STATE OF LIBYA

Sabratha University
Faculty of Engineering - Sabratha
Chemical Engineering Department

Process Design and Analysis of Dimethyl Ether

Production Plant

The Thesis was submitted in partial fulfillment of the requirement

for the Bachelor of science in chemical engineering

By
Mohammed Saeed Al-Suwaie.
Moad Ahmed Aoun

Supervised by
Prof.Dr. Omar Ahmed Al-geidi

Spring 2022
 ‫ى‬
‫إهداء‬
‫المصطف عليه أفضل صالة‬ ‫الحمد هلل والصالة والسالم عىل الحبيب‬
‫وسالم أما بعد‪:‬‬

‫مسيتنا الدراسية ى يف‬ ‫ى‬

‫الحمد هلل الذي وفقنا للوصول لهذه الخطوة يف ر‬
‫َّ‬
‫المرحلة الجامعية إىل نهايتها بعد تعب ومشقة‪.‬‬
‫ىُّ‬
‫ممتني لكل من كان له‬ ‫همة ونشاط‪،‬‬‫تخرجنا بكل َّ‬
‫وها نحن نختم بحث ُّ‬
‫ر‬
‫ى‬
‫المستني لمن كان معنا‬
‫ر‬ ‫السية العطرة‪ ،‬والفكر‬
‫مسيتنا‪ ،‬ألصحاب ر‬
‫فضل يف ر‬
‫باليسي‪.‬‬
‫ر‬ ‫وساعدنا ولو‬

‫العاىل (والدينا األحبة)‪ ،‬أطال هللا‬

‫ي‬ ‫األول ى يف بلوغنا التعليم‬
‫لمن كان له الفضل َّ‬

‫ى يف ُعمرهم ورحم من فارقنا‪.‬‬

‫إىل من وضعتننا عىل طريق الحياة إىل من وضع الموىل ‪ -‬سبحانه وتعاىل ‪-‬‬
‫َّ‬
‫الجنة تحت قدميها‪ ،‬و وقرها ى يف كتابه العزيز (أمهاتنا الحبيبات)‪.‬‬

‫كثي من العقبات والصعاب‪.‬‬ ‫ى‬

‫إىل إخوتنا؛ من كان لهم بالغ األثر يف ر‬
‫ى‬
‫صياتة؛ ممن لم يتوانوا‬‫إىل جميع أساتذتنا الكرام يف كلية الهندسة بجامعة ر‬
‫ى يف مد يد العون‪.‬‬
‫ر‬ ‫ُّ‬
‫ونحيمهم‪.‬‬ ‫إىل كل األصدقاء والمعارف الذين نجلهم‬

‫نهدي لكم بحثنا‬

 ‫الشكر والتقدير‬
‫األخية ى يف الحياة الجامعية من وقفة نعود‬
‫ر‬ ‫ال بد لنا ونحن نخطو خطواتنا‬

‫إىل أعوام قضيناها ى يف رحاب الجامعة مع أساتذتنا الكرام الذين قدموا لنا‬

‫كبية ى يف بناء جيل الغد‪.‬‬ ‫الكثي ر ى‬

‫باذلي جهود ر‬ ‫ر‬

‫نقدم أسىم آيات الشكر واالمتنان والتقدير والمحبة إىل الذين حملوا أقدس‬

‫رسالة ى يف الحياة إىل الذين أناروا لنا طريق العلم والمعرفة إىل جميع أساتذتنا‬

‫صياتة‪.‬‬
‫األفاضل بكلية الهندسة بجامعة ر‬

‫نتوجه بالشكر الجزيل إىل الذين تفضلوا ر‬

‫باإلشاف عىل هذا البحث جزاهم‬

‫الخي فلهم منا كل التقدير‪.‬‬

‫هللا عنا كل ر‬
 Abstract

As the energy demand is increasing constantly, sustainable energy resources are needed
to meet this demand and enable economic stability. In order to attain this goal, researchers
continue to develop new technologies and methods in the field of sustainable energy.
Dimethyl ether (DME) is a well-known propellant and coolant, an alternative clean fuel
for diesel engines which simultaneously is capable of achieving high performance and
low emission of CO, NOx and particulates in its combustion. It can be produced from a
variety of feed-stocks such as natural gas, coal or biomass; and also can be processed into
valuable co-products such as hydrogen as a sustainable future energy. The Aim of this
research work was a feasibility study to produce 50,000 metric tons of 99.5 wt% dimethyl
ether (DME) per year via the catalytic dehydration of methanol over an 𝛾 - Al2O3 catalyst.
Aspen HYSYS process simulation software version 11 was used to model the process
including both, synthesis section and separation section, in which a material and energy
balance were made for the entire process to estimate the operating condition, stream
composition and energy consumption. Heterogeneous catalyst was used to model the
reactor kinetically, where the effect of some key operating parameters on the reactor
performance was investigated. The results show that the optimum operating temperature
and pressure are 300 oC and 1500 kPa respectively, at which the maximum conversion is
achieved. For the separation and purification section a two distillation columns are
required, where the first once contains 12 sieve tray and total condenser to separate the
DME, while the second column contains 14 sieve tray with a total condenser to separate
the unreacted methanol which recycled back to the reactor. Moreover, hydraulic analysis
of the distillation columns was performed to size the column internals that ensure a
smooth operation. Project evaluation was performed including, design and cost estimation
of each equipment in the plant, where the result show that the total capital cost is about
5,910,210 USD and operating cost is around 4,614,130 USD/Year. Furthermore, the
selection of plant location and plant layout were considered.

I
 Table of Content
Abstract I
Table of content II
List of Tables IV
List of Figures VI
CHAPTER ONE
1. Introduction 1
CHAPTER TWO
2.1 Properties of dimethyl ether 3
2.2 Dimethyl ether market 3
2.3 Dimethyl ether as an Alternative Fuel Candidate 4
CHAPTER THREE
3.1 Methodology 6
3.2 Dimethyl ether production 7
3.2.1 Direct process 8
3.2.2 Indirect process 9
3.3 Comparison and selection of production methods 9
3.4 Indirect process description 10
3.5 Reactor performance 12
3.5.1 Catalyst type and selection 12
3.5.2 Operating Condition 12
CHAPTER FOUR
4.1 Preliminary design data 13
4.2 Process modeling and simulation setup 15
4.3 Material balance around unit operations 17
4.4 Energy balance around unit operations 19
4.5 Sensitivity analysis 24
CHAPTER FIVE
5.1 Introduction 26
5.1.1 Hand calculation and design of selected equipment 26
5.2 Process design and cost estimation 31
5.2.1 Evaluation methodology 31
5.2.2 Equipment mapping and sizing 32
II
5.2.3 Cost estimation 34
5.2.4 Hydraulic analysis of distillation column 35
5.3 Hazard and operability study (HazOp) 38
5.3.1 HazOp analysis on the reactor 38
5.4 Plant location and layout 41
5.4.1 Plant location and site selection 41
5.4.2 Plant layout 43
CHAPTER SIX
5.1 Conclusion 45
5.2 Recommendation 46
References

III
 List of Tables
Table (2.1): Physical properties of DME and other fuels 3
Table (3.1): Equipment description 11
Table (4.1): Specification of the main component. 13
Table (4.2): Standard specification for dimethyl ether for fuel purposes. 13
Table (4.3): Kinetic parameters of typical heterogeneous catalyst 14
Table (4.4): mass balance around mix-100 17
Table (4.5): mass balance around CSTR-100 17
Table (4.6): mass around CSTR-100 18
Table (4.7): mas balance around T-100 18
Table (4.8): mass balance around T-101 19
Table (4.9): Energy balance around P-100 19
Table (4.10): Energy balance around Mix-100 19
Table (4.11): Energy balance around E-100 20
Table (4.12): Energy balance around CSTR-100 20
Table (4.13): Energy balance around E-101 21
Table (4.14): Energy balance around VLV-101 21
Table (4.15): Energy balance around T-100 22
Table (4.16): Energy balance around VLV-102 22
Table (4.17): Energy balance around T-101 23
Table (4.18): Energy balance around P-101 23
Table (5.1): Input data for column design 26
Table (5.2): component properties 26
Table (5.4):Antoin constants for bubble temperature calculation 27
Table (5.5): Calculated feed specification 27
Table (5.6): Calculation of heat required to vaporize one mole of feed 28
Table (5.7): VLE data 28
Table (5.8): Shown the assumptions of the equipments 31
Table (5.9): Shown the assumptions to estimate the NPC 32
Table (5.10):Result of pump sizing 32
Table (5.11):Result of reactor sizing 32
Table (5.12): Result of Heat exchanger sizing 33

IV
Table (5.13): Result of distillation column sizing 33
Table (5.14): Result of vessel column sizing 33
Table (5.15): Result of reboiler sizing 34
Table (5.16): Result of individual equipment cost 34
Table (5.17): Result of utility cost 35
Table (5.18): Result of hydraulic analysis for column T-100 35
Table (5.19): Result of hydraulic analysis for column T-101 36
Table (5.20): Guide Word [26] 38
Table (5.21): Hazop Study on Reactor [27] 39

V
 List of Figures
Figure (2.1): The growth of the global DME capacity between 1993 and 2012 4
Figure (2.3): CO and NOx emissions for engine fueled with diesel, GTL and DME 5
Figure (3.1): Research methodology 6
Figure (3.2): Dimethyl ether production diagram 7
Figure (3.3): Direct synthesis route 8
Figure (3.4): Simplified block diagram of the indirect dimethyl ether production 9
Figure (3.5): Process flow diagram of indirect synthesis process of DME 10
Production
Figure (3.6): Conversion of Methanol using ɣ-alumina catalyst at different 12
temperatures
Figure (4.1) Show the HYSYS simulation of the process 16
Figure (4.2): Effect of reactor temperature on methanol conversion 24
Figure (4.3): Effect of reactor pressure on methanol conversion 25
Figure (4.4): Effect of reactor pressure reactor temperatur 25
Figure (5.1): Describe the project evaluation methodology 31
Figure (5.2): Hydraulic plot for column T-100 37
Figure (5.3): Hydraulic plot for column T-101 37
Figure (5.4): Show the selected location on the google earth map 42
Figure (5.5): Show the plant location in Sirt complex 42
Figure (5.6): Plant layout 44

VI
CHAPTER ONE
INTRODUCTIO
1. Introduction

Energy is a basic human need that continues to increase in line with the level of life. Oil
fuel or fossil energy is one of the non-renewable energy sources that has been the
[1]
mainstay of meeting energy needs in all activity sectors . Currently, petroleum is still
the primary energy source to meet the needs of people in Libya. The increase in
consumption of fossil-based energy, especially LPG (Liquid Petroleum Gas), which is
not balanced with the availability of energy reserves, demands the development of other
abundant and environmentally friendly alternative energy. Dimethyl ether (DME)
production has drawn increasing attention as a promising and clean and environmentally
sustainable alternative to diesel fuel, owing to its high cetane number, low auto ignition
temperature, and low emission of pollutants. Dimethyl ether is a simple ether compound
produced from various raw material sources such as natural gas, coal, and biomass. DME
has properties close to that of LPG, such as viscosity, boiling point, and pressure [2]. DME
can not only be used in industry and transportation as well as power generation as a
substitute for diesel oil, but also possesses the opportunity to replace LPG as a fuel in the
[3]
household, commercial, and industrial sectors . Dimethyl ether is classified as an
alternative material that can be renewed and used for diesel engines, diesel fuel, gas stoves
fuel as a multi-source and multi-use household fuel [4]. In general, the DME production
process can be carried out in two stages: methanol synthesis from the conversion of
biomass or the reaction of carbon monoxide or carbon dioxide gas with hydrogen, then
followed by the methanol dehydration process to produce DME and water molecules [3].
Zeolite is one type of catalyst that is commonly used in the DME manufacturing process.
The properties of the zeolite-based catalyst can be improved through dealumination and
[5]
calcination processes . Dealumination is the most common method for increasing the
SiO2/Al2O3 ratio resulting in mesoporosity in zeolites with high Si/Al ratios, to the newly
created porosity produced by preferential extraction of the Si frame due to hydrolysis in
[6]
the presence of OH- ions . Zeolite Y has an acidity comparable to amorphous silica-
[7]
alumina supports, so it has similar selectivity . Calcination is a way to remove water
content or organic molecules by heating to activate the material, creating pore structures
from the available structures [8]. Several researchers have studied on the reaction kinetics
model of the DME synthesis, studied the kinetics of the synthesis process of methanol
and DME with a commercial CuO / ZnO / Al2O3 catalyst (in the methanol formation) and

1
γ-alumina catalyst (in the dehydration process). They used the Van den Bussche and
Froment kinetics models for methanol + DME synthesis and the Bercic and Levec
[9,10]
kinetics models for methanol dehydration . Another study investigates the intrinsic
kinetics of the synthesis of dimethyl ether from syngas in a bifunctional catalyst mixed
with methanol synthesis catalyst and methanol dehydration catalyst with a mass ratio of
1:1 in a tubular integral reactor at 3-7 MPa and 220-260 oC [11]. Three reactions including
methanol synthesis from CO and H2, CO2 and H2, and methanol dehydration were
selected as independent reactions. Meanwhile, Ortega et al. (2018) explored the intrinsic
kinetics of the conversion of methanol to dimethyl ether using the ZSM-5 catalyst [9]. The
kinetic test was carried out in a fixed bed external recycling reactor, without temperature
and concentration gradient. Kinetics studies on converting methanol to dimethyl ether
using a dealuminated zeolite Y catalyst have not been found in previous studies.
Therefore, the aim of this work is to design a process capable to produce dimethyl ether
DME with a high purity (> 95 wt%). The plant is capable of producing 50,000 metric tons
of DME per year via the catalytic dehydration of methanol over an acid zeolite catalyst.
The goal is to design a grass-roots facility, which safely and efficiently produces DME.

2
CHAPTER TWO
PROPERTIES AND USES
2.1 Properties of dimethyl ether

Dimethyl ether is the simplest Ether, non-toxic and non-carcinogenic. It has no C-C bonds
and it has high H/C ratio. DME has similar physical characteristic with LPG and this
enables to store and deliver DME by using existing infrastructures with minor
modifications. Thus, DME is considered to be substitute with LPG for cooking and
heating purposes, but also as an aerosol propellant in spray cans. Also, DME is considered
as an alternative to diesel fuel due to its high cetane number and it generates lower NOx
emissions than the combustion of diesel. For these reasons, DME has high industrial
interest. It can be produced from different kinds of sources such as natural gas, crude oil,
residual oil, coal, waste products and bio-mass [2-3].

Table (2.1): Physical properties of DME and other fuels [4].

Properties DME Methanol Propane Methane Diesel fuel
Boiling point (K) 247.9 337.6 231 111.5 180 - 370
Liquid density (G/CM^3) 0.67 0.79 0.49 - 0.84
Heat of Vaporization (kJ/kg) 467 1097 426 510 -
Vapor pressure (atm) 6.1 - 9.3 - -
Cetane Number 55 - 60 5 5 0 40 - 55
Net calorifec value (10E6 J/Nm^3) 59.44 - 91.25 36 -

It can be seen physical properties of DME in Table (2.1). The vapor pressure of DME is
6.1 atm at 293 K, so it can easily liquefied by small amount of pressure. When compare
DME to propane, the DME and propane show similar physical properties. This feature of
DME enables it to be used in LPG as a blend. The calorific value of DME is higher than
Methanol and Methane. Ratios are 1.37 and 1.65, relatively. DME burns like a natural
gas. Decomposition of DME into the troposphere does not cause greenhouse effect and
ozone layer depletion [4].

2.2 Dimethyl ether market

Although DME has the promising future, its production and using amount is relatively
low in the world. On the other hand, the production capacity of DME had shown
significant improvement between 1993 and 2012 Figure (2.1). The capacity increased
from 20,000 metric tons to 11,317,000 metric tons in 20 years. The worldwide production

3
of DME is approximately 5 million tons per annum and it is estimated that the capacity
is more than 11.3 million tons globally. Asia has the biggest potential of DME market.
The studies and investments have been showing increment constantly in this region. The
majority of current DME is being produced in China, Japan, Korea and Brazil. Also, there
are new candidates to raise capacity and production such as Egypt, India, Indonesia, Iran
and Uzbekistan. In China, the annual capacity and production has increased 96% and 97%
between 2002 and 2006, respectively. Moreover, China has the plan of 20 million tons of
DME production capacity by 2020 [5, 6].

Approximately, 10,000 tons per year of DME is produced in Japan. The big companies
(JFE, Mitsubishi, Mitsui) in Japan have a plan to reach the production of 2 million ton
per year DME. South Korea is continuing the studies to commercialize DME to be energy
source of the 21 century. For future progress, the expected growth of the DME market in
Asia is from 18 MMTPA to 27 MMTPA by 2030 [7].

Figure (2.1): The growth of the global DME capacity between 1993 and 2012 [8]

2.3 Dimethyl ether as an Alternative Fuel Candidate

The calorific value of DME for per kg is lower than methane and propane but it is higher
than methanol. Because of this character of DME, more quantity of DME is needed to
travel same distance in transportation compared the other conventional fuels. On the other
hand, the calorific value of DME is higher than methane.

4
In terms of safety concern, DME is safer than propane because the lower limit of
explosion of DME is higher than propane. [9]

DME is an environmentally friendly fuel due to its advantage over other fuels. The
emission of NOx and CO in DME engines is lower than gas-to-liquid (GTL) and diesel
engines. The CO emission of diesel and GTL is lower at low loads but the CO emission
of diesel and GTL shows significant increment (Figure 2.3). Conversely, the CO emission
of DME stays same level by increase of load. At the low loads, the emission of NOx
increase for all fuels by high level of loads but even DME has the lowest emission Figure
(2.4) [12].

Figure (2.3): CO and NOx emissions for engine fueled with diesel, GTL and DME [12].

5
 CHAPTER THREE
METHODOLOGY AND DESCRIPTION
3.1 Methodology
The methodology followed in this research can be described in the next consecutive
sections as shown in figure (3.1), where the Aspen HYSYS simulator, and Excel 2019
were utilized for design, analyzing, and optimize of the process performance.

Step • Bibliographic Research and Establishment of Problem Statement

1
Step • Selection of Production Technology and Deepening of Process
2
Step • Material and Energy Balance
3
Step • Preliminary Design and Sizing of Process Equipments
4
Step • Perform a Cost Estimation and Investment Analysis
5
Step • Process Simulation and Sensitivity Analysis (Aspen HYSYS)
6
Step • Hydraulic Analysis, Risk Assessement, HazOp Study
7
Step • Observations, Conclusion and Recommendation
8

Figure (3.1): Research methodology

In the first stage of the project, the problem statement is well established and understood,
where the plant section to be designed and analyzed is to produce DME with a grade of
99.5%,

In the second stage of the project, an intensive literature survey is made, in order to select
the most propriety technology for DME production, where it found that there are two
methods that can be used, which made the decision more critical. Indirect process was
selected based on the fact that, the process is considered as a commercially available
technique, and it is considered as a most developed, and economically better that the other
methods.

In the third stage of the research, mass and energy balance are performed using excel
sheet, where the calculation was done based on the information that have been taken from
patented technology in order to meet the product requirements

In the fourth stage, preliminary design and equipment sizing are performed based on the
results of the mass and energy balances. The design and sizing of all equipments were
made automatically using some commercial software such as EDR, KG tower, excel

6
sheet, where the design criterion was made to meet the commercial standards, which
would help reducing the extra costs.

In the fifth stage, Once the design is done, the data (such as equipment geometry,
configuration, type material of construction…) is used along with APEA software and
MS excel to perform a cost estimation and investment analysis.

In the sixth stage of the research, taking the advantage of the useful tools and features
available in Aspen HYSYS V11 (optimizer, case study tool) which used along with Excel,
process simulation is performed, furthermore, sensitivity analysis was performed in order
to study the effect of key parameters on the process performance.

In the seventh stage the Hydraulic analysis, risk assessment, was performed, where the
HazOp study was implemented, moreover, the plant location and layout was done.

In the eighth stage the project documentation (Results, PFD, and equipment data sheet &
sketches), and writing the final report, conclusion, and recommendations.

3.2 Dimethyl ether production

In industrial applications, the DME is produced from the syngas by means of two
different configurations [12].

● One-step process (Direct process)

● Two-steps process (Indirect process).

3.2: Dimethyl ether production diagram [12]

7
3.2.1 Direct process

In the one-step process (direct production process), DME is produced directly from the
syngas in one single reactor where a bi-functional catalyst supports both the methanol
formation and the methanol dehydration according to the following reactions [13].

Methanol formation:

CO + 2H2 ↔ CH3OH ∆𝐻 = −90.4 𝑘𝐽/𝑚𝑜𝑙

Water-gas shift:

CO + H2O ↔ CO2 + H ∆𝐻 = −41 𝑘𝐽/𝑚𝑜𝑙

Methanol dehydration:

2CH3OH ↔ CH3OCH3 + H2O ∆𝐻 = −23 𝑘𝐽/𝑚𝑜𝑙

Overall reaction:

3CO + 3H2 ↔ CH3OCH3 + CO2 ∆𝐻 = −258.3 𝑘𝐽/𝑚𝑜𝑙

Figure (3.3): Direct synthesis route [13]

8
3.2.2 Indirect process

DME has been produced from syngas in a two-step process in which methanol is produced
from syngas, purified, and then converted to DME in another reactor as shown in figure
(2.4) [14].

(3.4): Simplified block diagram of the indirect dimethyl ether production [14]

The schematic of process flow diagram is shown in Figure 2.4. The commercialized
process reaction of DME production from methanol dehydration is shown in Eq. (1)

2CH3OH ↔ CH3OCH3 + H2O ∆𝐻 = −23 𝑘𝐽/𝑚𝑜𝑙

Many investigations on the kinetics of DME synthesis by dehydration of methanol on solid-

acid catalysts have been published. The majority of them agree that the mechanism follows
either Langmuir–Hinshelwood [15] or Eley–Rideal kinetic models [16], with water and DME
both acting as reaction inhibitors [17].

3.3 Comparison and selection of production methods

Compared with the methanol dehydration process for DME synthesis, the direct process
allows for a higher CO conversion and a simple reactor design that results in much lower
DME production costs. However, the separation process for high purity DME is relatively
more complex due to the presence of unreacted syngas and produced CO2 in the one-step
synthesis process [18].

In addition, because of the water-gas shift reaction which consumes stoichiometric amount
of CO to form CO2 and hydrogen, DME synthesis directly from syngas is not much suitable
for commercialized purposes [18].

9
3.4 Indirect process description

A PFD of the process is shown in shown in Figure 2.5. The essential operations in the
process are the preheating of the raw material (nearly pure methanol), reacting methanol
to form DME, product separation, contaminant separation, and methanol separation and
recycle [19].

V-102
11

10
E-105
P-103
E-106
7

E-101
V-101
E-104

E-103
P-105

P-102

E-101
E-102
9

R-101
V-104

E-101
P-101
1

Figure (3.5): Process flow diagram of indirect synthesis process of DME Production [19].

A fresh pure methanol is fed as a liquid in Stream 1, pumped up to 15 bar and combined
with a methanol recycle stream 9, Stream 3 is then sent into heat exchanger E-102 where
it is heated to a temperature of 250°C before it is sent to a packed bed reactor, R-101, to
form DME. The reaction is slightly exothermic and the reaction products are heated to
approximately 365°C before leaving the reactor. The reactor effluent is cooled in E-102

10
and then throttled to 10 bar before entering T-101. Here, the dimethyl ether is separated
from the other components as distillate, Stream 7. The bottom product, Stream 8, is
throttled to 7 bar and sent to T-102 where the methanol and water are separated. The water
exit as bottom product Stream 10, and is sent to a waste water treatment facility. The
methanol exits as a distillate stream 11. Stream 11 is then pumped up to 15 bar and recycled
back to be mixed with fresh methanol Stream 1. Description of all equipments included in
the PFD is shown in table 3.1 [19].

Table (3.1): Equipment description

E-101 Methanol Preheater P-103 Reflux Pumps
E-102 Reactor Effluent Cooler P-105 Recycle Pump
E-103 Reboiler R-101 Packed Bed Reactor
E-104 Condenser T-101 DME Distillation Column
E-105 Reboiler T-102 Methanol Distillation Column
E-106 Condenser V-101 Reflux Drum
P-101 Feed Pumps V-102 Reflux Drum
P-102 Reflux Pumps V-104 Feed Drum

11
3.5 Reactor performance

3.5.1 Catalyst type and selection

Candidate catalysts for converting methanol to DME are 𝛾 − 𝑎𝑙𝑢𝑚𝑖𝑛𝑎, various modified
alumina (such as silica-alumina, phosphorous-alumina and fluorinated-alumina),
hierarchical ZSM-5 (zeolite) and super-acid polymer resin (such as Amberlyst 35).
Hierarchical ZSM-5 has comparatively low conversion of methanol and is therefore not
considered. Amongst the possible catalysts, the most commonly used is 𝛾 − 𝑎𝑙𝑢𝑚𝑖𝑛𝑎 due
to its low cost (~ $2/kg), thermal stability and high surface area. The conversion of
methanol with 𝛾 − 𝑎𝑙𝑢𝑚𝑖𝑛𝑎 is strongly dependent on the operating temperature as seen in
Figure (3.6). [19]

Figure (3.6): Conversion of Methanol using ɣ-alumina catalyst at different temperatures [19]

3.5.2 Operating Condition

It can be concluded from literature that, the DME production is favored at CO-rich feed,
and low H2/CO ratio [20]. Increasing pressure has no effect on DME production [21]

Applying a high temperature profile at the beginning of the one-step DME synthesis for a
higher reaction rate and then reducing the temperature gradually for increasing the
equilibrium conversion are appropriate methods for more DME production [22].

12
 CHAPTER FOUR
MATERIAL AND ENERGY BALANCE
4.1 Preliminary design data

 Feed and product characteristics

Intensive literature review was made to collect the necessary information for the
calculation including the physical, chemical, and thermodynamic data as well as the
reaction kinetics, to perform process simulation, mass and energy balance. equipment
sizing, cost and estimation. Table 3.2 show the physical properties of component involved
in the process, while table 3.3 shows the standard composition requirements of DME
Fuel.

Table (4.1): Specification of the main component. [23]

Boiling Dencity
Molecular weight ΔH
Name Formula point Kg/m3
(g/mol) (kJ/mole)
(oC)
Methanol CH3OH (g) 32.042 64.7 795.7 -238.42
DME C2H6O (g) 46.07 -24.85 670.3 -184.02
Water H2O (l) 18.015 100 998 40.656

Table (4.2): Standard specification for dimethyl ether for fuel purposes. [24]
Property Requirement
DME, mass % (min. 98.5
Methanol, mass %, max. 0.05%
Water, mass %, max. 0.03%
Methyl Formate , mass % report

 Reaction kinetics

Turton describes the use of a gas phase reaction (above 250 and below 400 °C) for
producing DME with the following data by [23]

80.48
− 𝑅𝑎𝑡𝑒 𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙 = 1.21𝑥106 𝑒 − 𝑅𝑇 ∗ 𝑃𝑚𝑒𝑡ℎ𝑎𝑛𝑜𝑙

Since the reaction is commonly done using a heterogeneous catalyst, and it has been found
that water inhibits the reaction, other forms of the reaction equation could be used and
some typical values are shown in the table 4.3, where the Catalyst 1 is a Gamma Alumina
catalyst which used for gas phase reaction at high temperature, while the Catalyst 2 is a
high acid resin catalyst which used for the liquid phase reaction at low temperature. Since

13
the production process selected based on the Turton description is a gas phase reaction at
high temperature, the catalyst 1 is selected to be used in this study. [25]

Table (4.3): Kinetic parameters of typical heterogeneous catalyst [25]

Kinetic Parameters Catalyst 1 Catalyst 2

Heat of Reaction, kJ/kgmole -11712 -11712

A forward, kgmole/m3-s 1.0626x106 1.2457x1011
E forward, kJ/kgmole 65633 98000
m Forward Reaction Order 2 0
A’ reverse, kgmole/m3-s 1.4677x107 (no reverse rxn data)
E’ reverse, kJ/kgmole 88994 limited from pure to 5mol/litre
A1 0.5366 1.565x10-3
E1, kJ/kgmole -3450 -24642.7
f1_Methanol _exp 0.5 -1
f1_H2O_exp 0 1
A2 4.50x10-2 n/a
E2, kJ/kgmole -9395 n/a
f2_H2O_exp, 1 n/a
n, Denominator Exponent 4 2
Maximum Temp, °C 400 150 (catalyst limit)
Price $4.65/lb - $5.25/lb. $15 / lb in large quantities
Bulk Density (typical), gm/cm3 0.882 0.607
3
typical density (gm/cm ) 1.47 1.504
Void Fraction 0.4 0.6
Life 9 to 12 months unknown

14
4.2 Process modeling and simulation setup

To have a comprehensive design and clear vision of the process performance, the process
has been simulated using Aspen HYSYS v.11, where the mass and energy balance has
been performed. Model is then used to perform a sensitivity analysis to investigate the
effect of key operating parameters on the plat performance.

 Component list and Fluid package

The component list was selected directly from databank which including methanol, water,
and DME.

NRTL fluid package was selected due to its high capability of modeling the high pressure
system, and it can handle any combination of polar and non-polar compounds, up to very
strong non ideality. [25]

 Reaction set
Since the reaction is commonly done using a heterogeneous catalyst, the heterogeneous
catalytic reaction attached to CSTR reactor was used to model the reaction kinetics where
the forward and reverse reactions were accounted for based on the Alumina catalyst data
shown in table 3.4.

 Simulation setup
The process flowsheet has been constructed as it is proposed by the patent, and based on
the operating conditions that have been given in the literature. Figure 3.2 show the process
flowsheet that have been simulated using Aspen HYSYS V11.

15
Figure (4.1) Show the HYSYS simulation of the process

16
4.3 Material balance around unit operations

4.3.1 Mixer ( Mix-100 )

Table (4.4): mass balance around mix-100

Name 3 18 4
Molar Flow [kgmole/h] 248.68 61.80 310.47
Mass Flow [tonne/year] 69800.00 17212.95 87012.95
Std Ideal Liq Vol Flow [m3/h] 10.01 2.46 12.48
Heat Flow [kcal/h] -14225557.1 -3474562.1 -17700119.2
Composition (mole fraction)
Methanol 1 0.982213675 0.996459752
H2O 0 1.76E-02 3.51E-03
diM-Ether 0 1.47E-04 2.92E-05

4.3.2 Reactor ( CSTR-100 )

Table (4.5): mass balance around CSTR-100

Name 5 6
Molar Flow [kgmole/h] 310.47 310.47
Mass Flow [tonne/year] 87013 87013
Heat Flow [kcal/h] -1.41E+07 -1.41E+07
Composition (mole fraction)
Methanol 1 0.20
H2O 0 0.40
diM-Ether 0 0.40

17
 Table (4.6): mass around CSTR-100
Total inflow Total reacted Total outflow
Methanol 309.37 -247.50 61.87
H2O 1.09 123.75 124.84
diM-Ether 0.01 123.75 123.76
Summation 310.4731061 0 310.4731053

4.3.3 Distillation column ( T-100 )

Table (4.7): mas balance around T-100

8 DME 10
Flow Rate (kgmole/h) 310.47 124.29 186.18
Composition (mole fraction)
Methanol 0.199 4.31E-03 0.329
H2O 0.402 0 0.671
diM-Ether 0.399 0.996 0
Summation 1 1 1

4.3.4 Distillation column ( T-101 )

18
 Table (4.8): mass balance around T-101
14 16 15
Flow Rate (kgmole/h) 186.2 62.4 123.8
Composition
Methanol 0.329 0.982 5.63E-04
H2O 0.671 0.018 0.999
diM-Ether 4.91E-05 1.47E-04 0
Summation 1 1 1

4.4 Energy balance around unit operations

4.4.1 Pump (P-100)

Table (4.9): Energy balance around P-100

Name Methanol 2
Temperature [C] 25 25.75
Pressure [kPa] 101.32 1700.23
Heat Flow [kJ/h] -5.95E+07 -5.95E+07
Energy required
QP 6.003 KW

4.4.2 Mixer (MIX-100)

Table (4.10): Energy balance around Mix-100

Name 3 18 4
Temperature [C] 26 68 34
Pressure [kPa] 1530 1530 1530
Molar Enthalpy [kJ/kgmole] -239347 -235245 -238530
Molar Entropy [kJ/kgmole-C] 70 100 77
Heat Flow [kJ/h] -5.95E+07 -1.45E+07 -7.41E+07

19
4.4.3 Heater (E-100)

Table (4.11): Energy balance around E-100

Name 4 5
Temperature [C] 34.17 250.00
Pressure [kPa] 1530.01 1500.00
Molar Enthalpy [kJ/kgmole] -238530.22 -189598.52
Molar Entropy [kJ/kgmole-C] 76.52 181.51
Heat Flow [kJ/h] -7.41E+07 -5.89E+07
Energy required
QH 1.52E+07 kJ/h

4.4.4 Reactor (CSTR-100)

Table (4.12): Energy balance around CSTR-100

Name 5 6
Temperature [C] 250 368
Pressure [kPa] 1500 1500
Molar Enthalpy [kJ/kgmole] -189598.52 -189598.52
Molar Entropy [kJ/kgmole-C] 181.51 197.42
Heat Flow [kJ/h] -5.89E+07 -5.89E+07

20
4.4.5 Cooler (E-101)

Table (4.13): Energy balance around E-101

Name 6 7
Temperature [C] 367.59 135.19
Pressure [kPa] 1500 1490
Molar Enthalpy [kJ/kgmole] -189598.52 -223578.26
Molar Entropy [kJ/kgmole-C] 197.42 133.78
Heat Flow [kJ/h] -5.89E+07 -6.94E+07
Energy required
QC 1.05E+07 kJ/h

4.4.5 Valve (VLV-101)

Table (4.14): Energy balance around VLV-101

Name 7 8
Temperature [C] 135.2 122.4
Pressure [kPa] 1490 1040
Molar Enthalpy [kJ/kgmole] -223366.7 -223366.7
Molar Entropy [kJ/kgmole-C] 134.0 132.9
Heat Flow [kJ/h] -6.93E+07 -6.93E+07

21
4.4.6 Distillation column (T-100)

Table (4.15): Energy balance around T-100

Name 8 DME 10
Temperature [C] 122.36 46.72 154.29
Pressure [kPa] 1039.59 1039.59 1039.59
Molar Enthalpy [kJ/kgmole] -223366.71 -201188.41 -257920.52
Molar Entropy [kJ/kgmole-C] 132.95 160.95 76.06
Heat Flow [kJ/h] -6.93E+07 -2.50E+07 -4.80E+07
Condenser Reboiler
Column duty (kJ/h)
7.05E+06 3.37E+06

4.4.7 Valve (VLV-102)

Table (4.16): Energy balance around VLV-102

Name 10 14
Temperature [C] 154.29 139.07
Pressure [kPa] 1040 700
Molar Enthalpy [kJ/kgmole] -257920.52 -257920.52
Molar Entropy [kJ/kgmole-C] 76.06 73.27
Heat Flow [kJ/h] -48020758 -48020758

22
4.4.8 Distillation column (T-101)

Table (4.17): Energy balance around T-101

Name 14 16 15
Temperature [C] 139.07 66.89 102.33
Pressure [kPa] 700 110.44 110.44
Molar Enthalpy [kJ/kgmole] -257920.52 -235326.03 -279011.45
Molar Entropy [kJ/kgmole-C] 73.27 77.73 24.12
Heat Flow [kJ/h] -4.80E+07 -1.47E+07 -3.45E+07
Condenser Reboiler
Column duty (kJ/h)
6.04E+06 4.83E+06

4.4.9 Pump (P-101)

Table (4.18): Energy balance around P-101

Name 16 17
Temperature [C] 66.9 67.6
Pressure [kPa] 110.4 1530.0
Molar Enthalpy [kJ/kgmole] -235326.03 -235244.95
Molar Entropy [kJ/kgmole-C] 77.73 99.63
Heat Flow [kJ/h] -14678289.5 -14673232.5
Energy requirment
QP2 1.405 KW

23
4.5 Sensitivity analysis

Once the process has been simulated, and the material and energy balance was performed
for the entire process, the sensitivity analysis was made to investigate the effect of some
key parameters such as reactor temperature and pressure on the process performance.
From figure 4.2 it can be seen clearly that by increasing the reactor temperature from 150
o
C to 300 oC has a strong effect on the conversion where it is increased rapidly from 10%
to the maximum possible value of 75%, moreover, further increase more than 300 oC will
have no significant effect.

Figure (4.2): Effect of reactor temperature on methanol conversion

Figure 4.3 shows the effect of reactor pressure on the methanol conversion, where it can
be seen clearly that the pressure increase has a positive effect on the conversion, where it
reach the maximum at around 1500 bar, where it will have increase the reactor
temperature as well until reach the operating value of 350 oC as shown in figure 4.4.

24
Figure (4.3): Effect of reactor pressure on methanol conversion

Figure (4.4): Effect of reactor pressure reactor temperatur

25
CHAPTER FIVE
PROJECT EVALUATION
5.1 Introduction
This chapter covers the equipment sizing and cost estimation of the DME production
plant. Design of all unit operations were performed using an aspen HYSYS features and
the detailed result will be shown. Moreover, design procedure and sizing calculation of a
selected equipment will be explained in details in as a sample of hand calculation.

5.1.1 Hand calculation and design of selected equipment

The selected unit to be designed is a distillation column T-101, which used to separate
the unreacted methanol from water to be recycled to the reactor. The type of column is a
tray column, where the calculation was done to determine the number of stages, optimum
feed stage, condenser & reboiler duty, minimum & actual reflux ration, and other design
specification. Microsoft Excel was used to implement the calculations faster and easier.

Step 1: Collecting the Required data

The initial data required to start the column sizing are shown in table (5.1), including the
composition of feed, distillate, and bottom products are obtained from HYSYS.

Table (5.1): Input data for column design

Condition
Feed temperature 139.1 ( oC )
Reflux ratio 1.745
Operating pressure 760 mm Hg abs
Wt fraction Mole Fraction
Feed stream
Methanol 0.329 0.2163
Water 0.671 0.7837
Distillate
Methanol 0.99 0.9823
Water 0.010 0.0177
Bottom
Methanol 0.001 0.0006
Water 0.999 0.9994

Table (5.2): component properties

Specific Heat
Density Liq viscosity at Latent Heat
Solvent BP, °C MWt (kcal/ kgmole
kg/m3 BP, CP (kcal/kg mole)
°C)
Methanol 792 64.7 32.04 3 8490.6 19.54
Water 1000 100 18 0.24 9720 18.00

26
Step 2: Calculating the feed conditions

A. Using the Antoin equation and constants in table below the bubble point
temperature of the feed is calculated as shown in table (5.4), to be 87.79 oC.
Table (5.4):Antoin constants for bubble temperature calculation

B. The other feed specifications are calculated as shown in table (5.5) including,
average specific heat, average latent heat.
Table (5.5): Calculated feed specification
Solvent Methanol Water Average property
3
Density kg/m 792 1000 931.48
BP, °C 64.7 100 794.08
M.Wt. 32.04 18 999.79
Liq viscosity at BP, CP 3 0.24 21.04
Latent Heat (kcal/kg mole) 8490.6 9720 31.79
Specific Heat (kcal/ kgmole °C) 19.54 18.00 18.01

C. heat required to vaporize one mole of feed, feed quality (q) and slop of q line are
calculated as shown in table (5.6).

27
 Table (5.6): Calculation of heat required to vaporize one mole of feed

Step 3: Calculating the minimum reflux ration and operating reflux ratio

A. First of all, the VLE data is generated for the feed mixture using the Aspen
properties software, as shown in the table (5.5). and plotted as shown in figure
bellow.
Table (5.7): VLE data

28
 B. In the graph plot feed, distillate, bottom. and q line. Connect the lines and extend
up to Y axis and calculate the intercept, where it found to be 0.473981.

C. Calculate the minimum reflux ratio required as following.

𝑥𝑑
= 0.473981
𝑅𝑚𝑖𝑛 + 1

Rmin = 1.072527

D. The operating reflux ratio is = 1.5* Rmin

R = 1.608791

E. Plot top operating line, R line

Using the operating reflux ratio calculate the operating line intercept with Y axis

𝑥𝑑
= 0.376549
𝑅+1

plot the top and bottom operating lines as shown in the figure bellow.

29
Step 3: Construct the Mccabe Thiele graph

Based on the xd, xb, xf, the number of theoretical stages and the optimum feed stage can
be found as shown in the figure bellow, where the number of theoretical stages was 15
stage, and the optimal feed stage was No. 9.

Taking the tray spacing 0.6 m

The column high is 0.6*15 = 9 m + 2 m for safety
The total high of column is 11 m

30
5.2 Process design and cost estimation
5.2.1 Evaluation methodology
Methodology of project evaluation is shown in figure 4.1, and to eliminate or at least
reduce the human and random error that can be occur due to hand calculation and manual
design, all the evaluation steps including the flow sheet conversion, equipment mapping,
design and sizing, as well as the economic evaluation are performing automatically using
a package of softwares and features that are available commercially.

Flow sheet Equipment Auto sizing of Project

converged mapping the equipment evaluation

Figure (5.1): Describe the project evaluation methodology

First step is the flow sheet conversion (material and energy balance) which is already
performed and discussed in the preceding section, second step is the equipment mapping
which means the choose of the design criteria and the assumptions that can be
implemented to simplify the design and sizing procedure, where the mapping options and
assumptions applied are shown in the table (5.8).

Table (5.8) Shown the assumptions of the equipments

Equipment Mapping option and assumption
Cooler, heater, heat
Shell & Tube heat exchanger, with TEMA type BEM
exchanger, reboiler, condenser
Distillation column Sieve tray column
Pump Centrifugal, adiabatic efficiency 75%
Reactors Agitated tank
Vessel, Separator, Pressurized vessel

Once we have the results of material and energy balance along with a mapping criterion,
an auto-design and equipment sizing is performed as a following

 Exchanger design and rating software (EDR) is used for a design of all heat
transfer equipment, including coolers, heaters, heat exchangers, reboiler and
condenser
 Vessel sizing tool is used for a design of pressurize vessels, separators and reactors
 Tray sizing tool is used for a design of the tray section and column internals for
the absorber and regeneration columns

31
Based on the results of equipment design and sizing, economic analysis and cost
estimation are performed using Aspen process economic analyzer software (APEA)
where the capital, installation, and operating costs are calculated, moreover, for more
precise and reliability, the NPC is evaluated based on the assumptions shown in table

Table (5.9): Shown the assumptions to estimate the NPC

Option Assumption
Operation life of te plant (year) 20
Length of plant startup (year) 0
Operational time per year (hours) 8766
ROR Interest factor 1.2
Cost index 1 Q 2021

5.2.2 Equipment mapping and sizing

Results of equipment mapping and sizing are shown in tables bellow

Table (5.10):Result of pump sizing

Pumps
Reflux pump Reflux pump
User tag number P-100 P-101
@T-101 @T-100
Liquid flow rate [m3/h] 12.1 9.3 42.0 47.7
Fluid head [m] 207.7 195.5 - -
Fluid specific gravity 0.8 0.7 0.7 0.6
Design gauge pressure [kPag] 1771.3 1601.1 243.4 1110.6
Design temperature [C] 121.1 121.1 121.1 121.1
Fluid viscosity [cP] 0.5 0.3 0.5 0.5
Pump efficiency [%] 75.0 75.0 75.0 75.0

Table (5.11):Result of reactor sizing

REACTOR
User tag number CSTR-100
Remarks 1 Equipment mapped from 'CSTR-100'.
Liquid volume [m3] 2.401932948
Vessel diameter [m] 0.9144
Vessel tangent to tangent height [m] 3.6576
Design gauge pressure [kPag] 1589.907776
Design temperature [C] 365.1192
Operating temperature [C] 337.3414222

32
 Table (5.12): Result of Heat exchanger sizing
Heat exchangers
Condenser Condenser
User tag number E-101 E-100
@T-101 @T-100
Number of identical items 1 1 1 1
Heat transfer area [m2] 28.65344853 126.8084309 285.4003246 128.8528693
Front end TEMA symbol B B B B
Shell TEMA symbol E E E E
Rear end TEMA symbol M M M M
Tube design gauge pressure [kPag] 1026.162213 1601.05353 415.79608 706.6507264
Tube design temperature [C] 365.1192 343.3333333 121.1111111 121.1111111
Tube operating temperature [C] 35 250 35 35
Tube outside diameter [m] 0.0254 0.0254 0.0254 0.0254
Shell design gauge pressure [kPag] 1589.907776 1033.592713 243.42108 1110.640546
Shell design temperature [C] 365.1192 343.3333333 121.1111111 121.1111111
Shell operating temperature [C] 337.3414222 315.5555556 66.99381889 47.36983778
Tube length extended [m] 6.096 6.096 6.096 6.096
Tube pitch [m] 0.03175 0.03175 0.03175 0.03175
Number of tube passes 1 1 1 1
Number of shell passes 1 1 1 1

Table (5.13): Result of distillation column sizing

Distillation column
User tag number Main Tower_@T-101 Main Tower_@T-100
Diameter Bottom section [m] 2.7432 1.3716
Bottom tangent to tangent height [m] 10.9728 12.192
Design gauge pressure Bottom [kPag] 243.42108 1110.640546
Design temperature Bottom [C] 130.20351 172.444995
Operating temperature Bottom [C] 102.4257322 144.6672172
Number of trays Bottom section 12 14
Bottom Tray type SIEVE SIEVE
Bottom Tray spacing [m] 0.6096 0.6096
Molecular Wt Overhead Prod. 31.907251 46.054961

Table (5.14): Result of vessel column sizing

Horizontal drum
User tag number Accumulator @T-101 Accumulator @T-100
Liquid volume [m3] 4.448023966 5.854711548
Vessel diameter [m] 1.2192 1.3716
Vessel tangent to tangent length [m] 3.81 3.9624
Design gauge pressure [kPag] 243.42108 1110.640546
Design temperature [C] 121.1111111 121.1111111
Operating temperature [C] 66.75672611 46.58873722

33
 Table (5.15): Result of reboiler sizing
U-tube reboiler
User tag number Reboiler_@T-101 Reboiler_@T-100
Number of identical items 1 1
Heat transfer area [m2] 117.9001991 113.3712053
Tube design gauge pressure [kPag] 760.54608 760.54608
Tube design temperature [C] 192.1111111 192.1111111
Tube operating temperature [C] 164.3333333 164.3333333
Tube outside diameter [m] 0.0254 0.0254
Shell design gauge pressure [kPag] 473.254411 1110.640546
Shell design temperature [C] 130.2082428 174.136765
Shell operating temperature [C] 102.430465 146.3589872
Tube length extended [m] 6.096 6.096

Tube pitch [m] 0.03175 0.03175

Tube pitch symbol TRIANGULAR TRIANGULAR
Number of tube passes 2 2
Duty [kJ/h] 28754537.84 5835193.682
TEMA type BKU BKU

5.2.3 Cost estimation

Results of cost estimation is shown in tables bellow, where Table (5.16) show the results
of cost estimation for individual equipment including purchase cost, installation cost and
utility cost.

Table (5.16): Result of individual equipment cost

Equipment Installed Equipment Installed Utility Cost
Name
Cost [USD] Cost [USD] Weight [LBS] Weight [LBS] [USD/HR]
MIX-100 0 0 0 0 0
VLV-102 0 0 0 0 0
P-100 17400 50900 1400 4896 0.57815
T-101 293500 932800 68790 170499 271.864651
CSTR-100 18800 162100 3600 15894 0
P-101 17300 49700 1300 4558 0.433225
VLV-101 0 0 0 0 0
T-100 201500 700600 42430 111352 57.985951
RCY-1 0 0 0 0 0
VLV-100 0 0 0 0 0
E-101 16000 142900 2600 13894 10.88604
E-100 35400 155900 7900 36224 0

Results of total utility cost is shown in table (5.17), including the electricity, cooling water, and
steam requirements.

34
 Table (5.17): Result of utility cost
Name Fluid Rate Rate Units Cost per Hour Cost Units
Electricity 126.025 KW 9.766938 USD/H
Cooling Water Water 0.324403 MMGAL/H 38.92836 USD/H
Steam @100PSI Steam 36.89962 KLB/H 300.362907 USD/H

5.2.4 Hydraulic analysis of distillation column

Hydraulic analysis of both columns were performed to ensure a smooth operation and the
summary of the results are shown in tables (5.18) and (5.19), where the results show that
both columns are working within the operating range as shown in figures (5.2) and (5.3)
without any problems.

Table (5.18): Result of hydraulic analysis for column T-100

Section
Section Starting Stage 1__Main Tower 6__Main Tower
Section Ending Stage 5__Main Tower 14__Main Tower
Tray Type Sieve Sieve
Number Of Passes 1 1
Tray Spacing [m] 0.6096 0.6096
Section Diameter [m] 1.051898639 0.814383796
Section Height [m] 3.048 5.4864
Section Pressure Drop [mbar] 28.56002103 49.08442278
Section Head Loss [mm] 473.7133719 725.178932
Trays With Weeping None None
Hole Diameter [mm] 12.7 12.7
Hole Area to Active Area 0.1 0.1
Deck Gauge Thickness 10 Gauge 10 Gauge
Deck Gauge Thickness Value [mm] 3.4036 3.4036
Cross-Sectional Area [m2] 0.8690358 0.520892529
Active Area [m2] 0.695228641 0.416714024
Net Area [m2] 0.78213222 0.468803277
Downcomer Geometry
Downcomer Clearance (mm) 38.1 38.1
Downcomer Width Top (mm) 164.596456 127.4311818
Downcomer Width Bottom (mm) 164.596456 127.4311818
Downcomer Area Top (m2) 8.69E-02 5.21E-02
Downcomer Area Bottom (m2) 8.69E-02 5.21E-02
Weir Geometry
Weir Height (mm) 50.8 50.8
Weir Length (m) 0.764321384 0.591740428

35
 Table (5.19): Result of hydraulic analysis for column T-101
Section
Section Starting Stage 1__Main Tower 7__Main Tower
Section Ending Stage 6__Main Tower 12__Main Tower
Tray Type Sieve Sieve
Number Of Passes 1 1
Tray Spacing [m] 0.75 0.75
Section Diameter [m] 2 1.567945352
Section Height [m] 4.5 4.5
Section Pressure Drop [mbar] 36.8938586 63.58933199
Section Head Loss [mm] 494.40782 696.7420694
Trays With Weeping None None
Hole Diameter [mm] 12.7 12.7
Hole Area to Active Area 0.126007813 0.1
Deck Gauge Thickness 10 Gauge 10 Gauge
Deck Gauge Thickness Value [mm] 3.4036 3.4036
Cross-Sectional Area [m2] 3.141592654 1.930864179
Active Area [m2] 2.513274127 1.544691346
Net Area [m2] 2.827433391 1.737777762
Downcomer Geometry
Downcomer Clearance (mm) 49.8 49.8
Downcomer Width Top (mm) 312.9511723 245.345168
Downcomer Width Bottom (mm) 312.9511723 245.345168
Downcomer Area Top (m2) 0.314159263 0.193086416
Downcomer Area Bottom (m2) 0.314159263 0.193086416
Weir Geometry
Weir Height (mm) 62.5 62.5
Weir Length (m) 1.4532225 1.139286732

36
Figure (5.2): Hydraulic plot for column T-100

Figure (5.3): Hydraulic plot for column T-101

37
5.3 Hazard and operability study (HazOp)

The HAZOP study is a formal procedure to identify hazards in a chemical process facility.
The procedure is effective in identifying hazards and is well accepted by the chemical
industry. The basic idea is to let the mind go free in a controlled fashion in order to
consider all the possible ways that process and operational failures can occur. Before the
HAZOP study is started, detailed information on the process must be available. This
includes up-to-date process flow diagrams (PFDs), process and instrumentation diagrams
(P&IDs), detailed equipment specifications, materials of construction, and mass and
energy balances. Table 4.20 show the guide words and their meaning for the hazop
analysis. [26]

Table (5.20): Guide Word [26]

Guide Words Meaning
No Negation of design intent
Less Quantitative decrease
More Quantitative increase
Part of Qualitative decrease
As well as Qualitative Increase
Reverse Logical opposite of the intent
Other than Complete substitution

5.3.1 HazOp analysis on the reactor

The HazOp analysis well be limited to the reactor, which is the heart of the plant, where
the reactions taking place, because it is considered as a most critical and dangerous
equipment in the plat due to the presence of all hazard materials that is reacted
exothermally. Table (5.22) show the implemented HazOp study for the reactor.

38
 Table (5.21): Hazop Study on Reactor [27]

Guide Deviation Cause Consequences Action

 No Feed in  Cleaning of
storage tank line
 Feed pump  Level control
 Decrease
rupture system
Flowrate in production or
 Supply pipe  Maintenance of
no production
rupture pipes
 Valve is closed  Automatic valve
 Pump is off  Automatic pump

No  Blockage in  Decrease in  Maintenance of

Level line production or pipes
 Valve is closed no production  Automatic valve

 Fault in Preheater  Decrease

 Maintenance
Temperature  Steam pipe in production or
of pipes
rupture no production

 Decrease in
 Fault in  Maintenance of
Pressure production or
Preheater Preheater
no production

Flowrate  Automatic valve

 More valve  Explosion
 Check reactor
opening  Less conversion
conditions

 More valve
Level  Overflow  Check Valve
opening

More
 Fault in
Temperature  Explosion  Maintenance
Preheater

 Fault in  Less
Pressure  Check valve.
Preheater production

39
  Automatic valve
Flowrate  Less of  Less
 Temperature
opening of production
control at reactor
valves
feed preparation

 Less of
 Less
Level opening of  Check Valve
Less Production
valves

 Fault in  Low  Temperature

Temperature
Preheater Conversion Control

 Fault in  Less
Pressure  Maintenance
Preheater Production

 Low
 Problem in conversion  Quality control of
As Impurities in raw material rate raw material
well as feed stream  Fouling in  Decrease in and product
pipes product  Maintenance
quality
Higher or  High quality  More or less
Lower  Quality control of
of feed pure
Part of raw material
percentage of  Less quality of production
and product
Feed feed than intended

Replacement  Wrong  Better

Other connection management of
of Raw  Explosion
than during plant changing
Material modification procedure

40
5.4 Plant location and layout

The economic construction and efficient operation of a process unit will depend upon
how well the plant and equipment specified on the process flowsheet is laid out and on
the profitability of the project with its scope for future expansion

5.4.1 Plant location and site selection

Plant location and site selection should be made before the plant layout, where it has a
crucial effect on the profitability of the project. The important factors that are to be
considered while selecting a site are: [26]

 Location, with respect to market area

 Raw material supply
 Transport facilities
 Availability of Labour
 Availability of utilities
 Availability of suitable land
 Environmental impact and effluent disposal
 Local community considerations
 Climate
 Political and strategic considerations
Based on the factors mentioned above, the best site location for the proposed
formaldehyde production plant is in the Sirt petrochemical complex, which located in
centre of Libya. Figure 4.4 show the selected location on the google earth map.

The selected location has many advantageous, such as the free space inside plant for the
future expansion, availability of raw material especially, methanol which is produces at
the plant, and the availability of utility and transport facilities. Figure 4.5 show the plant
location in Sirt complex.

41
Figure (5.4): Show the selected location on the google earth map

Figure (5.5): Show the plant location in Sirt complex

42
5.4.2 Plant layout

After considering the site selection and selecting the plant location, the plant
layout is completed, where it involves placing of equipment so that the
following are minimized: [26]

 Damage to persons and property in case of fire explosion or toxic release

 Maintenance costs
 Number of people required to operate the plant.
 Construction costs
 Cost of planned expansion.
The various units that should be laid out include

 Main processing unit

 Storage for raw materials and products
 Maintenance workshops
 Laboratories for process control
 Fire stations and other emergency services
 Utilities: steam boilers, compressed air, power generation, refrigeration
 Effluent disposal plant
 Offices for general administration
 Canteens and other amenity buildings such as medical centers
 Car parks
Plant layout was drawn as shown in figure 4.6, taking in the account the design standard,
safety consideration, and flexibility during the operation.

43
 WASTE WATER
T-101
TANK

MeOH
TANK

DME
T-100
TANK

44
Figure (5.6): Plant layout
Reactor
CSTR-100
 CHAPTER SIX
CONCLUSION AND RECOMMENDAYION
 CHAPTER FIVE CONCLUSION

6.1 Conclusion
The project was aimed to perform an integrated detailed design for the production of
DME from methanol, with a capacity of 50,000 tone/year ad purity more than 99.5wt%.

Significant research has been conducted to explore a variety of methods for DME to be
produced efficiently, where it found that the commercially proven technology for DME
production is the dehydration of pure methanol using the 𝛾 - Al2O3 which considered the
most commonly used methanol dehydration catalysts. The optimum operating condition
was found at temperature range of 200 oC – 300 oC, and pressure up to 20 bar. The
hydraulic analysis of the distillation columns was performed using specialist tool in
Aspen Hysys, in order to ensure the safe operation of the columns, where the results show
that both columns will operate within the safe operating limits without any problems.
moreover, a quick project evaluation was performed where it found that the total capital
investment is 5,910,210 USD, and the total operating cost is 4,614,130 USD/year, which
relatively high, and indicates that the process needs more development by implementation
of heat integration methodology.

45
 CHAPTER FIVE CONCLUSION

6.2 Recommendation

By the end of this research, one can propose some recommendation to be taken as a
starting point for future work as following:

1. Perform a dynamic simulation of the process to study the plant operability and
design the control strategy.
2. Implementation of heat integration to reduce the energy consumption.
3. Study the other methods for production of MDE and compare the results.
4. Using other type of catalysts and compare the result

46
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