20 ◦ C. Therefore, it can
constrain. During this method, the number of trays remains con- be assumed that there is no heat transfer between both sides of the
stant. Fig. 6 shows how the SQP method reaches to the minimum wall and the modeled system is thermodynamically equivalent to
value (658 kW) for total required duty of the DWC–DME unit. The the Petlyuk column. As a result, the use of a DWC in DME process
simulation results of the optimized DWC system are presented in leads to significant reduction in operating and equipment costs and
Table 3. From Tables 2 and 3, it is found that the required heat it can be a suitable choice for this process in industrial scale.

Table 3
The results of vapor phase DME production in the DWC process.

Property Stream

Feed DME Water Methanol

Temperature (◦ C) 140 45.98 106 52.52

Pressure (kPa) 1000 1000 1100 1000
Flow rate (mol/s) 2.50 1.25 1.25 0.86
Composition (mol%)
Methanol 99 0.02 0.98 99.01
Water 1 0. 99.02 0.99
DME 0 99.98 0 0

Property Equipment

PF MC Flow

Total trays 6 16 –
Condenser duty (kJ/h) 374,414 187,460 –
Reboiler duty (kJ/h) – 1,807,757 –
Operating pressure (kPa) 1000 1000 –
Reflux ratio 4.46 0.75 –
Interconnection liquid flow – – 0.85
Interconnection vapor flow – – 1.48
Solving method Modified Hysim inside-out –
Equipment type Refluxed absorber Ordinary column –
 Y. Tavan, S.H. Hosseini / Chemical Engineering and Processing 73 (2013) 151–157 157

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