Synthesis of Dimethyl Ether: Capstone Ii

SYNTHESIS OF DIMETHYL ETHER
Bachelor of Chemical Engineering
CAPSTONE II
SUBMITTED BY: GROUP 7
AIGERIM BAKYTZHANOVA ID 201100705
DINARA GAPEYENKO ID 201101210
RUSLAN MARTEMYANOV ID 201102238
AZAT YERKINOVA ID 201103889
SUBMITTED TO:
PROFESSOR COSTIN-SORIN BILDEA
2016
DECLARATION
I/We hereby declare that this report entitled “Synthesis of Dimethyl Ether” is the result of
my/our own project work except for quotations and citations which have been duly
acknowledged. I/We also declare that it has not been previously or concurrently submitted for
any other degree at Nazarbayev University.
Names: Signature:
Aigerim Bakytzhanova
Dinara Gapeyenko
Ruslan Martemyanov
Azat Yerkinova
Date: 22.04.2016
Table of Contents
ii
1. INTRODUCTION 2
1.1 CAPSTONE I REVIEW 2
2. MATERIAL AND ENERGY BALANCE 5

2.1 MASS BALANCE 5
2.2 ENERGY BALANCE 9
PROCESS FLOW DIAGRAM 10
3. DESIGN OF PRIMARY EQUIPMENT 12

3.1 DESIGN OF REACTOR 12
3.1.1 REACTOR KINETICS 12
3.1.2 ADIABATIC TEMPERATURE CALCULATIONS 13
3.1.3 REACTOR VOLUME CALCULATIONS 14
3.1.4 COST CALCULATIONS 16
3.1.5 OPTIMIZATION AND CONVERSION CHOICE 16
3.1.6 DESIGN SPECIFICATIONS 16
3.1.7 PRESSURE DROP CALCULATIONS 17
2.1.9 VELOCITY CALCULATIONS 18
2.1.10 REACTOR WALL THICKNESS CALCULATIONS 18
2.1.11 ENERGY BALANCE OF THE REACTOR 20
2.1.12 SUMMARY OF REACTOR SECTION 23
2.2 DESIGN OF HEAT INTEGRATION UNIT 23
2.2.1 OPTIMIZATION OF HEAT INTEGRATION UNIT 24
2.2.2 DESIGN SPECIFICATIONS OF HEAT INTEGRATION UNIT 28
2.2.3 COST ANALYSIS 33
2.3 DISTILLATION COLUMNS 35
2.3.1 METHODS OF OPTIMIZATION 38
2.3.2 COST ANALYSIS ESTIMATION 38
2.3.3 DME TOWER 39
2.4 DESIGN OF DISTILLATION COLUMN 2 49
4. DESIGN OF SECONDARY UNITS 57
5. ECONOMIC ANALYSIS 58
6. PROCESS CONTROL AND SAFETY ANALYSIS 60

7.1 FIRE AND EXPLOSION 61
7.2 TOXICITY AND STORAGE CONDITIONS 61
7.3 CORROSION 62
7.4 HAZARDS AND OPERABILITY STUDIES (HAZOP) 63
7.5 SUSTAINABILITY OF THE PLANT. 66
7.6 PROCESS CONTROL 67
7. PLANT LAYOUT 71
8. APPENDIX A 74
9. APPENDIX B 75
10. APPENDIX C 78
11. APPENDIX D 83
iii
12. APPENDIX E 87
13. REFERENCE LIST 89
LIST OF FIGURES
iv
Figure 1A. Process Flow Diagram............................................................................................11
Figure 2. Comparison of calculated temperature and real temperature versus conversion......14
Figure 3. Pressure drop versus reactor length from Ergun equation........................................18
Figure 4. Compositions of components versus reactor length..................................................20
Figure 5. The Reactor outlet Temperature versus time for 10% increase in feed....................22
Figure 6. The reactor outlet temperature versus time for 10% decrease in feed......................23
Figure 7. Original heat integration unit....................................................................................24
Figure 8. First optimized heat integration unit.........................................................................25
Figure 9. TQ-diagram of the obtained heat exchanger in first optimization............................25
Figure 10. Total cost of heat integration vs. conversion...........................................................27
Figure 11 Schematic drawing of DME optimized heat integration unit including process
control.......................................................................................................................................28
Figure 12. The first heat exchanger sketch specifications........................................................31
Figure 13. The first heat exchanger TQ-diagram.....................................................................31
Figure 14. The second heat exchanger sketch specifications...................................................32
Figure 15. The second heat exchanger TQ-diagram.................................................................32
Figure 16. The third heat exchanger sketch specifications.......................................................33
Figure 17. The third heat exchanger TQ-diagram....................................................................33
Figure 18. Sieve-plate performance diagram, (Sinnott & Towler, 2012).................................37
Figure 19. DME tower total annual cost for different conversion............................................40
Figure 20. Total Annual Cost vs. Number of Trays.................................................................41
Figure 21. Feed Tray location...................................................................................................42
Figure 22. Condenser flow diagram.........................................................................................44
Figure 23. Kettle reboiler drawing............................................................................................44
Figure 24. Temperature profile (Rate based model).................................................................46
Figure 25. Composition Profile (Rate based model)................................................................46
Figure 26. Flow-rate change by 10%.....................................................................................47
Figure 27. DME purity response after decreasing flow rate by 10%.......................................48
Figure 28. Conversion vs. TAC for the second distillated column...........................................49
Figure 29. Total annual cost vs. Number of trays for 95% efficiency conversion...................50
Figure 30. Optimal feed tray 17 for Number of trays 25..........................................................51
Figure 31. Total condenser temperatures..................................................................................52
Figure 32. Kettle reboiler temperatures....................................................................................53
Figure 33. Optimal feed tray 25 for Number of trays 36..........................................................54
Figure 34. Temperature profile of distillation column.............................................................54
Figure 35. Composition profile.................................................................................................55
Figure 36. Tray efficiency........................................................................................................55
Figure 37. Flow rate +10%.......................................................................................................67
Figure 38. Purity +10%.............................................................................................................68
Figure 39. Steam characteristic for +10%................................................................................68
Figure 40.Temperature around the reactor for +10%...............................................................69
Figure 41. Schematic plant layout............................................................................................72
Figure A 1. Centrifugal pump efficiency (Sinnott & Towler, 2011).....................................78Y
Figure C1. Tray Efficiency profile for DME distillation column.............................................80
Figure C2. DME pressure control (PC) response for 10% change...........................................80
Figure C3. DME tower drum level controller performance.....................................................81
Figure C4. Stage 14 temperature controller for DME Tower...................................................81
v
LIST OF TABLES
YTable 1. The properties of γ-Al2O3 catalyst (Dlep et al., 1987, p. 332)
vi
Table 2. The properties of 3-mm γ-Al2O3 catalyst for Bercic model (Bercic, et al., 1993)......4
Table 3. Results obtained using Matlab program in k-mol/hour for each stream and each
component...................................................................................................................................5
Table 4. Mass balance of the reactor..........................................................................................6
Table 5. Distillation Columns mass balance...............................................................................6
Table 6. Stream specifications of first heat exchanger...............................................................6
Table 7. Stream specifications of second heat exchanger..........................................................7
Table 8. Stream specifications of third heat exchanger..............................................................7
Table 9. Stream specifications of flash drum.............................................................................7
Table 10. Stream specifications of heater...................................................................................8
Table 11. Stream specifications of mixer...................................................................................8
Table 12. Energy balance for distillation columns.....................................................................9
Table 13. Energy balance of heat exchangers.............................................................................9
Table 14. Energy balance of flash drum and mixer..................................................................10
Table 15. Energy balance of heater..........................................................................................10
Table 16. Methanol consumption equilibrium constant coefficients.......................................12
Table 17. Concentration exponents table in Aspen Plus softwaare..........................................13
Table 18. Adsorption constants for term 1,2 and 3 in Aspen Software....................................13
Table 19. Theoretical Volume Estimations..............................................................................15
Table 20. Reactor Cost..............................................................................................................16
Table 21. Design specifications of the reactor..........................................................................16
Table 22 The specifications of heater and cooler in original case............................................24
Table 23 Specifications of first optimized heat integration unit...............................................25
Table 24 Cost estimation of original and first optimized case.................................................26
Table 25. Cost estimation of heat integration for different conversions..................................26
Table 26. Design specifications of heat exchangers.................................................................30
Table 27. Specifications of mixer and flash drum....................................................................30
Table 28. Cost estimation of heat exchangers and heater.........................................................34
Table 29. Cost estimation of mixer and flash drum..................................................................34
Table 30. Type of plate contactors............................................................................................36
Table 31. Basic requirements for distillation column (Sinnott & Towler, 2012).....................37
Table 32. Utility cost (Luyben, 2011).....................................................................................39
Table 33. Total annual cost of DME tower at different conversion (only optimum values)....39
Table 34. Specified component compositions for DME Tower...............................................40
Table 35. Optimum DME Tower design..................................................................................41
Table 36. Base design specification of column and tray..........................................................43
Table 37. Size for reflux drum and sump................................................................................45
Table 38. Controllers’ Specification.........................................................................................47
Table 39. Comparison of Equilibrium and Rate Based models................................................48
Table 40. Characteristics for 95% efficiency conversion.........................................................50
Table 41. Flow rates of compounds to the second distillation column.....................................51
Table 42. Base design specification of column and tray for Methanol column.......................52
Table 43. Condenser results......................................................................................................52
Table 44. Reboiler results.........................................................................................................53
Table 45. Reflux drum and sump characteristics......................................................................53
Table 46. Stream results from Methanol column.....................................................................55
Table 47. Cost comparison.......................................................................................................56
Table 48. Secondary Unit Specifications..................................................................................58
Table 49. Manufacturing Capital Cost......................................................................................58
Table 50. Working Capital, Fixed and Variable costs of Production.......................................59
vii
Table 51. Types of incidents (Crowl, 2011, p. 15)...................................................................61
Table 52. Comparison chart of properties for carbon steel and stainless steel.........................63
Table 53. Guide words used for the HAZOP Procedure (Crowl, 2011, p. 511).......................63
Table 54 HAZOP for heat exchanger.......................................................................................64
Table 55. HAZAOP study for DME reactor.............................................................................65
Table 56. HAZOP analysis for Distillation column.................................................................66
Table B57 TEMA sheet of first heat exchanger.......................................................................75
Table B58 TEMA sheet of second heat exchanger...................................................................76
Table B 59 TEMA sheet of third heat exchanger.....................................................................77
Table 60. Finding an optimal feed tray for Number of stages 25.............................................85
Table 61. Cost estimation for the column.................................................................................85
Table 62. Cost estimation for trays...........................................................................................86
Table 63. Cost estimation for condenser..................................................................................86
Table 64. Cost estimation for reboiler......................................................................................86
Table 65. Operating cost for condenser....................................................................................87
Table 66. Operating costs for reboiler......................................................................................87
Table 67. Total annual cost for the whole distillation column.................................................87
viii
NOMENCLATURE
Q – heat transferred per unit time, W

U –overall heat-transfer coefficient, W/m2K
A – heat-transfer area, m2
∆Tm – mean temperature difference, oC
cp – specific heat coefficient, kJ/kgK
λ – latent heat of vaporization, kJ/kg
Fp – pressure correction factor
Fm – material correction factor
Fd – design type correction factor
Ph - Hydraulic power of the pump, kW
Ps - Shaft power of the pump, kW
Q̇ - Volumetric flow of fluid through the pump, m3/h
ρ - Density of the fluid
g - Gravity (9.81 m/s2)
h - Head produced by the pump, m
ηp - Pump efficiency , %
kJ
c p- heat capacity by mass basis,( )
kg∗K
kJ
C p - heat capacity by molar basis, ( )
mole∗K
kg
ρ - density of stream, ( )
m3
y A 0 - initial molar fraction of component A,
kmol
F A 0 - initial molar flowrate of component A,( )
m3
X A - conversion of component A
∆ p - the pressure drop across the bed,
L - the length of the bed (not the column),
D p - the equivalent spherical diameter of the packing,
ρ - the density of fluid,
μ - the dynamic viscosity of the fluid,
v s - the superficial velocity (i.e. the velocity that the fluid would have through the empty
tube at the same volumetric flow rate), and
ϵ - the void fraction of the bed (bed porosity at any time).
2
1. Introduction
In twenty-first century, large attention is paid to alternative energy sources, as coal, oil and
gas can become scarce in several decades’ time. Biofuel, being one of alternative energy
sources, can be produced from alcohols and used widely domestically and in industry.
Dimethyl ether as a green fuel type, is non-corrosive, non-toxic, colorless gas with a chemical
formula of CH3OCH3.
China consumes about 90% of world production. It is mainly applied for cooking and
residential heating. DME will be used as a fuel for commercial and municipal transport in
Shanghai and may spread to other cities to cover 85% of China vehicles. It is proposed to be
effective method to lessen the dependence on hydrocarbon resources. (Shana, 2011)
In Europe, similar strategy is implemented by Volvo Company. Low emission trucks using
DME as fuel are tested and four Sweden plants produce DME for that purpose. Concluding,
European Volvo Group, Total from France, Chemrec and Preem from Sweden and Haldor
from Denmark are main DME producers in Europe. (Kauffman, 2014).
DME is acting as propellant in range of personal care products, as it has high water solubility.
(DuPont, 2000).
The main applications of DME are as following:
 A substitute for liquefied petroleum gas in heating and cooking purposes.
 A substitute for chlorofluorocarbon during the production of paint-aerosols cans
and cosmetics as a propellant.
 A substitute for diesel fuel. If the engine is modified to operate on DME basis, high
cetane number DME is used as a fuel.
 A precursor during the acetic acid and dimethyl sulfate synthesis.
 A refrigerant.
 A rocket propellant.
 A carrier in foggers and sprays against insects.
 A solvent during the extraction of compounds that are organic.
1.1 Capstone I Review
Market analysis
During Capstone I, main DME producers were analysed. Haldor Topsoe from Denmark is
main technology provider and currently is constructing DME plant in Iran for Zagros
3
Petrochemical (ICIS News, 2004). Another major technology provider is China Energy with
largest DME production amounts in China. The annual production reaches 900,000 metric
tons (DME China Energy, n.d.). Third company working in the field is TOYO DME
Company with indirect chemical route technology and about hundred object designed with
this basis (Toyo Engineering, n.d.).
The value of DME market approaches US$ 4.5 billion. The expected compound annual
growth rate is 9.4% (GlobeNewswire, 2015).
Current world-wire production is 4,500 kilotons per year and demand for DME is expected to
be 6,500 kilotons/year in 2018. The suggested plant capacity is expected to cover 10% of that
demand increase. The production rate of the plant is 200 kilotons/year. The comparison to
currently operating plants showed, that size is realistic.
The main factor for location choice was availability of feed. As Methanol is used as feed, the
location should be near methanol production plant to minimize transportation costs. Malasian
Government cooperates with Kazakhstan companies to construct a methanol plant in
Mangystau region and start operating in 2017. The region is industrialized and has all
required infrastructure. Moreover, it is located near sea port in Aktau that can be used for
equipment transportation through Caspian Sea.
Chemistry
The Methanol dehydration reaction is reversible and forms one mole of DME and one mole of
water from two moles of methanol.
2CH3OH⇌ CH3OCH3 + H2O △ H = -23.4 kJ/mol
The catalyst used is γ-Al2O3 catalyst and activation energy is 143.7 kJ/mol. No secondary
reaction take place and selectivity of the process is 83,4% (Azizi, et al., 2014, p. 162).
Table 1. The properties of γ-Al2O3 catalyst (Dlep et al., 1987, p. 332)
BET surface area 195 m2/g

Pore volume 0.59 cm3/g
Mean pore radius 61 nm
Packed density 0.65 g/cm3
Different kinetics equation were analyzed and Langmuir-Hinshelwood equation was derived
manually.
Langmuir–Hinshelwood, 1926 k r K 2M P2M −k 'r K W P D PW
−r m =
(1+ K M P M + K W PW )2
4
Finally, the Bercic equation was chosen as the most realistic and as it is used widely in
industry.
Bercic, 1990 2 2 Cw C E
k s K M (C M − )
K
−r m = ¿¿¿
The catalyst used in the equation is 3-mm γ-Al2O3 and is convenient for plant catalyst choice.
The parameters chosen are as follows (Bercic, et al., 1993, p. 2478):
Table 2. The properties of 3-mm γ-Al2O3 catalyst for Bercic model (Bercic, et al., 1993)
Parameter Value
ks 5.35 × 1013exp(-17280/T)
KM 5.39 × 10-4exp(8487/T)
KW 8.47 ×10-2exp(5070/T)
Conceptual design
Isothermal and Adiabatic reactors were compared as the reaction is exothermic. The
isothermal reactor had to include the heat exchanger surfaces to prevent temperature increase
by use of coolant. The benefits of the isothermal reactor are availability of temperature
control and possibility to increase conversion in reversible reactions. On the other hand, the
tubular system for coolant and use of utilities significantly increase the capital and operation
costs.
Aspen Plus software was used to construct the conversion along temperature range for 100%
and 80% of equilibrium conversion. The safety margin was chosen 390 0C, as the deactivation
of catalyst (γ-Al2O3) occurs above 400 0C (Azizi, 2014, p. 162). Maximum achievable
conversion was found 0.66, as 80% of maximum conversion was used. The 80% usage
decision was based on the economic feasibility of reactor, as the reaction rate decreases near
maximum conversion margin and leads to longer residence time and catalyst amount. The
inlet temperature for adiabatic reactor was then 2900C and outlet temperature was 3900C.
Pressure of reactor was chosen to be 15 bar.
Separation process choice was based on comparison of direct and indirect sequences. Indirect
sequence removes components one-by-one as bottom product, when direct sequence removes
the components from the distillate. Direct sequence leads in lower Vapor flow rate, removing
components in order of lowering volatility that means lower operational cost. The methanol is
not vaporized twice in both columns and electricity usage is lower. Separation process was
chosen to be direct, therefore.
5
Reactor outlet mixture goes to first distillation column that operates at 10 bar an 440C. The
DME is removed as distillate. The guessed pressure due to pressure drop is 10.4 bar and
reboiler temperature is 1540C. The bottom product consisting of water and methanol goes to
second column through valve that decreases the pressure to 1 bar. Second column separates
water from methanol and methanol is recycled back to reactor and mixed with feed before
reactor inlet.
Preliminary mass balance was done using 22 equation of streams and conversion X=0.66. The
calculations were done using Matlab software and the results were as following:
Table 3. Results obtained using Matlab program in k-mol/hour for each stream and each
component.
Stream 0 1 2 3 4 5 6
MeOH 1100 1666.7 566.7 0 566.7 566.7 0
DME 0 0 550 550 0 0 0
Water 0 0 550 0 550 0 550
200 k-tons/year converted into molar basis gives 550 k-mol/hour. Assumptions were: 330
days a year, 24 hours per day, 46 g/mole molar mass of DME. That value was used for
preliminary mass balance. Mass consumption of methanol is 1100 k-mol/hour and 280 k-
tons/year for 200 k-tons/year DME production.
2. Material and Energy Balance
2.1 Mass Balance

The steady-state form of mass balance is following:
∑ ṁi = ∑ ṁe
inlet outlet
In case of shell-and-tube heat exchanger, since the hot stream and the cold stream do not mix,
the mass rate balance for the two streams reduce at steady state to give:
ṁ hot ,∈¿=ṁ hot,out ¿
ṁ cold ,∈¿=ṁ cold ,out ¿
6
Table 4. Mass balance of the reactor
Reactor Inlet (kg/h) Outlet (kg/hour)

Water 27,63677265 9926,098608
Methanol 45014,51969 9803,754983
Dimethyl Ether 19,73763189 25332,81036
Table 5. Distillation Columns mass balance
DME IN OUT (kg/hr)

Tower (kg/hr) Dist Bottom
39,8666
DME 25337,6 25297,74 9
18138,8 18111,0
Methanol 1 27,72618 8
9949,55
Water 1 0,0011788 9949,55
Total 53425,9 53425,96
(kg/hr) 6
Methanol OUT (kg/hr)

IN (kg/hr)
Tower Dist Bottom
DME 19.73725 19.73725 6.84E-10
Methanol 9788.258 9770.634 17.62381
Water 9925.708 27.61538 9898.092
Total
(kg/hr) 19733.7033 19733.7024
Table 6. Stream specifications of first heat exchanger
First Heat exchanger

Streams Hot stream Cold stream
Specifications Inlet Outlet Inlet Outlet
Temperature, 0C 377,0729 159,2848 37,734 150
Pressure, bar 10,4 10,4 15 15
Mole flow, kmol/sec 0,3907828 0,3907828 0,3907849 0,3907838
Mass flow, kg/sec 12,51722 12,51722 12,51728 12,51725
Vapor fraction 1 1 0 0
Mass fraction
Water 0,2202759 0,2202759 0,000613336 0,000613336
Methanol 0,2175608 0,2175608 0,9989487 0,9989487
Dimethyl ether 0,5621633 0,5621633 0,000437991 0,000437991
Table 7. Stream specifications of second heat exchanger
Second Heat exchanger

7
Temperature, 0C 159,2848 110 92,83261 120,2722
Pressure, bar 10,4 10,4 2 2
Mass flow, kg/sec 12,51722 12,51722 22,22224 22,22222
Vapor fraction 1 0,3740348 0 0,1288341
Mass fraction
Water 0,2202759 0,2202759 1 1
Methanol 0,2175608 0,2175608 0 0
Dimethyl ether 0,5621633 0,5621633 0 0
Table 8. Stream specifications of third heat exchanger
Third Heat exchanger

Temperature, 0C 110 44 25 84,95501
Pressure, bar 10,4 10,4 1 1
Mass flow, kg/sec 12,51722 12,51722 22,22222 22,22222
Vapor fraction 0,3740348 0 0 0
Mass fraction
Water 0,2202759 0,2202759 1 1
Methanol 0,2175608 0,2175608 0 0
Dimethyl ether 0,5621633 0,5621633 0 0
Table 9. Stream specifications of flash drum
Flash drum
Specifications Inlet stream Steam stream Outlet stream
Temperature, 0C 120,2722 104,8317 104,8317
Pressure, bar 2 1,2 1,2
Mole flow, kmol/sec 1,233521 0,1954734 1,038047
Mass flow, kg/sec 22,22222 3,521508 18,70071
Vapor fraction 0,1288341 1 0
Mass fraction
Water 1 1 1
Methanol 0 0 0
Dimethyl ether 0 0 0
Table 10. Stream specifications of heater
Heater
Specifications Inlet stream Outlet stream
Temperature, 0C 150 255
Pressure, bar 15 15
Mole flow, kmol/sec 0,3907838 0,3907838
Mass flow, kg/sec 12,51725 12,51725
8
Vapor fraction 0 1
Mass fraction
Water 6,13E-04 6,13E-04
Methanol 0,9989487 0,9989487
Dimethyl ether 4,38E-04 4,38E-04
Table 11. Stream specifications of mixer
Mixer
Specifications Inlet stream Fresh water stream Outlet stream
Temperature, 0C 104,8317 25 92,79833
Pressure, bar 1,2 1 1
Mole flow, kmol/sec 1,038047 0,1954745 1,233522
Mass flow, kg/sec 18,70071 3,521528 22,22224
Vapor fraction 0 0 0
Mass fraction
Water 1 1 1
Methanol 0 0 0
Dimethyl ether 0 0 0
2.2 Energy Balance

Overall energy balance can be written as:
[ ¿ ] − [ Out ] + [ Generation ] =[ Accumulation ]
∑ H ¿−∑ H out =Q+W
∑ ∆ H=Q+W
As W =0
∑ ∆ H=Q
The reactor is adiabatic and the heat duty is 0, therefore no heat goes in and no heat
goes out, no change in enthalpy.
The tables below show the energy balance for each heat-transfer unit’s stream.
Table 12. Energy balance for distillation columns
DME Tower IN [kJ/sec] OUT [kJ/sec]

Feed -111420 Distilate -30564,95
Reboiler 6161,28 Bottom -77601,58
Condenser 3843,09
Total 105258,7227 104323,44
Methanol Tower IN [kJ/sec] OUT [kJ/sec]

Feed -61203.94 Distilate -20035.75
9
Reboiler 4944.357666 Bottom -42695.23
Condenser 6471.3912
Total -56259.58233 -56259.588
Table 13. Energy balance of heat exchangers

Unit In Out Net duty In Out Net duty
Heat exchanger -73792 -79418 5626 -92713 -87087 kJ/s -5626 kJ/s
kJ/s kJ/s kJ/s kJ/s
1
kJ/s kJ/s kJ/s kJ/s
2
kJ/s kJ/s kJ/s kJ/s
3
Table 14. Energy balance of flash drum and mixer
Unit Inlet stream Steam/Fresh water stream Outlet Net

stream duty
Flash drum -336960 kJ/s -46742 kJ/s -290220 2 kJ/s
kJ/s
Mixer -290220 kJ/s -55867 kJ/s -346080 -7 kJ/s
kJ/s
Table 15. Energy balance of heater
Unit Inlet stream Outlet stream Net duty

Heater -87087 kJ/s -73792 kJ/s -13295 kJ/s
From the tables above it is noticeable that calculated net duties of heat exchangers and heater
are almost the same as the net duties recorded from Aspen Plus in Table 28.
Process flow diagram
Whole plant flowsheet are represented in Figure 1A with Equipment ID.
10
RECYCLE
Tin=25 oC
PC-2
M-1
METHANOL Tout= 35oC E-1

R-1
LC-3
LC-1 FC-1
DME
Rin Rout
TC-1 V-2
Tin = 30oC
TC-3 PC-3
TC-2
HEATER
1-EXCH E-3
P-1 T-1 Tout = 40oC LC-5
3-EXCH V-3
Recycle water TC-4
TC-5
P-124
LC-4
2-EXCH
P-122
T-2
WATER
LP, STEAM
160 oC METHANOL
P-2 TC-6
E-2 LC-6
FRESH WATER
LP STEAM
E-4 WATER
LC-2 160 oC
FC-2
M-2 STEAM
F-1
Figure 1A. Process Flow Diagram
ID V-1 V-2 V-3 V-4 M-1 M-2 1-EXCH 2-EXCH 3-EXCH

DME
MeOH Storage T-2 reflux Reactor in Steam gen. Sep. feed
NAME T-1 Reflux drum storage Feed Mixer Fresh Water mixer
tank drum preheater heater condenser
tank
ID HEATER E-1 E-2 E-3 E-4 P-1/P-2 R-1 T-1 T-2
Reator prep. T-2
NAME T-1 condenser T-1 reboiler T-2 reboiler Pump Reactor DME Tower Methanol Tower
heater condenser
11
Design of Primary Equipment
3.1 Design of reactor
3.1.1 Reactor kinetics
The reactor kinetics was based on work of Bercic and Levec (1992).
C ∗C
k s∗K 2M∗(C2M − w D )
K
r m ( C i , T )= 4
(1+2 √ K M ∗C M + K W ∗CW )
−17280
k s ( T )=5.35∗1013 exp ⁡( )
T
8487
K M ( T )=5.39∗10−4 exp ⁡( )
T
5070
K W ( T )=8.47∗10−2 exp ⁡( )
T
b f
(
K=exp a+ + c∗lnT +dT +e T 2+ 2
T ) T
Table 16. Methanol consumption equilibrium constant coefficients
a b*10-3 c d*104 e*108 f*10-3

-9.76 3.20 1.07 -6.57 4.90 6.05
W∗π D 2
F=
4
To insert the kinetics parameters into Aspen software, the coefficients were changed.
Reaction class was chosen as LHHW to insert the proper kinetics coefficients. The
stoichiometric coefficients change and for 1 mole of methanol, the reaction give 0.5 mole
of water and 0.5 mole of dimethyl ether. The reacting phase is vapor. Ci Basis is molarity
in kmol/cum units. The rate basis chosen is Catalyst by weight in kmol/kg*hr. The
kinetic factor is written without specification of T 0 in form of
kinetic factor=k∗T n∗e− E / RT
Where k=1.55e+07, n=0, E=2542.86 kJ/kmol.

The Driving Force Expression section included methanol as reactant with exponent 2
and water with dimethyl ether as products with exponent 0. Option to compute the
reverse rate using microscopic reversibility was chosen. The adsorption Expression
12
section used adsorption expression exponent = 4, concentration exponents and
adsorption constants were filled in as following:
Table 17. Concentration exponents table in Aspen Plus softwaare
Term no.1 Term no.2 Term no.3

Methanol 0 0,5 0
Water 0 0 1
Table 18. Adsorption constants for term 1,2 and 3 in Aspen Software
A B C D
1 0 0 0 0
2 -3,07 4243,5 0 0
3 -2,469 5070 0 0
The expressed coefficients are K1=1, K2=0.046*exp(4244/T), K3=0,085*exp(5070/T),

that correspond to initial kinetics equation by Bercic.
3.1.2 Adiabatic temperature calculations

Adiabatic temperature rise was calculated manually using the following equations.
F A ¿V −F A ¿V +∆ V −r A∗∆V =0 ¿∆ V
d FA
=−r A
dV
F A=F A 0∗( 1−X A )
d XA
F A0 =r A
dV
dX A 1
= ∗r ( X ,T ) =¿ r A∗dV =dX A∗F A 0
dV F A 0 A A
Q generated =∆ U
F∗c p∗dT =r A∗dV ∗(−H R )
F∗C p∗dT =dX A∗F A 0∗(−H R )=dX A∗F∗y A 0∗(−H R )
kJ kmol
dT −H R∗y A 0 −H R∗C A 0
= = =
( kmol )
∗( 3 )
m
=( K )
dX A Cp c p∗ρ kJ kg
( )∗( 3 )
kg∗K m
dT −H R∗C A 0
T =T 0+ ∗X A =T 0 + ∗X A
dX A c p∗ρ
Where H R is heat of reaction,

T0 is initial temperature. (K)
Component A taken as basis is Methanol.
13
Taking H R = -23.4 kJ/mol, C A 0=989.8 kmol/cum, ρ=9.05396 kg/cum, c p=16 kJ/kg*K. The
Adiabatic temperature rise is approximately equal to 160 K. Constructing the graph for
2550C adiabatic temperature growth, the similarity to software results is seen.
1
0.9
0.8
0.7
0.6
Conversion
0.5
0.4
0.3
0.2
0.1
0
250 270 290 310 330 350 370 390
Maximum conversion Real temperature
Temperature Calculated temperature
Figure 2. Comparison of calculated temperature and real temperature versus conversion

3.1.3 Reactor volume calculations
¿−Out +Generation= Accumulation

V
dN A
F A 0−F A +∫ r A dV =
0 dt
dN A
For steady state =0
dt
Differentiating, we get
dF A
=r A
dV
As conversion for single reaction
(F ¿ ¿ A 0−F A )
X A= ¿
FA 0
Substituting, we get
dX
F A0 =−r A
dV
X
dX
V =F A 0 ∫
0 −r A
To integrate, reaction rate equation must be dependent only on conversion of Methanol,

as it is a basis for the reactor.
14
C M = (1−X )∗C M 0
As only one mole of DME and one mole of water are generated from 2 moles of
methanol,
X X
C W = ∗C M 0 ; C D = ∗C M 0
2 2
F A 0 kmol/ s kmol
C M 0= = 3 = 3
Q m /s m
The dependence of temperature on the conversion was used from equation
dT −H R∗C A 0
T =T 0+ ∗X A =T 0 + ∗X A
dX A c p∗ρ
X∗F A 0 2
2 ( )
2 ( 1−X )∗F A 0 Q
k s∗K M∗(( )− )
Q 4K
rm ( X ) = 4
K W∗X
K M ∗( 1−X )∗F A 0 ∗F A 0
(1+2
√ Q
13
+
−17280
2
Q
)
Where k s ( X )=5.35∗10 exp ⁡( )

T
8487
K M ( T )=5.39∗10−4 exp ⁡( )
dT
T 0+ ∗X A
dX A
5070
K W ( T )=8.47∗10−2 exp ⁡( )
dT
T 0+ ∗X A
dX A
K (T )=exp ¿ ¿
Therefore, reaction rate r A ( X ) and using trapezoidal rule for numerical evaluation in
Matlab software, following results were obtained:
Table 19. Theoretical Volume Estimations
Percent of
Maximum
conversio Conversio
n Tin n Intervals Volume
80% 270 0.66 22 8.5184
90% 270 0.7411 37 8.7316
95% 270 0.7865 39 8.8426
98% 250 0.8247 41 15.3604
15
3.1.4 Cost calculations
The amount of catalyst needed is calculated using the volume, void fraction, density and
catalyst cost.
The void fraction of the reactor is 0.4, catalyst cost is 10$ per kg, density is 3,268 gm/cc.
The capital cost of the reactor is calculated using the equation listed above.
Finally, the costs for 4 different reactors and conversions are listed below in the table.
Table 20. Reactor Cost
Diamete Installation
r Length cost Catalyst cost TAC
77188,3
80% 1,35 2,87 70543,99584 53673,64997 2
89848,9
85% 1,35 3,37 80473,59801 63024,46007 9
183675,
90% 1,85 4 129585,1867 140480,2088 3
209599,
95% 1,87 4,5 144370,5188 161475,7918 3
714012,
98% 1,816 17 416146,9431 575297,2601 9
3.1.5 Optimization and conversion choice

The optimization of reactor by capital and operational cost would lead to lower
conversion. The lower conversion leads to higher operation costs for the separation.
Therefore, the compromise was found only after the optimization of the whole plant.
95% of maximum conversion at 2550C inlet temperature gave the lowest total annual
cost for the whole plant appeared to be most economically feasible. The conversion is
0.78 and the reactor conditions are as following:
3.1.6 Design specifications

Table 21. Design specifications of the reactor
Reactor length 4.5 m

Diameter 1.87 m
Pressure inlet 15 bar
Temperature inlet 255 C
Temperature outlet 377 C
Conversion 0,782209051
Void fraction 0.4
Gamma
Catalyst alumina
Particle density 3,268 gm/cc
16
Wall thickness 17.8 mm
3.1.7 Pressure drop calculations
Ergun equation was used to calculate the pressure drop in the reactor. (Ergun, 1952)
It uses the modified Reynolds number to obtain friction factor in packed column. The
equation is as follows:
150
f p= +1.75
Gr p
Where fp and Grp are expressed as:
∆p
∗D p 3
L ϵ
f p=
ρ v2s
∗ ( )
1−ϵ
And
ρ vs D p
Gr p=
( 1−ϵ )∗μ
where: Gr p is the modified Reynolds number,

The Ergun equation option was chosen for Aspen Plus Software pressure drop estimations.
17
15
15
Pressure [1/bar]
14.99
14.99
14.98
14.98
0 0.5 1 1.5 2 2.5 3 3.5 4 4.5
Reactor length [1/m]
Figure 3. Pressure drop versus reactor length from Ergun equation.
It can be seen on the graph that pressure drop is not significant and no extra pumping
equipment is needed.
2.1.9 Velocity calculations

Velocity was calculated for reactor using the following equation:
2
π∗D
Q̇ r =A r∗v r = ∗v r
4
Where Q̇˙ r is volumetric flow in reactor,
Ar is cross-sectional area of reactor,
v ris velocity of stream in the reactor.
The volumetric flow estimated is 1.47 cum/s and diameter is 1.87 m. The velocity of
stream is 0.53 m/s that is not far from recommended range of 0.3 m/s and gives
reasonable pressure drop by Ergun equation.
2.1.10 Reactor wall thickness calculations

The reactor wall thickness was calculated using the following equation:
18
Pdiff ∗R r
t= +t
S∗E−0.6∗Pdiff c
Where t=reactor wall thickness, (inch)
Pdiff=pressure difference between inside and outside of reactor, (psig)
Rr=radius of reactor, (inch)
S=maximum allowable stress for the stainless steel,
E=joint efficiency (0.85-0.9)
tc=corrosion allowance, (inch)
Taking, Pdiff=14 bar= 203.053 psig, Rr=0.94 m= 37.00787 inch, S for stainless steel at
4000C is 16900 psig, E=0.9, tc= 0.2 inch.
The corrosion allowance from water was taken as 0.1 mm/y for water and methanol.
The operational period taken as 20 years, the corrosion allowance is equal to 0.1*30=3
mm. Taking in consideration high temperature, the allowance is 5 mm. The result
reactor wall thickness is 0.7 inch = 0.0178 m = 17.8 mm. The calculated thickness lays in
the convenient range for industrial reactors. (Reactor types and catalysts test, n.d.)
Alternative equation for wall thickness is
Pr∗D r
t=
2∗σ d−P r
Where Pr is pressure in reactor,
Dr is diameter of reactor,
σ dis design stress,
Pr=15 bar = 1500000 Pa, Dr=1.87 m and σ d= tensile strength of stainless steel/ safety
factor=500/4=125.
t2=11.29 mm and is approximate to previous calculation.
For the safety considerations, the larger thickness should be used.
19
1
0.9
0.8
0.7
0.6
Composition
0.5
0.4
0.3
0.2
0.1
0
0 0.5 1 1.5 2 2.5 3 3.5 4 4.5
Reactor length [1/m]
Water Methanol DME

Figure 4. Compositions of components versus reactor length
2.1.11 Energy balance of the reactor

The reactor is adiabatic and the heat duty is 0, therefore no heat goes in and no heat
goes out, no change in enthalpy.
20
400
380
360
Temperature {1/K}
340
320
300
280
260
0 0.5 1 1.5 2 2.5 3 3.5 4 4.5
Reactor length {1/m}
Figure 6. Temperature versus reactoin length
Dynamic simulation included the pressure control. The increase and decrease in process
feed were simulated to observe the behavior of plant in non-operational conditions.
Initially, the feed was increased by 10% and the following graph shows the outlet
temperature change.
21
389
388.5
388
Temperature [1/K]
387.5
387
386.5
386
385.5
385
0 1 2 3 4 5 6 7 8
Time [1/hour]
Figure 5. The Reactor outlet Temperature versus time for 10% increase in feed
The immediate decrease in temperature was caused by lower conversion that occurred
from higher feed rate. However, during stabilization of the outlet, the temperature was
high than operational one. The fluctuations were eliminated during 3 hours.
The similar trends can be seen during the lowering of feed input by 10%.
22
390
389.5
389
Temperature [1/K]
388.5
388
387.5
387
386.5
386
0 1 2 3 4 5 6 7 8 9
Time [1/h]
Figure 6. The reactor outlet temperature versus time for 10% decrease in feed.
2.1.12 Summary of Reactor section

During Capstone II the reactor section was optimized. Initially, most of the estimations
were done manually, and only then manual calculations were checked by the simulation
results. The optimization of reactor section led to optimization of the whole plant.
Dynamic simulation of reactor section was done joint with other units.
2.2 Design of heat integration unit

The heat transfer to and from process fluids is a crucial part of most chemical processes. The
term ‘exchanger’ generally refers to the equipment in which heat is transferred between two
process streams. If a process stream in exchanger is heated or cooled down with a plant
service stream, then such exchangers are called heaters and coolers. If the process stream is
vaporized, the exchanger is called vaporizer, if associated with distillation column - a reboiler,
and if applied to concentrate a solution – an evaporator. The fired heaters are used for
exchangers heated by combustion gases (Sinnot&Towler, 2009, 816-817)
23
2.2.1 Optimization of heat integration unit
The optimization of heat-transfer equipment of DME synthesis process will be discussed in
following chapter.
First optimization steps

Originally, heat integration unit of the DME production process required one heater and one
cooler. The heater was needed to preheat the stream going to the reactor, while the cooler
served to cool down till the acceptable value the temperature of stream forwarded to
distillation unit.
Figure 7. Original heat integration unit
The following Table 22 represents the inlet and outlet temperatures and heat duties of heater
and cooler. Heat duties are very large and the process becomes less stable. Therefore it was
necessary to replace the heater and the cooler with one heat exchanger for control. As it can
be noticed from the Table 22there is enough heat available to replace the heater and the
cooler with one heat exchanger. However, when the heater and cooler were replaced by heat
exchanger, the Aspen Plus simulation did not work since there was loop in the TQ-diagram of
heat exchanger. The loop formation indicates that at some moment the temperature of cold
stream becomes higher than the hot stream temperature, which is thermodynamically
impossible.
Table 22 The specifications of heater and cooler in original case
Unit Inlet temperature, 0C Outlet temperature, 0C Heat duty, kw

Heater 42 290 23270
Cooler 389 44 24929
So, it was decided to add heat exchanger followed by heater in order to reduce the amount of
heat needed to transfer to the inlet stream of the reactor. Secondly, since the temperature
difference between inlet and outlet temperatures of the cooler is high, the cooler was divided
into two coolers: first one is for steam generation and second one uses cooling water. So the
initial optimization of the heat integration unit gave the following result represented in Figure
8.
24
Figure 8. First optimized heat integration unit
The temperatures indicated in the Table 23 were obtained as a result of work on Aspen Plus
simulation. The highest outlet temperature of cold stream in heat exchanger was desired in
order to reduce the heat duty of the heater. So, the highest outlet temperature possible to
design in this case of heat transfer is 150 0C. The higher values of outlet temperatures led to
the formation of loop in the TQ-diagram of heat exchanger.
Table 23 Specifications of first optimized heat integration unit
Unit Inlet temperature, 0C Outlet temperature, Heat duty, kw

0
C
Heat exchanger 42 150 6476
(cold stream)
Heater 150 290 16794
Cooler 1 180 110 11691
Cooler 2 110 44 6753
The TQ-diagram of the obtained heat exchanger is presented in Figure 9. As it can be

observed from the plot there is no formation of loop, which reports the appropriate operation
of designed heat exchanger.
Figure 9. TQ-diagram of the obtained heat exchanger in first optimization

Consequently, the heat duties in first optimization were significantly reduced, which is
advantageous for safety and economic considerations. The installation cost analysis of
25
original and first optimized cases presented in Table 24. Despite the fact that in initial case
there are only two operation units, the total installed cost of them considerably higher than the
total cost of optimized heat integration unit.
Table 24 Cost estimation of original and first optimized case
Operation unit Original case, $ First optimized case, $

Heat exchanger - 106 489,71
Heater 3 768 529,896 2 856 117,469
Cooler 1 385 254 468 745,5815
Cooler 2 - 343 148,8835
Total Cost 4 153 783,896 3 774 501,644
Second optimization steps

During the first optimization the heat integration unit contained 1 heat exchanger, 1 heater and
2 coolers. The first optimization of the process was done for 66% conversion of methanol.
The further optimization of the heat integration unit was done based on the economic
evaluation of the heat integration unit (including 2 heat exchangers, 1 heater and 1 cooler) for
different conversions. As the conversion changes, the temperatures and compositions of
streams also change as well. Subsequently, these changes affect the heat exchangers
specifications. The Table 25 contains the total costs of the whole heat integration unit for
several conversions of methanol. To clarify, installation costs of two coolers were calculated
as costs for heat exchangers. As mentioned before first cooler was for vapor generation and
second cooler used cooling water.
Table 25. Cost estimation of heat integration for different conversions
Conversion 0,66 0,74 0,78 0,825

Heat $ 106 489,7 $ 64 719,4 $ 107 887,1 $ 64 893,8
exchanger 1
Heat $ 468 745,6 $ 237 112,1 $ 93 770,3 $ 244 664,9
exchanger 2
Heat $ 343 148,9 $ 320 856,6 $ 47 804,4 $ 301 257,6
exchanger 3
Heater $ 2 856 117,5 $ 2 853 948,96 $ 2 341 693,9 $ 2 220 041,8
Total cost $ 3 774 501,6 $ 3 476 637,1 $ 2 591 155,7 $ 2 830 858,2
From the Figure 10 it can be observed that the cost line of the heat integration unit gradually
decreases as the conversion increases till 0,78 conversion. After that the cost profile
noticeably begins to increase. So the lowest installed cost for the heat integration unit
including one heat exchanger, one heater and two coolers is for 0,78 conversion of methanol.
26
In other words, the most optimal conversion based on the economical evaluation of heat
integration unit is 0,78 with total cost of $ 2 591 155,72.
Total cost of heat exchangers vs conversion

4000000
3500000
3000000
Total installation cost, $
2500000
2000000
1500000
1000000
500000
0 0.66 0.74 0.78 0.83

Conversion of methanol
Figure 10. Total cost of heat integration vs. conversion

In the next step in optimization of the heat integration part of the process the separator and
mixer were added to the simulation. The outlet cold stream from the second heat exchanger
goes to the flash drum, which generates steam. The outlet stream of the separator goes to the
mixer where it mixes with fresh water. Additionally, the coolers were replaced by the heat
exchangers in the simulation on Aspen Plus. Moreover, the cooling water stream was added to
the third heat exchanger. On this stage the optimization of heat integration unit for the DME
production is finished. The whole flowsheet diagram of optimized heat integration unit
including process controllers is presented in Figure 11.
27
Figure 11 Schematic drawing of DME optimized heat integration unit including process
control
2.2.2 Design Specifications of heat integration unit
For the basic design of heat exchangers the common equation for heat transfer is:
Q=UA ∆T m
where Q=heat transfer per unit time ,W
W
U =the overall heat transfer coefficient ,
m 20 C
A=heat transfer area , m 2
∆ T m=themean temperat ure difference
Generally, for the design of exchanger the main objective to determine the surface area
needed for particular heat duty using temperature differences given. When area is unknown,
the design of exchanger is estimated by trial-and-error procedure when the value of overall
coefficient is predicted. However, heat exchangers in this process were designed using Aspen
Exchanger Design and Rating software. The areas and sizing parameters obtained for heat
exchangers are presented in Table 26.
For the cost estimation all of the heat exchangers of this DME production plant are assumed
to be shell and tube, fixed-tube sheet and counter-current. Such configuration provides large
heat transfer area and high log mean temperature difference for better heat exchange. The
material carbon steel has higher thermal conductivity and lower cost in comparison with
28
stainless steel. The thermal conductivities of carbon steel and stainless steel are equal to 43
and 16 W/ (m*K) correspondingly. (Sinnot&Towler, 2009) Therefore the material chosen for
heat exchangers is carbon steel. However, carbon steel is more corrosive than stainless steel,
thus the material for process heater is stainless steel. For the process heater we assume that the
heater is fired heater. The heater is heated using natural gas. The heating value of natural gas
is equal to 0,0377 GJ/m3. Taking into account that required heat duty for heater is equal to
13,295 MW (from Table 28) and assuming 8000 operating hours per year, the annual
required heat duty is:
13,295∗60∗60∗8000=382896 GJ per year
NG 382896 m3 3
Amount of = =10156392 ∨1269,6 m /hr
yr 0,0377 yr
Moreover, the heat integration contains the flash drum and mixer. The flash drum is applied
to separate the vapor and liquid. The vapor and liquid are assumed to be in equilibrium and
the vessel is adiabatic. Likewise, vessels assumed to be made of stainless steel. The
specifications of vessels sizing are presented in Table 27. The sizing of these vessels was
obtained based on these assumptions:
 Residence time t is equal to 10 minutes
 The volume of vessel is found using flow rate from Aspen Plus and residence time
 The mixer is full for 5/6, the flash drum is half full in order to provide sufficient space
between inlet and vapor stream for liquid drops
 Height = 2 * Diameter
So, the equations for volume of fluid in mixer and diameter of mixer are following:
5
∗( π D2 )
6
V fluid = ∗2 D
4
12¿ V fluid
D=
√
3
5π
For the flash drum is following:
1
∗( π D2 )
2
V fluid = ∗2 D
4
4 ¿V fluid
D=
√
3
29
The mixer and the third heat exchanger need water for cooling: 13000 kg/hr and 80000 kg/hr
correspondingly. The condenser of first distillation column produces sufficient amount of
output water of the same specifications (temperature and pressure) needed for water
consumption in heat integration. Therefore, streams of fresh water and cooling water in the
Figure 11 provided by the first distillation column’s output water stream. This is very
beneficial since it reduces annual operating costs (OPEX) of heat integration.
Table 26. Design specifications of heat exchangers
Heat exchanger First Second Third

Area, m2 52,9 43,7 15,5
Shell ID, m 0,6 0,8 0,4
Tube length, m 2,4 4,9 6,1
Table 27. Specifications of mixer and flash drum
Specification Mixer Flash drum

Volume flow rate, m3/s 0,0240009 2,621112
Volume, m3 14,40054 1572,6672
Residence time, sec 600 600
Diameter, m 2,224437069 12,6063412
Height, m 4,448874139 25,2126824
The temperature and pressure specifications of all streams in heat integration unit can be
found in following Material balance section.
The schemes and more detailed mechanical characteristics of heat exchangers can be found
from the Figure 12, Figure 14 and Figure 16. As it can be seen the first heat exchanger has 1
pass in shell side and 6 passes in tube side, while second and third heat exchangers are 1 pass
in both sides. Moreover, according to the TQ-diagrams in the Figure 13, Figure 15 and Figure
17 the heat transfer in heat exchangers occur adequately without formation of loops. For more
deep specifications of heat exchanger TEMA sheets of heat exchangers are provided in
Appendix B.
30
Views on arrow A
A 139.625 Overall
T2
13.625 8.1875 12.0 70.5
23
T2 S1
23
T1
S1
23
23
24
S2
T1 S2
8.1875 23.25 47.0
Pulling Length 75 2.0 2.0
6
22.3
22.3
4.0 4.0
2 Bolts 2 Bolts
Fixed Sliding
N o z z le Data De s ign D ata Un its Shell Ch annel
Re f OD W all Sta ndar d No tes De s ign Pr es s ure ps i 160. 240. Aspen Shell & Tube Exchanger
S1 16.0" 0.3 75" 150 AN SI Slip on De s ign Temp era tur e F 780. 370.
S2 14.0" 0.3 75" 150 AN SI Slip on Full Va c uum
T1 4.0 " 0.2 26" 150 AN SI Slip on Co rr os ion Allow anc e in 0.1 25 0.1 25 Setting Plan
T2 4.5 " 0.2 37" 150 AN SI Slip on Tes t Pr es s ur e ps i
Nu mber o f Pa s s es 1 6 De s ign C ode s BEM 25 - 96
Ra diogr aphy ASME Sec tion VIII D iv . 1
PW H T TEMA R
Inter nal Volume ft³ 28.1581 11.1215 Drawing Number
C u s tomer Spec ific ations
W eigh t Su mmary
Empty Flo oded Bundle Re v is ion D a te Dw g. C h k . App.
44 91 lb 63 78 lb 24 86 lb 17.04.201 6
Figure 12. The first heat exchanger sketch specifications
Figure 13. The first heat exchanger TQ-diagram
31
Views on arrow A
A
265.25 O verall
18.6875 15.9375 15.0 168.5 20.4375
S2 T1
25
T2
S2
25
T2 S1
15.9375 38.375 115.25
25
27
Pulling Length 158
S1
2.0 2.0
T1
7
28.5
28.5
25
4.0 4.0
2 Bolts 2 Bolts
Fixed Sliding
N o z z le Data De s ign D ata U n its Shell C h annel

Re f OD W all Sta ndar d N o tes D e s ign Pr es s ur e ps i 50. 170. Aspen Shell & Tube Exchanger
S1 6.6 25" 0.2 8" 150 ANSI Slip on D e s ign Temp era tur e F 390. 390.
S2 14.0" 0.3 75" 150 ANSI Slip on Full Va c uum
T2 10.75" 0.3 65" 150 ANSI Slip on C o rr os ion Allow anc e in 0.1 25 0.1 25 Setting Plan
T1 12.75" 0.3 75" 150 ANSI Slip on Tes t Pr es s ur e ps i
N u mber o f Pa s s es 1 1 D e s ign Code s BEM 32 - 192
R a diogr aphy ASME Sec tion VIII Div . 1
PW H T TEMA R
Inter nal Volume ft³ 87.8549 32.2727 Drawing Number
W eigh t Su mmary
Empty Flo oded Bundle R e v is ion Da te Dw g. C h k . App.
13 585 lb 19 700 lb 88 36 lb 17.04.201 6
Figure 14. The second heat exchanger sketch specifications
Figure 15. The second heat exchanger TQ-diagram
32
Views on arrow A
A
288.125 O verall
11.6875
6.125
8.75 223.25 18.25
S2 T1
17
T2
S2 T2 S1
6.125 48.0 144.0
223
17
Pulling Length
17
19
S1
2.0 2.0
15.6
15.6
T1
3.8906
3.8906
4.0 4.0
17
2 Bolts 2 Bolts
Fixed Sliding
No z z le D ata De s ign D ata Un its Shell Ch annel

Re f OD W all Sta ndar d No tes De sign Pr es s ur e ps i 50. 170. Aspen Shell & Tube Exchanger
S1 6.6 25" 0.2 8" 150 AN SI Slip on De sign Temp era tur e F 250. 300.
S2 6.6 25" 0.2 8" 150 AN SI Slip on Full Va cuum
T2 4.5 " 0.2 37" 150 AN SI Slip on Co rros ion Allow anc e in 0.1 25 0.1 25 Setting Plan
T1 10.75" 0.3 65" 150 AN SI Slip on Tes t Pr es s ur e ps i
Nu mber o f Pa ss es 1 1 De sign C ode s BEM 17 - 240
Ra diography ASME Sec tion VIII Div . 1
PW H T TEMA R
Internal Volume ft³ 32.1092 6.5 Drawing Number
W eigh t Su mmary
Empty Flo oded Bundle R e v is ion Da te Dw g. Ch k. App.
52 81 lb 72 10 lb 30 72 lb 17.04.201 6
Figure 16. The third heat exchanger sketch specifications
Figure 17. The third heat exchanger TQ-diagram

For smooth, safe operation and control there are several controllers in the heat integration
unit. In the Figure 11 there level controllers for mixer and flash drum, temperature controllers
after heater and before the third heat exchanger, flow controllers for the feed, cooling water
and mixer outlet streams and pressure controllers after the reactor and for steam stream.
2.2.3 Cost Analysis

Cost estimation of heat integration unit was evaluated using capital installed investment cost
equations. The heat exchangers costs were calculated using equation for heat exchangers,
33
mixer and flash drum using equations for pressure vessels, heater applying equation for
furnaces.
All obtained installed costs are shown in Table 28 and Table 29.
As mentioned before the material for heat exchangers is carbon steel, for heater, mixer and
flash drum – stainless steel. The type of heat exchangers is fixed-tube shell. The values of all
factors relevant to the calculations are presented in tables below.
Table 28. Cost estimation of heat exchangers and heater
Unit Heat Duty, kW Area, m2 Fm Fd Fp Fc Cost, $

Heat Exch. 1 5626,5 52,9 1 0,8 0,05 0,85 107 887,12
Heat Exch. 2 9085 43,7 1 0,8 0 0,8 93 770,27257
Heat Exch. 3 5626,7 15,5 1 0,8 0 0,8 47 804,39742
Heater 13295 0,75 1 0 1,75 2 341 693,926
Total
installed cost 2 591 155,716
Table 29. Cost estimation of mixer and flash drum
Specifications Mixer Flash drum

Diameter, m 2,224437069 12,6063412
Height, m 4,448874138 25,2126824
Pressure, bar 1,2 1,2
Fm 3,67 2,25
Fp 0,984323632 0,984323632
Fc 3,612467729 2,214728172
Installed cost, $ 242 806,3717 4 854 922,293
Total installed cost of optimized heat integration unit including three heat exchangers, heater,
mixer and flash drum is equal to $ 7 688 884,4 which is by definition is Capital installed
investment (CAPEX = $ 7 688 884,4).
CAPEX
TAC= +OPEX
payback period
Operating costs (OPEX) are represent costs for natural gas consumption of heater. The price
for natural gas is 11,1 $/GJ (Richard Turton, 2009)
Q heater ∗Cost NG
Annual cost of NG=
efficiency
Assuming efficiency oh heater is 90% and taking value for Q from Table 28:
Annual cost of NG=¿$ 4 722 384 = OPEX
Taking into account that payback period is 3 years:
34
7 688 884,4
TAC= +4 722384
3
The total annual cost for heat integration unit is:
TAC = $ 7 285 345,5
2.3 Distillation Columns

Distillation is separation process of two liquids having different boiling points and the larger
difference between boiling points of those liquids the more accurate process will be (McCabe,
1993). The separation process takes place in continuous distillation column consisting from
the following major parts:
 Condenser
 Reboiler
 Reflux drum
 Trays
The designed plant uses “tray column” which has perforated plates (trays) inside and number
of plates defines the height of the column and its cost (ibid.).
The liquid enters the distillation column at optimal feed tray, which can be determined by
economic evaluation as well as number of trays (Bravo, 1990).
After liquid entered the column it falls down to reboiler which sends heat to falling liquid in
order to vaporize it. Vaporized liquid is sent back to the column, while liquid leaves the
reboiler as bottom product. Vapor from the reboiler touches the falling liquid allowing the
separation process to be. Vapor reaching the condenser is turning to liquid phase and leaves
the condenser as distillate product, while the steam turns back to the column via reflux drum
(ibid).
DME production plant requires two distillation columns to complete the separation process:
the first distillation column is used to obtain dimethyl ether and the second one is to separate
methanol from water which is sent back to the reactor.
To design distillation columns via Aspen plus software “Radfrac” model was used as this type
of column can offer a huge range of results ofr sizing and rating of tray, column, reboiler and
condenser (Sinnott, 2005, p. 118-123).
In configuration parameters the type of condenser and reboiler can be specified. For the DME
processing plant the condenser was chosen to as “total” as all vapor leaving the column is
35
condensed. The reboiler was specified as “kettle” as it is simpler than “thermosiphon” and
requires pumping to send liquid to the reboiler (McCabe, 1993).
In order to achieve good separation in column, liquid and vapor flow should have good
contact on each tray. According to Table 30, tray type was chosen. Both columns’ trays are
designed to be sieve tray, and spacing between them taken as 0.6019 m. Sieve plate is the
simplest type of cross-flow plate. It is perforated plate, and vapor flows upward through
holes, thus contacting with liquid on each plate.
Table 30. Type of plate contactors
Tray type Bubble Cup Dual Flow Sieve Dual Flow
Capacity Moderate High High High
Low to Low to
Pressure drop High Moderate
moderate moderate
Moderate Low High High

Efficiency
(0.6 - 0.8) (0.5 - 0.7) (0.7 – 0.9) (0.7 – 0.9)
Very high. Low. 2:1 3 -5:1

Suitable for Cannot handle Not suitable Higher
Turndown
very low varying loads for varying turndown can
liquid rates loads be provided
Relatively Low to
Maintenance Low Low
high moderate
Extremely
High. Tends to
Fouling low. Suitable Low to
accumulate Low
tendency for Severe moderate
solid particles
fouling
For columns,
High fouling When
Main Very low flow where
and corrosive turndown not
application conditions turndown
services important
important
High. 3 times
Higher that for
Cost more than for Low Low
sieve trays
sieve trays
36
It is important to note that there exist some restrictions for distillation column and sieve-plate
hydraulic design. Sieve trays have specified range for satisfactory operation. Basic
requirements are sufficient area and spacing to have acceptable pressure drop and sufficient
downcomer (DC) area for liquid to flow freely between plates. Figure 18 shows the operating
range of sieve plate.
Figure 18. Sieve-plate performance diagram, (Sinnott & Towler, 2012)

Also, sieve plate design based on vapor and liquid flow rates in column. Flooding is taken as
70%, it sets the upper limit of vapor flow rate, and flooding calculation method was chosen to
done by Fair correlation in Aspen Plus software. Weeping conditions refer to the lower limit
of vapor flow rate. The acceptable range of liquid flow rate is provided by weeping and
downcomer backup.
Table 31. Basic requirements for distillation column (Sinnott & Towler, 2012)
Restrictions
Less than 15% of
Weir height
spacing (40-90mm)
Entrainment <0.1
Weir length 0.6-0.85 (m)
Weir loading <0.01944 (m2/s)
DC back-up <0.5
DC velocity <0.21 (m/s)
37
2.3.1 Methods of Optimization
As it was previously mentioned, conversion of methanol was 80% of equilibrium from
Capstone I results. Therefore, distillation towers were optimized basing on that value.
However, in order to optimize the whole process, conversion of methanol has been changed
and each time new optimization of distillation columns was performed. Eventually, there are
four optimized results of tower, for 80%, 90%, 95% and 98% of equilibrium.
Optimization of columns was based on calculation of total annual cost (TAC), which is an
effective economic objective, and by using cost equations the cheapest one is suggested to be
the most optimal.
Step 1: With specified bottom and distillate compositions, optimum design is determined by
changing the total number of stages over a range of values. Moreover, for each case required
reboiler and condenser duty, diameter and height of the column were evaluated. In addition,
the feed tray location was changed for each case of total stages, until the minimum reboiler
duty was found.
Step 2: In order to calculate heat-transfer areas of heat exchangers, reasonable overall heat-
transfer coefficient, which was taken as 500 W/m2K.
Step 3: The information obtained from step 1 and step 2 was used to calculate the capital cost
of column, trays, reboiler and condenser. Energy cost was calculated by determining the
amount of used utilities for reboiler and condenser.
2.3.2 Cost analysis estimation

Cast estimation of both distillation columns was performed in the same manner. Economic
estimation used Installed cost which includes cost of equipment and all expenditures of its
installation. Marshall and Swift (M&S) factor was taken as 1536.5 as it was estimated in
2012. Payback period initially was taken as 3 years (Lyuben, 2011, p. 73).
Equipment Capital Costs

Equipment cost ( $)=column+ trays+reboiler+ condenser
For estimating price of Column
M ∧S
Column cost ( $ )= ( 957.9∗D1.066∗H 0.82 ) ( 2.18+ F cc )
280
Where F c c =F m∗F p
F p=1+0.0074 ( P−3.48 )+ 0.00023 ( P−3.48 )2
and value for Fm =3.67 is taken from
Purchased cost of trays was calculated from the following equations.
38
M ∧S
Trays ( $ )= ∗97.2 D 1.55∗F c
280
F c =Ft + Fm
Ft is 0 for sieve trays, and Fm is 1.7 for stainless steel.
Condenser and Reboiler were calculated as heat exchangers.
M ∧S
Exchanger ( $ )= ∗474.7 A 0.65∗( 2.29+ F c )
280
F c =( F ¿ ¿ d + Fm )∗F m ¿
Fm = 3.75 for stainless steel; Fd is1.35 for kettle reboiler and 1.0 for condenser.
Operating costs
$
Energy cost ( year )=cooling wate r+ steam
Table 32. Utility cost (Luyben, 2011)
Utility Specification Cost

Cooling water - $ 0.72/GJ
Steam LP steam, 6 bar, 160 oC $ 7.78/GJ
Equipment cost
Total annual cost ($ / year )= + Energy cost
Payb ack period
2.3.3 DME TOWER
Optimization
Optimization process through Step 1 to Step 3 was done for each case of conversion. All
optimal TAC results are shown in Table 33 and Figure 19.
Table 33. Total annual cost of DME tower at different conversion (only optimum values)
Conversion 80% 90% 95% 98%

TAC ($ millions) 2.71 2.77 2.76 2.81
39
2820000
2800000
2780000
2760000
TAC [$ millions]
2740000
2720000
2700000
2680000
2660000
80% 85% 90% 95% 100%
Conversion
Figure 19. DME tower total annual cost for different conversion
According to the Figure 19 the optimum case of distillation tower is for 80% conversion.
However, to reach process optimization, TAC of heat exchangers, 1st and 2nd column and
reactor were summed up. As a result, at 95% conversion process has its optimal value. From
this point, project will provide distillation column results only for conversion of 95% of
equilibrium. Other conversion results will be provided in Appendix C.
In order to obtain required purity, Design Specification in Aspen Plus was used, where mole
purity of Methanol at the top and DME at the bottom is specified to be 0.001 and 0.0005,
respectively and distillate rate calculated to be 550.252 k-mol/hr.
Table 34. Specified component compositions for DME Tower
Component Feed Distillate Bottom

Mole Flow (k-mol/hr)
Water 551.073 0.00003 551.073
Methanol 298.233 0.550 297.683
DME 550.126 549.702 0.424
Mole Fraction
Water 0.394 0 0.648
Methanol 0.213 0.001 0.351
DME 0.393 0.999 0.0005
40
The optimum number of stages in DME Tower was found to be 21 stages including reboiler,
with TAC equal to $ 2 763 211.
Table 35. Optimum DME Tower design
NT 18 19 20 21 22
ID (m) 2.16 2.18 2.11 2.14 2.10
Qr (MW) 6.397 6.340 6.221 6.161 6.164
Qc (MW) 4.081 4.024 3.904 3.843 3.845
TAC ($ millions) 2.813 2.806 2.772 2.763 2.768
2900000
2800000
2700000
TAC [$ millions]
2600000
2500000
2400000
2300000
2200000
18 18.5 19 19.5 20 20.5 21 21.5 22 22.5
Number of Trays
Figure 20. Total Annual Cost vs. Number of Trays

Feed tray location was obtained based of heat input of reboiler and as a result, Feed Stage is
found to be 10 (Figure 21), with corresponding duty of 6161.25 kW (Appendix C).
41
6350
6300
Reboiler Duty [MW] 6250
6200
6150
6100
6050
9 10 11 12
Feed Tray
Figure 21. Feed Tray location
Operating Conditions
Distillation column was designed to separate DimethylEther (DME) from water/methanol
mixture with 99% purity. Separation process in column is continuous distillation and
thermodynamic model is NRTL-RK. Amount of feed to DME tower flows at rate 1399.43 k-
mol/hr in a liquid phase with T=44 oC and P=10.4 bar. Components composition specification
is shown in Table 34. Pressure drop in column is taken to be 0.01 bar. Both distillate and
bottom products are drawn in a liquid phase. Outlet temperature of distillate product is 44.43
o
C and pressure is 10 bar. Bottom product is a mixture of water and methanol, and it leaves
column at T = 152 oC, P =10.2 bar.
Distillation design is carried out by Aspen Plus process simulation software, which allows
determining the stage and reflux requirements that satisfies desired separation. Firstly,
calculation type of simulation for distillation column was conducted in EQUILLIBRIM
model, which means ideal separation on each tray. After determining optimum stage number
and reflux ratio, and by predicting tray efficiency, simulation was performed in RATE
BASED model, which shows more realistic results. Normally, column efficiency (E o) for
preliminary design assumed to be 70% (Sinnott & Towler, 2012).
number of theoretical stages

E0 = ∗100 %
number of actual stages
42
The number of stages depends on reflux ratio, as reflux ratio increases number of required
stages decreases. Hence capital cost decreases, but utility and operating costs increases. After
optimization the optimal Reflux Ratio found to be 0.457 (equilibrium model).
Column Design
The optimum number f stages obtained to be 21 stages, and by using Equation 3.10, number
of actual tray calculated as 30 stages. In Aspen Plus, Tray Sizing was used to estimate
diameter of column and Tray Rating used to determine if the tray design satisfies
requirements mentioned in Table 31. Results of column and tray design are provided in table
below. According to Table 36, column meets all design restrictions.
Table 36. Base design specification of column and tray
Theoretical number of stages 21

Real number of stages 30
Feed tray 10
Diameter 2.14 m
Height 18 m
Weir height 50 mm
Weir loading 0.0155m2/s
DC velocity 0.06m/s
DC backup 0.31
Total Condenser
In DME tower vapor is totally condensed by using total condenser and thus distillate product
flows from tower in a liquid phase. Condenser required to change fluid phase, from saturated
vapor to saturated liquid and cooling water is used as utility.
43
CW
Tin=25 oC
Saturated Vapor
Condenser
T=44.4 oC
Saturated Liquid
CW T=44.4 oC
Tout=35 oC
Figure 22. Condenser flow diagram

Heat duty of the total condenser is taken from Aspen Plus simulation and is equal to 3843
kW. Heat transfer coefficient is taken as 850 W/m 2K (Table A2) and cooling water flows
counter-currently at 1 bar. In order to calculate area of condenser Equation XX was used.
Consumption rate of cooling water is obtained by hand calculation and by Aspen, results are
identical.
Q=UA ∆T m
( T 1−T ¿ ) −(T 2−T out )

∆ T m=
( T 1−T ¿ )
ln
(T 2−T out )
Q=mc p ∆ T
As a result, ∆Tm = 13.84 K, taking cp=4.18 kJ/kg*K and area for total condenser Ac = 327 m2
and mw = 331224 kg/hr.
Kettle Reboiler
According to Aspen simulation, heat duty of reboiler is 6161 kW, and heat-transfer
coefficient is taken also as 850 W/m2K. Low pressure steam at 6 bar, and T = 160 oC is taken
as utility. Latent heat of vaporization is 2085.03 kJ/kg.
Saturated vapor
T2 = 152 oC
Steam
Tin = 160 oC
Product
Steam
Tout = 160 oC Saturated liquid
T1 = 152 oC
Figure 23. Kettle reboiler drawing

Q=mλ
44
By using Equations XXX area of reboiler was calculated, Ar = 869.7 m2. Required amount of
vapor is mv = 10637 kg/hr.
Reflux Drum and Sump

In order to calculate the size of reflux drum and sump, several assumptions were made.
Firstly, reflux drum assumed to be vertical, and sump is. Height is a twice diameter (H=2D).
Diameter of reflux drum and sump calculated from volume flow rate of liquid at top stage and
bottom stage, respectively. Residence time is taken to be 10 min. Also, estimated sizes were
used for Dynamic simulation.
π D2
V= ∗H
4
Assuming that reflux drum is filled by liquid only half, H in equation equals to D.
Table 37. Size for reflux drum and sump
Volume flow rate

Hydraulics 3
Volume (m3) D (m)
(m /min)
Reflux drum 0.98 9.90 2.32
Sump 0.45 4.45 1.78
Aspen Plus Simulation

Above-mentioned results are provided for distillation process which calculation was done on
EQUILIBRIUM model. Table 39 shows results for RATE BASED model.
From Figure 24 temperature profile of real DME distillation column can be observed.
Temperature rises uniformly along column.
45
140
120
Temperature [oC]
100
80
60
40
0 5 10 15 20 25 30
Stage
Figure 24. Temperature profile (Rate based model)
Figure 25 shows that top of the column contains mainly DME, which molar fraction is 0.999
and bottom product has methanol and water. From that Figure 25, it can be concluded, that
distillation column reached satisfactory separation.
1
0.8
Water
Mole Fraction
0.6 Methanol
DME
0.4
Water+Metha
nol
0.2
0
0 3 6 9 12 15 18 21 24 27 30
Stages
Figure 25. Composition Profile (Rate based model)
Moreover, Tray efficiency was obtained from Aspen Plus. Overall tray efficiency at
Equilibrium was guessed as 70%, and from simulation on Rate based model, overall tray
efficiency of actual distillation column found to be 84%. Plate efficiency plot can be found in
Appendix C. Stream results also provided in Appendix C.
46
Dynamic Simulation
In order to satisfy product quality, which is 99% pure DME and to maintain steady plant
process during plant operation several controllers were installed. The key process variables
are liquid level in reflux drum and sump, pressure at the top of tower and temperature at 14 th
stage. Therefore four controllers were adjusted. LC-1 refers to controller that is responsible
for the reflux drum liquid level and LC-2 is controller that monitors liquid level of sump.
Table 38. Controllers’ Specification
Controlle Gain Integral Controlle

Set Point Range
r [%/%] time [min] r action
LC-1 2.9 m 10 60 direct 2–4m
PC 10 bar 20 12 reverse 5 – 15 bar
LC-2 2.23 m 10 60 direct 1.75 – 3 m
TC 120 0C 1 20 reverse 105 – 135 0C
Feed flow rate was manipulated to observe controllers action, it was decreased by 10% and
increased by the same amount. First hour run at initial condition, after flow rate was
decreased, controllers are able to stabilize production rate within 1 hour, as shown in Figure
26.
1250,0 1300,0 1350,0 1400,0
500,0520,0540,0560,0
DME distillate
Feed
0,0 0,2 0,4 0,6 0,8 1,0 1,2 1,4 1,6 1,8 2,0
Time Hours
Figure 26. Flow-rate change by 10%
Also, DME purity at distillate kept 99% with negligible change after flow rate has been
changed.
47
0,9992 0,9998
DME purity
0,0 0,2 0,4 0,6 0,8 1,0 1,2 1,4 1,6 1,8 2,0
Time Hours
Figure 27. DME purity response after decreasing flow rate by 10%
Cost Analysis
Economic analysis for DME tower used the equations that were written in 2.3.2 Cost analysis
part. Moreover, cost estimation for Rate based model was performed too. As it can be seen in
Table 39 Rate based model results slightly deviates from Equilibrium one. However, Rate
based results were taken when whole plant economic analysis calculated, as it has more
realistic column performance.
Table 39. Comparison of Equilibrium and Rate Based models
Equilibriu
Model Rate Based
m
COLUMN $ 758 031 $ 792 680
Tray number 21 30
Feed tray 10 14
ID (m) 2.14 2.23
H (m) 17.8 17.8
Reflux Ratio 0.457 0.497
TRAYS $ 82 586 $ 88 131
REBOILER $ 1 558 905 $ 1 622 890
Qr (kW) 6160.8 6275.8
Ar (m2) 870 925
mvapor (kg/hr) 10637.3 10760
CONDENSER $ 614 590 $ 625 384
Qc (kW) 3843 3949
Ac (m2) 327 335
48
mwater (kg/hr) 340 105 340 671
Capital Cost ($
3.02 3.13
millions)
Energy Cost ($
1.46 1.48
millions)
TAC ($ millions) 2.46 2.53
2.4 Design of distillation column 2
Optimization
To optimize the whole plant the second distillation column was evaluated for finding total
annual cost for four different conversions (80%, 90%, 95% and 98%):
Conversion 80% 90% 95% 98%
2447245 1869870 1909355
TAC ($) 1615197
2500000
2300000
2100000
TAC ($/year)
1900000
1700000
1500000
80 85 90 95 100
Percentage conversion
Figure 28. Conversion vs. TAC for the second distillated column.
From the Figure 28 it can be clearly seen that the cheapest option for the methanol column
design is using 98% conversion but taking into account that the whole plant should be
optimized 95% of equilibrium conversion was chosen and therefore the following design and
optimization will be based on this value.
To start the optimization of the unit theoretic guess of number of stages referring to the total
annual cost was obtained and for each number of trays an optimal feed tray was found by
defining reboiler duty. So that for 95% efficiency conversion the optimal number of trays was
49
found to be 25 (Figure 29) and other optimal number of trays for other efficiency conversion
may be found in the Appendix D.
Table 40. Characteristics for 95% efficiency conversion
NT D (m) Qcon (W) Qreb (W) Tac ($/yr)

21 2.41 6717916.13 5165589.32 2145150.92
23 2.31 6566080.69 5033077.88 2098821.79
24 2.30 6494620.26 4964613.48 2101148.06
25 2.28 6427711.64 4900684.52 2075932.09
26 2.27 6379485.86 4855412.32 2085010.00
27 2.18 6588856.99 4981445.46 2099847.34
29 2.10 6775750.67 5171262.76 2138523.05
From the Table 40 it is seen that the minimum TAC 2075932.09 $ is for 25 Number of trays
and the graph gives the visual representation of how the total annual cost varies with different
number of trays:
1980000
1960000
1940000
TAC ($/year)
1920000
1900000
1880000
1860000
20 21 22 23 24 25 26 27 28
Number of trays
Figure 29. Total annual cost vs. Number of trays for 95% efficiency conversion.
After the number of trays was obtained an optimal feed tray was determined by the
minimizing the reboiler duty and the result can be seen from the Figure 30 that feed tray being
equal to 17 the reboiler duty is the lowest 3522 kW.
50
3700
3650
3600
Reboiler duty (kW)
3550
3500
3450
3400
15 16 17 18 19
Feed tray
Figure 30. Optimal feed tray 17 for Number of trays 25.
Operation conditions
The purpose of the second distillation column is to separate water and methanol which is
recycled back to the feed. Taking into consideration stream results from the first distillation
column and pressure drop though the valve the feed characteristics of the second column were
the following:
Table 41. Flow rates of compounds to the second distillation column.
DME (kmol/hr) 0.4284276

Water (kmol/hr) 550.9605
Methanol (kmol/hr) 305.4806
Total Flow (kmol/hr) 856.8695
The output temperature and pressure from the DME column were 152 oC and 10.2 bar
respectively. To achieve desirable operation pressure of the second column 1 bar a valve was
installed which decreased pressure inside of the pipe till 1.25 bar and temperature till
84.15°C. Also the pressure drop inside the column was specified to be 0.01 bar. Taking into
account low operation pressure and that the process flows in liquid phase the thermodynamic
model was chosen to be NRTL.
Using the Design specification in Aspen plus desirable purity was defined 0.001 for methanol
in the bottom steam and 0.005 for water in the distillate stream and as a result Reflux ratio
and Distillate rate was calculated automatically: 1.16 and 299.17 kmol/hr respectively.
51
Column design
The optimization process was made in “equilibrium” model, which refers to ideal conditions
and to run the simulation for real state “rate-based” model was chosen.
As it was mentioned earlier the efficiency of the column was determined as 70% andthe real
number of stages was calculated to be 36. To check if achieved results satisfy the restrictions
in Table 31 the following parameters were recorded:
Table 42. Base design specification of column and tray for Methanol column.
Theoretical number of stages 25

Real number of stages 36
Feed tray 17
Diameter 2.28 m
Height 20.83 m
Weir height 0.050800 m
Weir loading 0.044 m2/s
DC velocity 0.017800 m/s
DC backup 0.12757 m
The results from Table 42 showed that the design of the methanol distillation column satisfies
the requirements.
Condenser specifications
Figure 31. Total condenser temperatures.

The flow in condenser is counter-current and cooling water enters at 1 bar. According to
Aspen Plus results heat duty of the condenser is 6427712 W and heat transfer coefficient was
assumed to be 500 W/m2K.
Considering cp=4.18 kJ/kg*K and the following data was calculated:
Table 43. Condenser results
∆Tm 26.8 K
52
Ac 478.89 m2
Mw 206560 kg/hr
Reboiler specifications
Figure 32. Kettle reboiler temperatures.

Kettle reboiler for the second distillation column uses the same steam as DME column: 160
0
C at 6 bar, assumed latent heat of vaporization is 2085.03 kJ/kg and the reboiler duty is
4901 kW basing on the Aspen Plus results.
Table 44. Reboiler results.
Ar 118 m2
Mv 8462 kg/hr
Reflux Drum and Sump

The same assumptions which were made for the DME separation column were used:
Table 45. Reflux drum and sump characteristics.
Volume flow rate H (m)

Hydraulics Volume (m3) D (m)
(m3/min)
Reflux drum 0.46 4.6 1.80 3.6
Sump 0.18 1.81 1.32 2.64
Aspen Plus simulation

Previously, simulation was made using “equilibrium” model and this section will consider the
“rate-based” model. Firstly, the optimal feed tray was obtained basing on minimal reboiler
duty and it is equal to 25:
53
5400
5350
Reboiler duty (kW)
5300
5250
5200
5150
22 23 24 25 26 27 28
Feed tray
Figure 33. Optimal feed tray 25 for Number of trays 36

Also the temperature profile was plotted and it can be clearly seen that with increase of
number of trace the temperature rises.
110
100
90
Temperature
80
70
60
50
40
0 3 6 9 12 15 18 21 24 27 30 33 36
Number of trays
Figure 34. Temperature profile of distillation column

Composition profile for methanol and water was plotted and as it was expected the liquid
fraction of methanol is decreased with number of trays increase and vice versa behavior for
water compound (Figure 35).
54
1
0.8
0.6
Composition
Water
0.4
Methanol
0.2
0
0 6 12 18 24 30 36
Number of trays
Figure 35. Composition profile

Finally, the efficiency of trays was checked and it can be noticed that they are working lower
than at 67% of their potential therefore the initial assumption than efficiency is equal to 70%
was justified.
0.7
0.65
0.6
Efficiency
0.55
0.5
0.45
0.4
1 3 5 7 9 11 13 15 17 19 21 23 25 27 29 31 33 35
Number of trays
Figure 36. Tray efficiency
Table 46. Stream results from Methanol column.
FEED BOTT DIST

Substream:
MIXED
Mole Flow
kmol/hr
DIMET-01 0.550126 2.88E-10 0.550126
55
WATER 551.0733 549.5774 1.495902
METHA-01 297.6831 0.550126 297.133
Mole Frac
DIMET-01 0.000648 5.24E-13 0.001839
WATER 0.648851 0.999 0.005
METHA-01 0.350501 0.001 0.993161
Total Flow
kmol/hr 849.3065 550.1275 299.179
Total Flow kg/hr 19491.49 9918.418 9573.075
Total Flow l/min 84301.99 181.2908 212.6138
Temperature C 85.13932 105.5809 59.60644
Pressure bar 1.25 1.24 1
Vapor Frac 0.249087 0 0
Liquid Frac 0.750913 1 1
Solid Frac 0 0 0
Enthalpy cal/mol -60945.5 -66750.5 -56160.3
Enthalpy cal/gm -2655.59 -3702.33 -1755.13
Enthalpy cal/sec -1.4E+07 -1E+07 -4667200
Entropy cal/mol-K -34.8937 -34.5657 -54.7676
Entropy cal/gm-K -1.52043 -1.9172 -1.7116
Density mol/cc 0.000168 0.050575 0.023452
Density gm/cc 0.003854 0.911833 0.750428
Average MW 22.94989 18.02931 31.99782
Liq Vol 60F l/min 366.5406 165.701 200.8396
The simulation was finished and desired results were obtained: Methanol in distillate stream
with high purity (99%) and water in bottom stream with 99% purity.
Cost analysis.
Table 47. Cost comparison
Rate
Model Equilibrium
Based
Column
Tray number 25 36
Feed tray 17 25
ID (m) 2.28 2.08
H (m) 20.83 20.83
Reflux Ratio 1.11163196 1.17162028
Reboiler
Qr (kW) 4901 5264
Ar (m2) 118 142
mvapor (kg/hr) 8462 9088
Condenser
Qc (kW) 6427 6611
Ac (m2) 479 335
mwater (kg/hr) 206560 212450
Cost
Capital Cost ($ millions) 2.03 2.28
56
Energy Cost ($ millions) 1.32 1.31
TAC ($ millions) 1.97 2.07
From the Table 40 it can be clearly seen that the rate-based model gives slightly differ results
because of the real assumptions but nevertheless the obtained results are close to each other.
3. Design of Secondary units
All pumps used in this project assumed to be centrifugal and for centrifugal pump typical
efficiency is taken in 60-85% range. Shaft power of pumps was calculated from liquid flow
rates that were obtained by Aspen simulation. Moreover, pump power also depends on
differential pressure and liquid viscosity, density and motor efficiency.
Q∗ρ∗g∗h
P h=
3.6∗106
Ph
Ps =
η
h – taken from Figure C1.
Plant is expecting to have two major storage tanks, for produced DME before it will be
transported, and methanol storage tank. Liquids usually stored in vertical cylindrical steel
tank, and that tanks are assumed to be filled only for 5/6 and Radius = Height. Assuming that
storage tank for DME will be designed to keep product for couple of days, and volume flow
rate of DME from distillation column is 978 m3/day, rough size estimation of DME storage
tank was done. The same procedure performed for Methanol storage tank that should supply
1075 m3/day of methanol. It was decided to have two tanks to store weekly capacity of
methanol. All design specification results are shown in Table 48.
V =π R2∗H
Installation cost of pumps was calculated by the following equation:
C e =6900+206 S 0.9
C=F l∗∑ C e
S - the flow rate, l/s
Ce - purchased cost
C – capital cost
Lang Factors for pumps is 4 (Sinnott & Towler, 2011)
57
Storage tanks and mixer were calculated by Equation for vessels, but material factor was
taken as 2.25.
Table 48. Secondary Unit Specifications
SECONDARY EQUIPMENT
Pumps Flow rate [L/s] Ps [kW] Efficiency (%) Cost
Feed pump 16 3,51 70 37592
Fresh water pump 24 6,23 70 41992
DME reflux pump 11,3 3,16 60 34904
DME reboiler pump 7,56 2,69 60 32688
Methanol reflux pump 3,63 0,67 70 30228
Methanol reboiler pump 3,02 0,58 70 29828
Storage Tanks D [m] H [m] Capacity [m3]
DME 14 6,7 2000 1830206
Methanol 11 5,3 3800 (x2) 1167823
Mixer D [m] H [m] Residence time
Feed and recycle mixer 1,95 4 10 min 198517
4. Economic Analysis
¿ Capital Investment=ISBL+OSBL+ Engineering Costs+Contingency
ISBL, inside battery limits is the cost of the plant itself. OBSL is known as off-site costs, and
can be taken as 40% of ISBL as an initial estimate. Engineering costs, which are
administrative charges, construction supervision, inspection and other, assumed to be equal to
the 10% of ISBL+OSBL. Contingency is extra costs that were added to project budget in
order to allow variation from the cost estimate. It will help to cover change in project scope,
changes in price, labour disputes and other unexpected results.
Table 49. Manufacturing Capital Cost
EQUIPMENT COST
Item ID Equipment Name Quantity Total Cost ($)
V-1 Methanol Storage Tank 2 2335646
58
V-2 DME Reflux Drum 1 206951
V-3 Methanol Reflux Drum 1 123490
V-4 DME Storage Tank 1 1830206
M-1 Recyle and Feed Mixer 1 198517
M-2 Mixer of fresh water 1 242806
Reactor preparation
1EXCH 1 107887,12
preheater
2EXCH Steam generation heater 1 93770,27
3EXCH Seperator feed condenser 1 47804,39
HEATER Reactor preperation heater 1 2341693,93
E-1 DME tower condenser 1 625384
E-2 DME tower reboiler 1 1622890
E-3 Methanol tower condenser 1 868931,94
E-4 Methanol tower reboiler 1 425685,5376
P-1 FEED Pump 2 75184
P-2 Fresh water Pump 2 83984
P-3 DME Reflux Pump 2 69808
P-4 DME reboiler Pump 2 65376
P-5 Methanol Reflux Pump 2 60456
P-4 Methanol reboiler Pump 2 59656
T-1 DME Tower 1 880811
T-2 Methanol Tower 1 739390,82
F-1 Flash Drum 1 4854922,3
R-1 Reactor 1 15896,19
Total Equipment and Installation Cost (ISBL) 16 371 682,02
Off-site costs (OSBL) 6 548 673
Engineering Costs 22 922 036
Contingency Charges 22 922 036
FIXED CAPITAL INVESTMENT (FCI) 27 504 426
Table 50. Working Capital, Fixed and Variable costs of Production
WORKING CAPITAL Cost ($/year) Definition

Raw Material
61 970 927
Inventory
Utilities
Water 2504244 0.72 $/GJ
59
Steam 215165 7.78 $/GJ, LP steam
Fixed cost of
production
Maintenance 818584 5% of ISBL
Taxes and Insurance 163716 1% of ISBL
Rent of land 229203 2% of ISBL+OSBL
Labor cost 460800 20 $/h per worker
Price of DME is 1$/kg

kg
∗24 hr
hr
∗333 days
$ day
Revenue=1 ∗25330 =202,437,360 $/ year
kg year
Price of Methanol is 0.22$/kg,
$
∗35246 kg
kg
∗24 hr
hr
∗333 days
day
Raw material=0.22 =61,970,927 $ / y ear
year
Labor cost.
NOL=(6.29+31.7 p+0.23 Nnp) 0.5
Nnp=1 reactor+2 columns+4 heat exchangers = 7
NOL=(6.29+0.23x7)0.5=2.81 (KLM, 2014).
As it was mentioned, total operation hour of plant 8000hr. If worker works 8 hours a day 6
days a week and 48 weeks a year, therefore working hour of a worker is 2304 hr/year.
Working hour of a worker in a year=8hours/dayx6days/weekx48weeks/year=2304 h/year
Number of workers= ( 8000

2304 )
x 2.81=9.75=10
Assuming salary is 20.00$/h , Labor Cost will be 380160$/year.

NET PROFIT =Revenue−CCOP−taxes
CCOP is the sum of fixed and variable cost. 15% taxes are applied in Kazakhstan for large
projects.
As a result, Net Profit = 105 709 117 $/year.
60
5. Process Control and Safety Analysis
Safety and process control is the most important study for plant maintenance and therefore
this chapter will cover the possible danger occurred during the plant operation, measures
which can be applied to avoid it, storage conditions of chemicals and HAZOP analysis made
for DME plant to cover possible scenarios of hazard appearance.
There are several types of incidents which can be occurred at the chemical plant:
- Fire and explosion
- Toxic release
- Corrosion
Table 51. Types of incidents (Crowl, 2011, p. 15)
Incident probability Fatalities occurrence

Fire low Intermediate
Explosion Intermediate high
Toxic release low Low
7.1 Fire and explosion

As it was mentioned earlier potential accidents which can be occurred in a chemical plant are
fires and explosions. There are three main components for combustion: source of ignition,
fuel and oxidizing agent (Crowl, 2011, p. 240). Another possible scenario is explosion which
can be occurred from rapid oxidation reaction releasing huge amount of energy and gases
(ibid., p. 243).
The DME plant has a reactor which runs at high temperature (255-390 °C) and to avoid
explosions as well as fire occurrence safety regulations must be applied.
The first factor which will help to avoid incidence is absence of source of ignition near to hot
surfaces (reactor, heat exchanger, distillation columns). The second is installation of valves
and controllers to equipment so that in case of wrong equipment operation it could
automatically detect and fix the problem (more detailed in Chapter 7). The third is provision
of proper ventilation system. Hopefully, dimethyl processing plant is an open-air plant and
therefore all explosive vapors which can be formed around the plant are diluted and cannot
bring any harm (Crowl, 2011, pp. 360-361). Finally, it is very important to have a well-trained
personnel who is aware about the potential dangerous from the DME processing and will
immediately take actions in case of accident occurrence.
61
7.2 Toxicity and storage conditions
Workers on the plant must be aware about toxicology of chemicals used at the process.
According to the search dimethyl ether and methanol in low amounts are not harmful for
people (Hazardous substance fact sheet, 2002, p. 1). Nevertheless, chemicals can enter the
human body by inhalation via mouth and nose or penetrate an organism by skin. The best
option to avoid penetration of chemicals into a human body is to wear protective clothes and
additionally, to provide appropriate ventilation conditions for the plant.
Product and reactants of dimethyl ether plant are stored in vessels covered by stainless steel.
Both methanol and dimethyl ether are volatile liquids and therefore during the storage in the
tanks they form vapors which are in equilibrium with liquid phase. When the liquid is pumped
into the storage vessel by a tanker truck and goes up the vapor is collected by this truck and
recycled (Thomas, 2014). Even though the vessels are closed the issue regarding the chemical
leakage can be raised.
Storage regulation of substances can be affected by weather conditions such as wind speed
and temperature. It should be noticed that the plant is located at the Western Kazakhstan
which stands out with its sharply continental climate, low amount of sedimentation and
average temperature -7 °C on winter and +27 °C at summer time (OrexCa, 2003). In
Mangystau region, which is the potential location of DME plant, the speed of wind is not high
(approximately 2-6 m/s) and therefore vapors of chemical which can be released from storage
tanks are stagnant and there is a high concentration of them. But taking into account that the
sun heats the ground and the temperature near the ground is higher than in upper layers of
atmosphere there is a constant buoyancy effect due to the air density difference and vapors of
chemicals are not concentrated near the storage vessels (Crowl, 2011, p. 181-185).
7.3 Corrosion
Initially, to make dimethyl ether processing plant cheaper the working material was chosen to
be carbon steel. However, after exploring the corrosive properties of water and methanol the
carbon steel was replaced by stainless steel for reactor and two distillation columns to make
process safe (TheyDiffer, 2014).
There are several types of corrosion which can affect the stainless steel:
Pitting corrosion. Passive layer created by stainless steel can be damaged by chloride ions but
taking into account that there is no chemical species with chloride involving in the process no
pitting corrosion will be occurred.
62
General corrosion. Passive layer may be broken by hydrochloric and sulfuric acids but during
the DME synthesis those acids are not used therefore such type of corrosion is not typical for
the process.
Galvanic corrosion. This type of corrosion may occur if stainless steel is in contact with
another metal via electrolyte acting as a “sacrificial anode”. However, galvanic corrosion may
be avoided if metals are separated by non-metallic insulator (British stainless steel
association, 2016).
Finally, stainless steel are not affected to rust therefore the dimethyl processing plant can be
considered to be protected from corrosion damage.
Carbon and stainless steel are both metal alloys, where carbon steel is a mixture of carbon
with steel while stainless steel is made of chromium and steel. Stainless steel is less corrosive
in contrast to other materials (ibid).
Table 52. Comparison chart of properties for carbon steel and stainless steel.
Carbon steel Stainless steel

Affected to be rusted No
Hard Softer
Brittle No
7.4 Hazards and operability studies (HAZOP)

HAZOP study is a process which is used to recognize the danger in a chemical processing
plant (Crowl, 2011, p.510). Table 53 provides explanation of the guide words used during the
HAZOP study which will be used later to define possible hazard from DME plant.
Table 53. Guide words used for the HAZOP Procedure (Crowl, 2011, p. 511).
Guide words Meaning Comments

No, not, none The complete negation of the No part of the design
intention intention is achieved, bit
nothing else happens.
More, higher, greater Quantitative increase Applies to quantities such as
flow rate and temperature and
to activities such as heating
and reaction.
Less, lower Quantitative decrease
As well as Qualitative increase All the design and operating
intentions are achieved along
with some additional activity,
63
such as contamination of
process streams.
Part of Qualitative decrease Only some of the design
intentions are achieved, some
are not.
Reverse The logical opposite of Most applicable to activities
such as flow or chemical
reaction. Also applicable to
substances, for example,
poison instead of antidote.
Other than Complete substitution No part of the original
intention is achieved – the
original intention is replaced
by something else.
Sooner than Too early or in the wrong Applies to process steps or
order actions.
Later than Too late or in the wrong
order
Where else In additional locations Applies to process location,
or locations in operating
procedures.
There are different parameters which can be combined with guide words and for the dimethyl
ether production plant the flow into reactor and purity will be analyzed.
Table 54 HAZOP for heat exchanger
Guide word Deviation Possible causes Possible Actions

consequences required
Less Less flow rate of Pipe blockage Temperature of High
cooling water hot stream temperature
stream remains constant alarm, adjust
temperature
controller
More More cooling Breakdown of Temperature of Low
flow rate cooling water outlet process temperature
valve fluid decrease alarm, adjust
temperature
controller
More More pressure Failure of Bursting of tube Set high
on tube side process fluid pressure alarm
valve
Contamination Contamination Leakage of tube Contamination Proper
of process fluid and cooling of process fluid maintenance
line water goes in and operator
alert
Corrosion Corrosion of Hardness of Less cooling Proper
tube technical water water and maintenance
64
fracture of tube
NONE No cooling water Breakdown of Hot stream Set
flow inlet cooling temperature is temperature
water valve to not lowered controllers at
open inlet and outlet
of hot stream
MORE More cooling Breakdown of Hot stream outlet Set
water flow rate inlet cooling temperature too temperature
water valve to low controllers at
close inlet and outlet
of hot stream
LESS Less cooling Pipe leakage Process fluid Install flow
water temperature is meter
too low
REVERSE Reverse flow Breakdown of Product off set Install flow
direction of process fluid controller
process fluid inlet valve
Contamination Contamination Contamination Output Proper
in process fluid in cooling water temperature is maintenance
too low and operator
alert
Table 55. HAZAOP study for DME reactor
Process Deviations Possible causes Possible Action required

parameter (guide words) consequences
Flow No Valve or pump Production rate Automatic
are closed; is decreased valves and
Pipe is pumps;
damaged; Pipeline repair
No methanol works;
supply. Maintenance of
methanol level
More Valve is opened Explosion; Automatic
to much Increase amount valves
of methanol in
recycle stream
Less Valve is opened Production rate Automatic
too low; is decreased; valves;
Methanol is Feed Temperature
poor recovered temperature is controllers
from the 2nd increased
distillation
column
Impurities in As well as Feed methanol Conversion is Purity control of
feed & water is defective; decreased; chemicals;
in recycle Disorder of Quality of DME Constant
stream distillation is decreased; maintenance of
column; pipeline.
65
Pipe corrosion.
Flow Reverse High backup Production rate Check valve
pressure is decreased installation
Liquid enters Where else Connection of Explosion Pre-check and
vapor phase pipes with supervision
feed equipment is
wrong
Table 56. HAZOP analysis for Distillation column
Process Deviations Possible causes Possible Action required

parameter (guide words) consequences
Flow to the 2nd no DME column Flowrate is Automatic
distillation damage; decreased; valve;
column Pipe is blocked; Pipeline
Valve is closed; maintenance
less Pipeline is Level in column Installation of

blocked; is decreased; check valves
Feed T to
column is
increased.
more High pressure Flooding in Installation of
from the 1st distillation bypass line
column column
Level low Leakage; Level in the Check Level
Pipe is blocked column is Controller;
decreased; Pipe
high Output stream is Level in the maintenance
blocked column is
increased;
Overpressure in
the reflux drum
Temperature low High flowrate in Specification of Constant
heat-exchanger. the products is supervision of
changed. valve and
high Valve before the Products in temperature
2nd DC does not vapor phase; controllers
work; Explosion
Low flowrate in
Heat-exchanger
7.5 Sustainability of the plant.

Sustainability study is an integral part of chemical engineering industry as all performance
made by the processing plant affects the human’s life. Therefore it is very important to take
into consideration aspects such as waste treatment, energy consumption, in-site recycle, safe
storage and release to atmosphere.
66
The purpose of DME production plant was not only to achieve a highly pure product but also
to make sure that its process will not harm the environment. To achieve this goal the whole
DME plant was optimized by decrease of the cost which in its turn lead to reduction of energy
consumption. Additionally, the process was focused to minimize the waste generation and
therefore, produced methanol was separated and recycled back to the feed, while produced
water was with high purity and can be sent to water treatment facility.
Heat integration of the process was also upgraded so that the plant could consume less energy
and release less carbon dioxide emissions to the atmosphere.
However, there is one of arguable issues regarding the storage conditions of the chemicals.
Both methanol and dimethyl ether are volatile liquids but with right approach of their use as it
was describe in Chapter 7.2 no emissions will be to the atmosphere.
7.6 Process control

The operation of DME plant requires the presence of controllers around the equipment
(mixer, cooling tower, heat exchanger, pumps, and distillation columns).
1600
1400
1200
1000
DME
Flowrate(kmol/hr)
800 Water
Recycle
600 Feed
Stream 1
400
200
0
0 1 2 3 4 5 6 7 8 9
Operating time (hours)
Figure 37. Flow rate +10%
67
1
0.99
0.98
DME Water
0.97
Recycle
0.96
Purity
0.95
0.94
0.93
0.92
0 1 2 3 4 5 6 7 8 9
Operation time (hours)
Figure 38. Purity +10%
14000
12000
mass flowrate (kg/hr), P(bar), T(°C)
10000
8000
Fresh-W Fm (kg/hr)
6000 Steam Fm (kg/hr)
Steam P (bar)
Steam T (C)
4000
2000
0
0 1 2 3 4 5 6 7 8
Figure 39. Steam characteristic for +10%
68
410
390
370
350
Stream 1 Stream 2
Temperature(°C)
330
310
290
270
250
0 1 2 3 4 5 6 7 8
Figure 40.Temperature around the reactor for +10%

Process control section is used to simulate real life conditions, when the system can work in
non-ideal conditions and the parameters will vary. The controllers were added and the
simulation was done in Aspen Dynamics. The controllers’ function was to return the system
back to operational conditions and prevent from unexpected and undesired consequences. For
safe and proper maintenance of the DME production plant it is necessary to install controllers
around the units (distillation columns, reactor, heat-exchangers and mixers). Dimethyl ether
processing plant requires installation of the following controllers: level, flowrate, temperature
and pressure controllers.
So that there is one level controller around the mixer where fresh methanol is mixed with
recycled, another level controller is installed around the mixer where fresh water is supplied.
Also, level controllers are put around reflux drum and distillation units for the first and the
second columns. There is one temperature controller after heater and one is around the third
heat-exchanger. Also temperature controllers are installed along the distillation column and
reboiler. One Flowrate controller is installed before the first heat-exchanger and another
flowrate controller is put after the mixer where fresh water is supplied. Finally, the pressure
controllers are installed around the condenser of both distillation columns.
To check if the controllers are installed correctly and can react at any disturbances the
following parameters where changed and the behavior of plant response was observed. 3 main
realistic scenarios were simulated in the software. Sudden increase of feed by 10% and feed
drop by 10% that may result from feed pump failure. Third scenario assumed the catalyst
deactivation by 10% that may be caused by extreme temperature increase and further
69
deactivation. The 10% increase situation is discussed in that part; other 2 cases are listed in
the appendix.
Figure 1 shows that DME and water products purity is not affected from the disturbance. The
decrease of methanol recycle is not so important, as main products are still pure. Figure 2
shows the change in flowrates of main streams. Product streams are slightly increased, but as
purity is same, the product flowrate increase is not a concern. Figure 3 shows that the amount
of fresh water usage has increased that would lead to higher operational costs. Figure 4,
showing the temperature at inlet and outlet of the reactor slight decrease of the temperature
that was neglected in 3-hour time.
Summing up, the controllers allowed the reactor inlet and outlet temperature to return back to
operating conditions and the main outcomes of the feed increase were observed from
Dynamic simulation.
70
6. Plant Layout
DME processing plant can be schematically represented as it is shown at Figure 41. It
involves the following facilities:
- DME and methanol storage zone where chemicals are kept on the safe distance from
the crowded places;
- Raw material and equipment storage where catalyst and different equipment stored;
- Industrial zone where the DME process is running;
- Waste water treatment where by-product water is cleaned;
- Control room where the personnel constantly supervising the industrial zone;
- Workshop where equipment is repaired and checked;
- Firefighting room where all necessary equipment and facilities against fire are stored;
- Medical center where first aid and medical check-up can be offered;
- Administrative center where the engineers and staff are working;
- Canteen and living room for none-local employees;
- Parking zone to leave the transport.
71
st nd
D1 – 1 Distillation column D2 – 2 Distillation column R - Reactor
Figure 41. Schematic plant layout
7. Conclusion
During the Capstone II project reactor, distillation columns, and heat exchanger system
were designed separately, on the basis of the preliminary mass balance obtained from
the Capstone I. By theoretical assumptions 80% of maximum conversion was decided to
be used leading to 0.66 conversion in the reactor and the units were designed and
optimized on that initial mass balance.
However, when all units were optimized basing on the economic evaluation it was
decided to optimize the whole process to maximally decrease the cost of installation and
maintenance of the DME plant.
The optimization process was repeated for four different conversions (80%, 90%, 95%
& 98%) and economic analysis showed that conversion of 0.7822, matching to 95% of
72
maximum conversion is the best choice. Therefore all further calculations were done
basing on that conversion. To make comparison calculations for 80%, 90% and 98% of
maximum conversion cases were listed in appendix. As a part of Capstone II project,
detailed economic analysis, material and energy balance were done and the safety study
was conducted focusing on each unit in details. Controllers were installed around the
plant to provide a process control that was simulated using Aspen Dynamics. Looking
for a realistic scenario, feed input was changed by 10% higher and lower conditions. The
process control efficiently eliminated the fluctuations during a short period of time.
Moreover, the scenario of catalyst deactivation was investigated and the outcomes were
observed. Summing up it can be said that the process of dimethyl ether was designed
and optimized considering economical side and moreover, it has a great potential to
become a sustainable plant which will not harm the environment by providing clean
biofuel and releasing low amount of pollution.
73
8. Appendix A
Matlab code for reactor volume calculation
X=0:0.02:0.8247
T=(X+1.6412)/0.0066+273 %1.7732 for 270 Tin, 1.6412 for 250 tin
ks=5.35*10^13*exp(-17280./T)
km=5.39*10^(-4)*exp(8487./T)
kw=8.47*10^(-2)*exp(5070./T)
k=exp((-9.76)+3200./T+(1.07)*log(T)+(-6.57)*(0.0001).*T+(4.9)*0.00000001.*T.^2+(6050)./T.^2)
ra=1./(ks.*km.^2.*((1-X).^2.*0.3322^2-(X.^2.*0.3322^2)/(4.*k))./((1+2.*((km.*(1-X).*0.3322).^(0.5))
+kw.*X.*0.3322/2).^4))
B=trapz(X,ra)
C=(2*1100*(2-0.8247)*B/(0.4*1285))^0.5
74
9. Appendix B
Table B57 TEMA sheet of first heat exchanger
75
Table B58 TEMA sheet of second heat exchanger
76
Table B 59 TEMA sheet of third heat exchanger
77
10. Appendix C
Figure A 1. Centrifugal pump efficiency (Sinnott & Towler, 2011)
Table A. 1. Stream results of DME tower for 95% conversion (Rate Based model)
BOTTO DISTILLAT
Component Mole Flow FEED M E
KMOL/H 551,073
WATER R 3 551,0733 1,27E-05
KMOL/H 298,233
METHA-01 R 3 297,6831 0,550252
KMOL/H 550,126
DIMET-01 R 3 0,424591 549,7018
Component Mole Fraction
0,39378
WATER 3 0,648947 2,31E-08
METHA-01 0,21311 0,350553 0,001
0,39310
DIMET-01 7 0,0005 0,999
KMOL/H 1399,43
Mole Flow R 3 849,181 550,252
44827,5
Mass Flow KG/HR 7 19485,71 25341,86
999,715
Volume Flow L/MIN 2 448,4894 679,2302
Temperature C 44 152,0204 44,44
Pressure BAR 10,4 10,29 10
78
Vapor Fraction 0 0 0
Liquid Fraction 1 1 1
Solid Fraction 0 0 0
-
Molar Enthalpy CAL/MOL 57683,8 -61589,6 -48019,74
-
Mass Enthalpy CAL/GM 1800,78 -2684,06 -1042,66
-
Enthalpy Flow CAL/SEC 2,2E+07 -1,5E+07 -7339700
CAL/MOL -
Molar Entropy -K 54,2288 -37,2016 -74,06857
CAL/GM- -
Mass Entropy K 1,69292 -1,62123 -1,608263
0,02333
Molar Density MOL/CC 1 0,031557 0,0135018
0,74733
Mass Density GM/CC 9 0,724124 0,6218281
Average Molecular 32,0326
Weight 7 22,94647 46,05501
Table A. 2. DME Tower specification for different conversions
Conversion 80% 90% 98%

Column ($) 580789,4 795394,9 758793,1
NT 15 22 22
real trays 21 31 31
feed tray 9 11 11
D (m) 2,22 2,18 2,09
H (m) 12,192 18,288 18,288
Trays ($) 59254,11 88100,18 82267,47
Condenser
844085 868711,2 855868,5
($)
Duty kW -3682,89 -3.849 -3.762
Area 532,3157 556,3953 543,7912
Reboiller
1750758 1998531 2523791
($)
Duty kW 6957,848 6420 5897
Area (m2) 1039,726 1274 1825,024
CAPEX ($) 3234887 3750737 4220720
OPEX ($) 1635372 1518294 1399243
TAC ($) 2713667 2768539 2806149
79
0.95
0.9
0.85
Efficiency %
0.8
0.75
0.7
0 5 10 15 20 25 30
Stage
Figure C1. Tray Efficiency profile for DME distillation column

10,04
-3,0
Controller Output MMkcal/hr
Process Variable bar
10,02
-3,1
Set Point bar
10,0
-3,2
9,98
-3,3
9,96
0,0 0,2 0,4 0,6 0,8 1,0 1,2 1,4 1,6 1,8 2,0
Time Hours
Figure C2. DME pressure control (PC) response for 10% change
80
24000,0 26000,0
2,91
Controller Output kg/hr

Process Variable m
Set Point m
2,89 2,9
0,0 0,3 0,6 0,9 1,2 1,5 1,8

Time Hours
Figure C3. DME tower drum level controller performance
Controller Output MMkcal/hr
5,5
Process Variable C
121,0
Set Point C
5,0
116,0 118,5
0,0 0,5 1,0 1,5 2,0

Time Hours
Figure C4. Stage 14 temperature controller for DME Tower
Table A. 3. Material factors for pressure vessels (Dimian, 2003)
Shell material Carbon steel Stainless steel Monel Titanium

Fm (solid) 1 3.67 6.34 7.89
Table A. 4. Material, design and pressure correction factors for heat-exchangers

(Dimian, 2003)
Shell/ CS CS CS CS SS Monel CS
Tubes CS Brass Monel SS SS Monel Titanium
Fm 1.0 1.3 2.15 2.81 3.75 4.25 8.95
81
Fixed-tube
Design type Kettle Floating U-tube
sheet
Fd 1.35 1 0.85 0.80
Pressure (bar) <10 20 30 60
Fp 0 0.1 0.25 0.52
82
11. Appendix D
2696000
2694000
2692000
2690000
2688000
2686000
TAC($/year)
2684000
2682000
2680000
2678000
2676000
2674000
25 26 27 28 29 30 31 32 33 34 35
Number of trays
83
1980000
1960000
1940000
1920000
TAC($/year)
1900000
1880000
1860000
1840000
1820000
25 26 27 28 29 30 31 32
Number of stages
84
1530000
1520000
1510000
1500000
1490000
TAC($/year)
1480000
1470000
1460000
1450000
1440000
20 21 22 23 24 25 26 27 28 29 30 31 32
Number of stages
Table 60. Finding an optimal feed tray for Number of stages 25.
Feed tray Qreb (kW)

3619.98720
15 6
3548.89833
16 1
3521.96931
17 9
3550.95658
18 3
3670.24581
19 3
Table 61. Cost estimation for the column.
NT D (m) H (m) Capex ($)

21 2.41 17.40 764767.50
23 2.31 19.11 789675.65
24 2.30 19.97 813185.12
85
25 2.28 20.83 836415.43
26 2.27 21.69 860582.55
27 2.18 22.54 848687.64
29 2.10 23.40 839608.47
Table 62. Cost estimation for trays.
NT Capex ($)
21 76916.62
23 79142.82
24 81897.87
25 84635.03
26 87533.62
27 85141.73
29 83221.18
Table 63. Cost estimation for condenser.
N ΔTm Qcon (W) U A Capex ($)

T (K) (W/m2K) (m2)
2 6717916. 500 501.3 1115127.20
26.80
1 13 4
2 6566080. 489.3
26.80 500 1097677.27
3 69 2
2 6494620. 484.6
26.80 500 1090892.30
4 26 7
2 6427711. 478.8
26.80 500 1082418.30
5 64 9
2 6379485. 476.0
26.80 500 1078282.67
6 86 8
2 6588856. 491.7
26.80 500 1101155.08
7 99 1
2 6775750. 471.5
26.80 500 1071525.31
9 67 0
Table 64. Cost estimation for reboiler.
N ΔTm Qreb (W) U A CAPEX($)

T (K) (W/m2K) (m2)
2 74.55 5165589.3 500 138.5 588496.81
1 2 8
2 5033077.8 120.8
74.52 500 538312.20
3 8 2
2 4964613.4 134.1
74.49 500 576278.07
4 8 8
2 4900684.5 118.0
74.35 500 530271.47
5 2 6
86
2 4855412.3 131.2
74.21 500 568006.79
6 2 3
2 4981445.4 116.2
74.12 500 524853.01
7 6 1
2 5171262.7 115.7
73.91 500 523536.90
9 6 6
Table 65. Operating cost for condenser.
NT cost of steam ($/GJ) hour/yea Qreb OPEX total

rs (GJ/hr) ($/year)
21 7.78 8000 18.60 1157415.04
23 7.78 8000 18.12 1127731.56
24 7.78 8000 17.87 1112391.16
25 7.78 8000 17.64 1098066.98
26 7.78 8000 17.48 1087923.11
27 7.78 8000 17.93 1116162.37
29 7.78 8000 18.62 1158722.08
Table 66. Operating costs for reboiler.
N cost of water ($/GJ) hour/year Qcon total

T s (GJ/hr) ($/year)
21 0.72 8000 24.18 139299.84
23 0.72 8000 23.64 136154.25
24 0.72 8000 23.38 134672.45
25 0.72 8000 23.14 133285.03
26 0.72 8000 22.97 132285.02
27 0.72 8000 22.64 130405.82
29 0.72 8000 24.39 140503.68
Table 67. Total annual cost for the whole distillation column
Capex ($) Payback Tac ($/yr) NT

(year)
2545308.13 3 2145150.9 21
2
2098821.7
2504807.94 3 23
9
2101148.0
2562253.36 3 24
6
2075932.0
2533740.24 3 25
9
2085010.0
2594405.63 3 26
0
2099847.3
2559837.46 3 27
4
2517891.87 3 2138523.0 28
87
5
12. Appendix E
Stream Results
2 5 7 11 111 222 333

Substream:
MIXED
Mole Flow
kmol/hr
550.982 550.982 550.982 550.982 4440.67
WATER 8 2 2 1.53412 2 1.53412 5
305.968 305.417 305.967 1404.86 305.967 1404.86
METHA-01 1 1 1 7 1 7 0
549.877 549.876 549.876
DIMET-01 2 0.42841 5 0.42841 5 0.42841 0
Mole Frac
0.39164 0.64304 0.39164 0.39164
WATER 9 9 9 0.00109 9 0.00109 1
0.21748 0.35645 0.21748 0.99860 0.21748 0.99860
METHA-01 8 1 8 5 8 5 0
0.39086 0.39086 0.00030 0.39086 0.00030
DIMET-01 3 0.0005 3 5 3 5 0
Total Flow 1406.82 856.827 1406.82 1406.82 4440.67
kmol/hr 8 7 6 1406.83 6 1406.83 5
19732.0 45062.2 45062.3 45062.2 45062.3
Total Flow kg/hr 45062.3 6 3 5 3 5 80000
83564.9 454.098 27404.1 81056.7 965.803 1440.12
Total Flow l/min 3 1 5 964.904 1 4 6
383.848 150.813 37.1381 159.270 37.7335 92.8332
Temperature C 3 5 110 8 2 2 4
14.9843
Pressure bar 5 10.2 10.4 1 10.4 15 2
0.37403
Vapor Frac 1 0 5 0 1 0 0
0.62596
Liquid Frac 0 1 6 1 0 1 1
Solid Frac 0 0 0 0 0 0 0
- - - - - -
Enthalpy cal/mol 45101.5 61417.2 54115.1 56679.8 48540.2 -56666 67011.2
- - - - - - -
Enthalpy cal/gm 1408.05 2666.93 1689.45 1769.52 1515.41 1769.09 3719.69
88
- - - - - - -
Enthalpy cal/sec 1.8E+07 1.5E+07 2.1E+07 2.2E+07 1.9E+07 2.2E+07 8.3E+07
Entropy cal/mol- - - - - - -
K 25.3117 37.1601 44.6603 -56.498 31.0222 56.4558 35.2183
Entropy cal/gm- - - - - - -
K 0.79022 1.61361 1.39428 1.76385 -0.9685 1.76253 1.95491
0.00028 0.03144 0.00085 0.00028 0.02427 0.05139
Density mol/cc 1 8 6 0.0243 9 7 2
0.00898 0.72422 0.02740 0.77835 0.00926 0.77763 0.92584
Density gm/cc 7 2 6 6 6 2 5
32.0311 32.0311 32.0311 32.0311 32.0311 18.0152
Average MW 4 23.0292 4 4 4 4 8
Liq Vol 60F 1015.08 371.569 1015.08 945.375 1015.08 945.375 1335.90
l/min 3 9 1 5 1 5 3
13. Reference list
Bravo, J. L. and James K. F. Distillation Columns. Chemical Engineering Progress, 19-29.

1990
British stainless steel association. Retrieved from http://www.bssa.org.uk/faq.php?id=9.

Accessed on 18 March, 2016
Crowl, D and Joseph, L. Chemical process safety. Fundamentals with applications. 3rd edition.
Pearson Education International
Dimian, A. (2003) Integrated Design and Simulation of Chemical Processes. Computer-

Aided Chemical Engineering, 13, pp.680-684
Hazardous substance fact sheet. (2002). Retrieved from

http://nj.gov/health/eoh/ rtkweb/documents/fs/0758.pdf. Accessed on 14 October 2015
Lyuben, W. (2011). Principles and Case Studies of Simulation Design. pp. 53-57.
McCabe, W.L., J.C. Smith, P. Harriott. Unit Operations of Chemical Engineering, 5th

Edition, McGraw-Hill. 1993
OrexCa. Western Kazakhstan. About Kazakhstan regions. Retrieved from

http://www.kazakhstan.orexca.com/western_kazakhstan.shtml. Accessed on15 March, 2016
89
Sari, M (2014).General Process Plant Cost Estimating. KLM Technology Group.
Sinnot, R., Towler, G. (2009). Chemical Engineering Design.
Sinnott, R. Chemical Engineering design, 4th Edition, pp. 816-817. Elsevier. 2005
TheyDiffer. Difference between Carbon steel and Stainless steel. Retrieved from
http://theydiffer.com/difference-between-carbon-steel-and-stainless-steel/. Accessed on 20
March, 2016
Thomas, C. Introduction to process technologies. Content Technology Inc. 3rd edition. 2014
90
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Synthesis of Dimethyl Ether: Capstone Ii

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Synthesis of Dimethyl Ether: Capstone Ii

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SYNTHESIS OF DIMETHYL ETHER

Bachelor of Chemical Engineering

SUBMITTED BY: GROUP 7

AIGERIM BAKYTZHANOVA ID 201100705

DINARA GAPEYENKO ID 201101210

RUSLAN MARTEMYANOV ID 201102238

AZAT YERKINOVA ID 201103889

2. MATERIAL AND ENERGY BALANCE 5

3. DESIGN OF PRIMARY EQUIPMENT 12

4. DESIGN OF SECONDARY UNITS 57

6. PROCESS CONTROL AND SAFETY ANALYSIS 60

13. REFERENCE LIST 89

Q – heat transferred per unit time, W

1.1 Capstone I Review

BET surface area 195 m2/g

2. Material and Energy Balance

2.1 Mass Balance

ṁ cold ,∈¿=ṁ cold ,out ¿

Reactor Inlet (kg/h) Outlet (kg/hour)

Table 5. Distillation Columns mass balance

DME IN OUT (kg/hr)

Methanol OUT (kg/hr)

Table 6. Stream specifications of first heat exchanger

First Heat exchanger

Table 7. Stream specifications of second heat exchanger

Second Heat exchanger

Table 8. Stream specifications of third heat exchanger

Third Heat exchanger

Table 9. Stream specifications of flash drum

Table 10. Stream specifications of heater

Table 11. Stream specifications of mixer

2.2 Energy Balance

Table 12. Energy balance for distillation columns

DME Tower IN [kJ/sec] OUT [kJ/sec]

Methanol Tower IN [kJ/sec] OUT [kJ/sec]

Table 13. Energy balance of heat exchangers

Streams Hot stream Cold stream

Table 14. Energy balance of flash drum and mixer

Unit Inlet stream Steam/Fresh water stream Outlet Net

Table 15. Energy balance of heater

Unit Inlet stream Outlet stream Net duty

Process flow diagram

Whole plant flowsheet are represented in Figure 1A with Equipment ID.

METHANOL Tout= 35oC E-1

Figure 1A. Process Flow Diagram

ID V-1 V-2 V-3 V-4 M-1 M-2 1-EXCH 2-EXCH 3-EXCH

3.1 Design of reactor

3.1.1 Reactor kinetics

Table 16. Methanol consumption equilibrium constant coefficients

a b*10-3 c d*104 e*108 f*10-3

Where k=1.55e+07, n=0, E=2542.86 kJ/kmol.

Table 17. Concentration exponents table in Aspen Plus softwaare

Term no.1 Term no.2 Term no.3

The expressed coefficients are K1=1, K2=0.046*exp(4244/T), K3=0,085*exp(5070/T),

3.1.2 Adiabatic temperature calculations

Where H R is heat of reaction,

Figure 2. Comparison of calculated temperature and real temperature versus conversion

¿−Out +Generation= Accumulation

To integrate, reaction rate equation must be dependent only on conversion of Methanol,

Where k s ( X )=5.35∗10 exp ⁡( )

Table 20. Reactor Cost

3.1.5 Optimization and conversion choice

a b10-3 c d104 e108 f10-3

The expressed coefficients are K1=1, K2=0.046exp(4244/T), K3=0,085exp(5070/T),