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Final Report – Design of

Polyester Resin Plant –


Chem Eng 4W04
Submitted to: Dr. M. Saban
Team Magenta
B. Pambianco
A. Ladd
G. Voloshenko
N. Kirupa
S. Neheli
S.Wani

4/6/2011
McMaster University 6 April, 2011
1280 Main Street West
Hamilton, ON
L8S 4L9
To: Dr. M. Saban
From: Team Magenta (B. Pambianco, A. Ladd, G. Voloshenko, N. Kirupa, S. Neheli, S. Wani)
Subject: Design of Polyester Resin Pant

Dear Dr. M. Saban,


As requested in the Chemical Plant Design and Simulation class, please find attached the
final version of the polyester resin plant report. The report studies the production of polyester
resin from dimethyl terephthalate (DMT), and includes an overview of plant setup and
operation, as well as process safety and economics.
Resin production from DMT requires a two-step process. DMT and glycols are first
charged into a 2500 gallon reactor. Transesterification and polycondensation reactions are
then undertaken in high temperature and vacuum conditions. The final product is poly (1,2-
g
propylene-diethylene-terephthalate) resin with a Mn of 6000 mol and an average DP of 95%.
Two 2500 gallon reactors operate in parallel on a 24 hour cycle, offset by 12 hours to allow for
shared use of processing facilities. Plant capacity is 3000 tonnes of resin per year, operating 42
weeks of the year. The plant is located in Sarnia, Ontario.
Alternatives available to the process described in this report are summarized below.

Within this Report Alternative


Process Used Ester Route Acid Route
Number of Reactors Two, Parallel Configuration One
Processing Equipment Cooling Belt Rotoform
Current market price for the resin is $5 per kilogram. Based on this value, cost analyses
were conducted for both this process and a popular alternative, the acid route.

(cost / kg resin) Ester Route Acid Route


Raw Material $2.75 $1.92
Manufacturing $0.65 $0.82
Profit $1.60 $2.26
Capital Investment $11,000,000 $10,000,000
NPV (12 years) $25,400,000 $40,700,000
Based on the conclusions reached within this report, it is recommended that further
development of this project be approved.

Sincerely,
B. Pambianco
Team Magenta

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Contents
1.0 Introduction ...................................................................................................................................... 5
2.0 Process Description ........................................................................................................................... 6
3.0 Work Schedule ........................................................................................................................................ 9
4.0 Process Mass and Energy Balance ........................................................................................................ 10
5.0 Process Control ..................................................................................................................................... 12
5.1 Preliminary P&ID diagram................................................................................................................. 12
5.2 End point control strategy description ............................................................................................. 13
5.3 Vacuum application control strategy ................................................................................................ 14
5.4 Control of major pieces of equipment .............................................................................................. 14
6.0 Reactor Design and Sizing ..................................................................................................................... 15
6.1 Reactor Design .................................................................................................................................. 15
6.2 Ports .................................................................................................................................................. 16
6.3 Agitator System ................................................................................................................................. 17
7.0 Other Equipment Design and Sizing...................................................................................................... 18
7.1 Condensers........................................................................................................................................ 18
7.1.1 Take-Off Condenser ................................................................................................................... 18
7.1.2 Methanol Condensor ................................................................................................................. 18
7.2 Packed Tower .................................................................................................................................... 19
7.3 Vessels............................................................................................................................................... 21
7.3.1 Raw Material Storage................................................................................................................. 21
7.3.2 Receivers .................................................................................................................................... 23
7.3.3 Methanol Storage and Glycol Recycle ....................................................................................... 24
7.3.4 Product Storage Silos ................................................................................................................. 25
7.4 Downstream Equipment ................................................................................................................... 26
7.4.1Cooling belt system ..................................................................................................................... 26
7.4.2 Disintegration equipment .......................................................................................................... 27
7.5 Utility Equipment .............................................................................................................................. 28
7.5.1 Hot Oil Utility.............................................................................................................................. 28
7.5.2 Cooling Tower Utility.................................................................................................................. 30
7.6 Pumps ............................................................................................................................................... 32
8.0 Process Safety ................................................................................................................................. 33

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8.1 Hazardous Conditions ....................................................................................................................... 33
8.2.1 Plant Classification (electrical safety) ........................................................................................ 33
8.2.2 Operational Safety ..................................................................................................................... 33
8.2.3 Thermal Process Safety .............................................................................................................. 35
8.3 Waste Disposal .............................................................................................................................. 35
9.0 Floor Plan .............................................................................................................................................. 36
10.0 Economic Analysis ............................................................................................................................... 37
10.1 Capital Costs, Installation Costs and Expense/Fees ........................................................................ 37
10.2 Operating Costs............................................................................................................................... 40
10.3 Income statement over 12 years accounting period ...................................................................... 41
10.3.1 Sensitivity Analysis on the selling price.................................................................................... 43
10.3.2 Sensitivity Analysis on the raw feed prices .............................................................................. 44
10.4 Acid Route Alternative Analysis ...................................................................................................... 44
11.0 Conclusions/Recommendations ......................................................................................................... 46
12.0 Acknowledgments............................................................................................................................... 47
13.0 References .......................................................................................................................................... 48

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1.0 Introduction

The assigned project for Team Magenta was to design a safe, simple, robust and economical plant
for production of a specialty polyester resin. The team made some initial decisions about the overall
plant design, such as the use of two reactors, and proceeded to design the plant for an annual
production capacity of 3000 tonnes. Team members were delegated responsibility for specific parts of
the design. Brandon was responsible for reactor design, impeller/agitator design, economic analysis and
cooling tower design; Greg was responsible for the initial process description and production schedule,
pump sizing and costing, and the acid route alternative; Shariq was responsible for the downstream
equipment sizing and selection, process chemistry, and overall editing; Scott was responsible for the
process energy balances, reactor kinetics and profiles, utilities, and operating costs; Alex was
responsible for the PFD, P&ID, floor plan and packed column design; Nijastan was responsible for raw
material and product tanks, selection of the hot oil column; condenser design, and process safety.

A plant location was selected in Sarnia as the area has housed large industrial plants for
decades, is considered to be an international leader in chemical production, and has access to
continental railways. A marketing study was conducted and determined that the industry has an annual
demand of 160,000 tonnes/year (in US alone) with an average market price of 5-7 $/kg.

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2.0 Process Description
The transesterification (TE) reaction, which involves the substitution of an organic group from an
ester with an organic group from an alcohol, is conducted between 160°C and 210°C at atmospheric
pressure for approximately 5 hours. The pre-polymer formed from the TE reaction is used in the
polycondensation (PC) reaction to produce the polyester resin by applying a vacuum over about a 6 hour
period for a temperature ranging between 200°C and 220°C. The final product will be discharged onto a
classic cooling belt as a film in a molten state before passing through a flaker and hammer-mill
pulverizer to allow for easy storage in silos.

250
Reactor Temperature (C)

200

150

100

50

0
0 2 4 6 Time (h) 8 10 12 14

Figure 1: The temperature profile for the reactor in the process.

800
Reactor Pressure (mmHg)

700
600
500
400
300
200
100
0
0 2 4 6 8 10 12 14
Time (h)

Figure 2: The pressure profile for the reactor in the process

The ester route chemistry involves reacting dimethyl terephthalate (DMT), diethylene glycol
(DEG), and 1,2-propylene glycol (PG) to form the prepolymer, while evolving the byproduct methanol.

DMT + 2(DEG + PG) ↔ BHDT/PT + 2MeOH ↑ (1)


Monomer ↔ poly (1, 2-propylene-diethylene-terephtahalate) + glycol ↑ (2)

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The direct esterification (DE) process, or acid route, is the alternative to the transesterification
process. The acid route chemistry involves the reaction of purified terephthalic acid with ethylene
glycol to form the prepolymer, while evolving the byproduct water.

PTA + 2EG ↔ BHET + 2H2O ↑ (3)


Monomer ↔ poly(ethylene terephthalate) (4)

The DE process is capable of generating a resin with a higher average degree of polymerization
in a shorter period of time than the TE process [1]. A short comparison between the two processes is
made in the table below.

Table 1: Comparison of Direct Esterification and Ester-Interchange Routes

Specification Direct Esterification Process Transesterification Process


Process type Batch Batch
Feed Purified terephthalic acid, ethylene DEG, PG, DMT
glycol
Catalyst required? Yes Yes
Reactor configuration Two stirred reactors in series, Single stirred reactor
followed by multi-stage polymerizer
Process description Catalyzed esterification in primary Transesterification of DMT with
reactor to 90% conversion, then glycols to form intermediate
esterification in second reactor to 98% oligomers, followed by catalyzed
conversion, then heated and polycondensation
pressurized in polymerizer
Reaction time 9 hours 11 hours
Reaction conditions 245 - 275 oC; 0.133 - 275 kPa 215 oC, 0.133 kPa
Vacuum required? Yes Yes
Byproducts Water Methanol
Average DP 200 100

The plant scale-up and equipment selection was based on a required production of 3,000
tons/year of polyester resin. A classic cooling belt and two reactor system arrangements were chosen.
The ester route chemistry is used since data was previously made available from the pilot plant. The
reactor design parameters were based on an end-point viscosity of approximately 5.3 Pa-s which was
determined using MFI pilot plant data and adjusting for the temperature requirements. Table 2
summarizes advantages and disadvantages of this plant configuration.

Table 2: Summary of Configuration Costs and Benefits for a Two Reactor Plant

Advantages Disadvantages
Redundancy High initial capital cost due to additional
equipment needed for redundancy
Maximize use of downstream equipment
Two products can be made in the same plant

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The catalyst chosen, Fascat 4100, is compatible with both the TE and PC reactions while
minimizing potential side reactions. It does not require any special handling or filtration once the
reactions are complete. A single 50kg bag is added per reactor charge.
Table 3: Information for Start-up Batch Charges (A) and Normal Batch Charges (B) per Reactor

Stream Stream Information Batch Charges A (Kg) Batch Charges B (Kg)


1 DMT 5156 5156
2 PG 3536 2263
3 DEG 704 386
4 Product 5669 5669

Table 4: Physical properties of all materials in the plant

Material Properties
Dimethyl Terephthalate (DMT) Diethylene Glycol (DEG)
Chemical formula C10H10O4 C4H10O3
Flash Point (oC) 153 138
Form Solid/Molten Liquid Liquid (clear viscous)
Melting Point (oC) 140 -8
Molecular Weight (g/mol) 194.19 106.12
o
Vapour Pressure (mm Hg) 1.2 at 20 C (solid) 1.12
Colour White Colourless. Clear
Odour Slight to none Odorless
Density (g/cm3) 1.35 1.036
Toxology (acute effects mg/kg) 3200 12565
Propylene Glycol (PG) Methanol (MeOH)
Chemical formula C3H8O2 CH3OH
Flash Point (oC) 99 11
Form Liquid (oily liquid) Liquid
Melting Point (oC) -59 -98
Molecular Weight (g/mol) 76.1 32.04
Vapour Pressure (mm Hg) 1.035 97.7
Colour Colourless. Clear Colourless. Clear
Odour Odorless Mild alcohol odour
Density (g/cm3) 1.118 0.7918
Toxology (acute effects mg/kg) 20000 5628

The cycle time for each reactor is summarized in Table 5. As all downstream equipment is
shared between the two reactors, the cycles are staggered by 10 hours to allow sufficient processing
time for each batch. Having two staggered cycles also provides increased process flexibility as it is
possible to continue operation of one cycle while the other is down.

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Table 5: Operating Schedule

Task Time for Reactor A (hours) Time for Reactor B (hours)


Start time Duration Start time Duration
Raws charging 0600 3 2100 3
Heating up 0900 1 0000 1
Transesterification stage 1000 5 0100 5
Polycondensation stage 1500 6 0600 6
Discharging 2100 3.5 1200 3.5
Resin cooling 2100 3.5 1200 3.5
Resin crushing 2130 3.5 1230 3.5
Resin grinding 2130 3.5 1230 3.5
Batch Complete 0100 1600

Total cycle time: 20 hours 20 hours

The recycled glycols have an 80:20 PG to DEG ratio once condensed from the PC stage. Under normal
operating conditions the recycled glycols will be blended with new glycols to match batch specifications.
Periodically some of the recycled glycols will be purged from the system to minimize impurities. After
being separated and collected the methanol is then sold on the market for $350/ton.

3.0 Work Schedule


The plant will be in operation for 42 of the 52 weeks per year. This will allow for 2 weeks of
scheduled holiday for Christmas and New Year’s time, along with 2-scheduled shut downs, each
consisting of 3 weeks, and a remaining 2 weeks for unscheduled shutdown. These scheduled shutdowns
will allow for maintenance, repairs, and upgrades which can be made to ensure reliable performance of
the equipment during plant operating.

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4.0 Process Mass and Energy Balance

Table 6: Process Mass and Energy Balance Summary

Process Flow In Process Flow Out Peak Utility Flow Power Required
Utility Type
(kg/batch) (kg/batch) (m^3/h) (kW)

Unit 1: Upstream
Tanks: TK 101 A/B 386.39
TK 102 A/B 2263.39
TK 103 A/B 5155.66 0.180 (both tanks) Oil 11.185 (both tanks)
Unit 2: Processing
Reactor: R 201 A/B Raws Feed 7805.44 21.82 Oil 15.4
R 201 A/B Glycols 1590.14 2014
R 201 A/B Methanol 1674
R 201 A/B Product 5668.88
Exchanger: E 201 A/B 1674 1674 3.46 Water
E 202 A/B 2014 2014 9.29 Water
Column: T 201 A/B Total Feed 16740
T 201 A/B Methanol 1674
T 201 A/B Glycols 15066
Tanks: V 201 A/B 1674 1674
V 202 A/B Total Feed 2014 0.6987 Water
V 202 A/B To Storage 1913
V 202 A/B To V-203 A/B 101
V-203 A/B 101 101 0.0369 Water
V-204 2014

TK 201 1674

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Unit 3: Downstream
Equipment: CB 301 5668.88 5668.88 4.067 Chilled Water 155.83
HM 301 5668.88 5668.88 29.83
CB 302
CB 303
Silos: TK 301 A/B 5668.88
TK 302
Unit 4: Utilities
Equipment: F 401 22 Oil 13.4
CT 401 13.48 Water 3.19
*duty for both
Pumps Capacity (m^3/h) Material Pumped pumps where
applicable*
Unit 1: P 101 37.855 DEG 19
P 102 A/B 3.43 DEG 4
P 103 34.01 PG 19
P 104 A/B 0.629 PG 4
P 105 37.855 DMT 19
P106 A/B 4.29 DMT 4
Unit 2: P 201A/B 1.13 Methanol 4
P 202 A/B 4 Air (For Vacuum) 44
P 203 A/B 1.8 Glycols 4
P 204 1.71 Glycols 2
Unit 4: P 401 A/B 22 Water 60

Oil
P 402 A/B 20.2 60

Misc.
Lighting and
Instrumentation 13.75

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5.0 Process Control
5.1 Preliminary P&ID diagram
14

1A
TK-102A TK-201
E-201A E-201B
15A 15B
P-102A 6A 6B
1B
P-101 TK-102B TRC
202A
TRC
202B

P-102B 7A 7B

V-201A P-201A P-201B


10A
P-202A V-201B P-202B
V-203A 10B V-203B
T-201A T-201B
2A E-203B
TK-101A E-203A

P-104A FRC FRC


201A E-202A 201B E-202B
9A 9B
P-103 2B V-202A V-202B
5A 8A 5B 8B
TK-101B
P-104B PRC PRC
TRC 202B TRC 202B
201A 201B
11B 12B

3A
R-201A R-201B
TK-103A
11A 12A
P-106A C-201

4A 4B
P-105 3B
P-203B V-204
TK-103B
P-106B 13
P-203A

P-204

F-401
LRC
401

CT-401 TK-301A
CB-302

CB-301
P-402A P-401A TK-301B
WATER SUPPLY 16 17
P-402B P-401B
HM-301 TK-302

Figure 3: P&ID

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Section 4 includes a detailed list of each piece of equipment labeled on the P&ID including some key
equipment properties. The red and yellow lines on the P&ID are the outlet and inlet flows for the hot oil
unit, respectively, while the dark and light blue lines are the outlet and inlet streams for the cooling
tower, respectively. Table 5 below corresponds to the stream labeling on the P&ID for both start up
conditions and normal operating conditions.

Table 7: P&ID Mass Charging and Process Requirements

Start-up Material Normal Operation Material


Stream Description Requirements (kg) Requirements (kg)
1 A/B DEG 704 322
2 A/B PG 3536 2005
3 A/B DMT 5156 5156
4 A/B Reactor Product 5669 5669
5 A/B Packed Column Feed 16738 16738
6 A/B Packed Column MeOH 1674 1674
7 A/B Packed Column MeOH Reflux ---- ----
8 A/B Packed Column PG 15064 15064
9 A/B Take-off Condensor Glycol 2014 2014
10 A/B Glycol Receiver Feed 101 101
11 A/B Glycol Receiver 1 Outlet 1913 1913
12 A/B Glycol Receiver 2 Outlet 101 101
13 Glycol Purge ---- ----
14 Glycol Recycle to Reactor 0 1913
15 A/B Methanol Byproduct 1674 1674
16 Crusher Feed 5668 5668
17 Storage Feed 5668 5668

5.2 End point control strategy description


The exponential increase of the molecular weight over the extent of reaction makes it
challenging to ensure a correct and consistent viscosity is achieved. The window is a narrow one such
that if it is gone above, equipment damage is possible; and if too low, the polymer will not have the
required properties needed. Hence for this reason, a proven inline viscosity measuring device is used
along with the temperature and pressure sensors to accurately determine when to stop the reactor.
The proposed device is a Dynatrol Viscosity Probe that utilizes a vibrating rod immersed in the reactor.
[2]

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Figure 4: Dynatrol® Viscosity Measurement Probe [2]

It is made of stainless steel and can operate under pressure as well as vacuum, and can be
made to operate at high temperatures. The advantage to this device is that there are no moving parts
and it is extremely wear resistant. This will allow the process to run uninterrupted without having to
break the vacuum to test the product quality. It will be placed on the side of the reactor approximately
25% of the height from the bottom. This placement is important to ensure that it is not in a dead spot
and to ensure that it is low enough that polymer will be present at this spot always, as the reactor will
never be less than 25% full.

5.3 Vacuum application control strategy


To control the vacuum application during the transesterfication stage, a control system using a
pressure gauge in the reactor will be used. The controller will mimic the pressure profile required to
remove the glycols over time by operating a valve preceding the take-off condenser. A two valve system,
a main and trim valve, or a single valve which includes a trim feature can be used to improve the
precision of the applied vacuum and stabilize any large abnormalities. Choke valves, more specifically
butterfly valves, are a common valve used in pressure controlled systems since they always induce a
pressure drop in the system. They also have built in fail open and close features to prevent safety issues
and potential damage to equipment.

5.4 Control of major pieces of equipment


It is important to ensure that the employees know everything that is happening in the major
pieces of the system in the most efficient way possible. This will ensure that if something does go wrong
that it can be rectified quickly with minimal damage economically and physically. Each major
component of the system has a variety of sensors and control systems in place. The reactor has
temperature sensors that regulate the hot oil entering the heating jacket to ensure the system is under
a constant and specific temperature. The function of the pressure sensor and controller is to ensure the
right amount of vacuum is used for the second part of the reaction. The level sensor can be used for
safety reasons as well as another indicator of when the reaction is completed. The distillation column
has temperature sensors on the top and bottom trays to create a temperature gradient which will use to
control the reflux ratio. The Cooling belt has temperature sensors that regulate the flow rate of water
and to ensure constant cooling of polymer.

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6.0 Reactor Design and Sizing
6.1 Reactor Design

Table 8: Reactor Design Specifications

Volume [m3] 10
Internal Diameter [m] 2.2
Height [m] 2.8
Number of Ports 8
Number of Instrument Ports 4
Material Of Construction NiCrMo stainless steel
Jacketed Yes
Vacuum rated Yes, up to 4mmHg
Light/Camera equipped Yes, for remote viewing capabilities.

Figure 5: Reactor Dimensions

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Glycols to Column
(2 inches)
Glycols from
Column (2 inches)

Nitrogen
(1 inch)

Agitator Inlet
(5 inches)
Manhole
(20 inches)

DEG Loading
(3 inches)

DMT Loading
(6 inches)
PG Loading
(5.5 inches)

Figure 6: Reactor Overhead (to scale)

6.2 Ports

On top of reactor:

1. PG loading 5.5”
2. DEG loading 3”
3. DMT (molten) loading 6”
4. Agitator shaft inlet 5”
5. Manhole – 20” ID equipped with a sightglass, also used for solid catalyst loading
6. MeOH/Glycol outlet 2”
7. Glycol from column 2”
8. Nitrogen port 3”

Sensor Probes needed:

1. Temperature sensor
2. Pressure sensor
3. Viscosity sensor (see section 5b)
4. Level sensor

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Discharge:

One heat traced discharge line at the bottom of the reactor is used for discharging of finished product to
the single cooling belt. This will be a segment ball valve to reduce maintenance due to larger bore
diameter and containing a polished inner surface. The cutting and cleaning action of the ball and seat
eliminate wear and valve blockage due to the high viscosity polymer.

The outlet valve on each reactor will be connected by a heat traced line to a common pipe to travel to
the single cooling belt. All lines travelling to the cooling belt containing the polymer resin are heat
traced and lengths will be minimized to ensure ease of travel. The line will also have the capability of
being purged so that no product will be trapped in the line to avoid possible blockage.

6.3 Agitator System

Table 9: Agitator System Specifications

Agitator Power [kW] *see memo #1 15.4


Agitator speed [RPM] 24 and 42 (dual setting)
Number of Impellers 3
Blade Type P4/45
Number of Baffles 4
Baffle Width [m] 0.122
Baffle Clearance [m] 0.025
Agitator Height [m] Located at 0.7, 1.4, 2.1 meter from the bottom
Agitator Diameter [m] 1
Agitator Shaft Diameter 5”

 Three P4/45 turbine blades will be used and placed at 0.25H, 0.5H, and 0.75H of the
tank. This will allow proper mixing during the beginning of the reaction when the
reactor is at its fullest. As the volume decreases the top blade will become exposed and
act as a foam breaker if any occurs when the vacuum is applied.
 According to [4] the number of baffles needed per tank is 4. A given relationship of
baffle width versus viscosity is given in the documentation.

17
7.0 Other Equipment Design and Sizing
7.1 Condensers
7.1.1 Take-Off Condenser

Table 10: Specifications of our take-off condensers for our proposed plant [6]

Material 316 Stainless Steel


Type Shell & tube heat exchanger
Straight tube, Fixed tubesheet shell & tube heat exchanger
Features Rated for 225 PSI and 450 oF on shellside, 150 PSI and 450 oF on tube side
Surface Area 103 ft2
Length 5 ft
Diameter 8 inches
Number of Passes 1

The take-off condenser which is used for glycols is sized from the heat balance giving the
condenser surface area. The surface area was calculated to be 98 ft2. A condenser meeting our
requirements was found at ITT Standard and was chosen with a surface area of 103 ft2.

7.1.2 Methanol Condenser

Table 11: Specifications of our take-off condensers for our proposed plant [6]

Material 316 Stainless Steel


Type Shell & tube heat exchanger
Straight tube, Fixed tubesheet shell & tube heat exchanger
Features Rated for 225 PSI and 450 oF on shellside, 150 PSI and 450 oF on tube side
Surface Area 144 ft2
Length 7 ft
Diameter 8 inches
Number of Passes 1

The methanol condenser is sized the same way from the heat balance and a surface area of 144
ft2 was calculated. A condenser which fits our sizing requirements was chosen from ITT Standard. It is
the same type of condenser as the take-off condenser except of different size. A sample calculation for
sizing of the take-off condenser is shown below.

∆𝑇1 − ∆𝑇2
𝑄 = 𝑈𝐴
∆𝑇
𝑙𝑛 ∆𝑇1
2

∆𝑇1 = 𝑇𝑖𝑛 𝑔𝑙𝑦𝑐𝑜𝑙𝑠 − 𝑇𝑜𝑢𝑡 𝑤𝑎𝑡𝑒𝑟 = 205℃ − 48℃ = 157℃

∆𝑇2 = 𝑇𝑜𝑢𝑡 𝑔𝑙𝑦𝑐𝑜𝑙𝑠 − 𝑇𝑖𝑛 𝑤𝑎𝑡𝑒𝑟 = 70℃ − 20℃ = 50℃

18
𝑘𝑊
𝑈 = 0.35
𝑚2 ∙ ℃
𝑄𝑠𝑒𝑛𝑠 = 𝑀𝑔𝑙𝑦𝑐𝑜𝑙𝑠 𝐶𝑝𝐷𝐸𝐺 𝑇𝑖𝑛 𝑔𝑙𝑦𝑐𝑜𝑙𝑠 − 𝑇𝑜𝑢𝑡 𝑔𝑙𝑦𝑐𝑜𝑙𝑠 0.2 + 𝑀𝑔𝑙𝑦𝑐𝑜𝑙𝑠 𝐶𝑝𝑃𝐺 𝑇𝑖𝑛 𝑔𝑙𝑦 𝑐𝑜𝑙𝑠 − 𝑇𝑜𝑢𝑡 𝑔𝑙𝑦𝑐𝑜𝑙𝑠 0.8

𝑄𝑙𝑎𝑡𝑒𝑛𝑡 = 𝑀𝑔𝑙𝑦𝑐𝑜𝑙𝑠 × 𝐻 𝑣 𝐷𝐸𝐺 + 𝐻 𝑣 𝑃𝐺

𝑄𝑠𝑒𝑛𝑠 + 𝑄𝑙𝑎𝑡𝑒𝑛𝑡
𝑄= 𝑠 = 300 𝑘𝑊
2 𝑕𝑟 × 3600
𝑕𝑟
𝑄 300 𝑘𝑊
𝐴= = = 9.17𝑚2
∆𝑇1 − ∆𝑇2 𝑘𝑊 157℃ − 50℃
𝑈 ∆𝑇 0.35 157℃
𝑚2 ∙ ℃
𝑙𝑛 ∆𝑇1 𝑙𝑛
2 50℃

7.2 Packed Tower


An insulated packed bed tower was selected since the pressure drop in this column is minimal.
Also, the separation of methanol and PG is relatively simple since their volatilities significantly vary. The
saddle configuration was chosen for packing because they have increased surface area, are commonly
manufactured out of ceramics, and have increased hydrodynamics during low pressure operation. Table
12 below shows the various packing specifications required to operate the packed column at total
reflux. [7]
Table 12: Column Packing Specifications

-1
Fill Factor 360.89 m
2 3
Surface Area 250 m /m
Size 1 Inch

Orientation Random
Type Berl Saddles
Material Ceramic
Vendor Norton

The minimum tower requirements were calculated using scale-up methods from the pilot plant
column as well as the Fenske and Underwood equations for the minimum number of trays and
minimum reflux ratio, respectively.[8] [9] The minimum requirements along with the steady state
calculations, determined in Aspen, are shown in Table 13.

19
Table 13: Packed Bed Column Minimum and Steady State Requirements

Nmin 2
Nreal 4
Rmin 6.59
R 9.89
HETP 1.64 ft
Diameter 3 ft
Length 10 ft
Condenser Duty 34.19 kW

The Fenske Equation, shown below, was used to determine the minimum number of trays with
the specified distillate and bottoms composition, xD and xB, along with the relative volatilities, αAVG, as
per Aspen.
𝑥𝐷 1−𝑥 𝐵
log ⁡
1−𝑥 𝐷 𝑥𝐵
𝑁𝑚𝑖𝑛 = −1 (1)
log α AVG

The Underwood Equation, Equation 2, is evaluated by solving for θ in equation 3 using trial and
error methods and the same values which were used in the Fenske Equation with a known flow rate q.
𝛼 𝑖 𝑥 𝑖𝐷
𝑅𝑚𝑖𝑛 = 𝛼 𝑖 −𝜃
−1 (2)

𝛼 𝑖 𝑥 𝑖𝐹
𝑞= +1 (3)
𝛼 𝑖 −𝜃

The real number of trays is twice the minimum, where every tray is 1.64 feet in length, plus the
condenser accounts for the approximate column length of 10 feet also taking into account a safety
factor. A safety factor of at least 10% above the number of stages determined should be incorporated.
[8]

The inlet PG and methanol stream will be fed into the bottom of the column since no reboiler is
required. The column will be operated near 70% flooding and separate the required methanol from PG
over the entire 5 hour transesterfication reaction.

The reflux drum will be a horizontal tank with an elliptical head used to feed condensed
methanol back to the packed column. The volume was determined by assuming a length to diameter
ratio of 2, using the volume flow rate from the condenser to determine diameter when the tank is at
half capacity with a 5 minute hold-up time.

20
Table 14: Reflux Drum Specifications Based on 5 Minute Hold-up Levels at Half Capacity

3
Volume 18.68 ft
Diameter 2.5 ft
Length 5 ft
The sump vessel was sized using a similar method as the reflux drum, however the PG flow rate
from the bottom of the column was used to determine diameter.
Table 15: Sump Vessel Specifications Based on 5 Minute Hold-up Levels at Half Capacity

3
Volume 20.80 ft
Diameter 2.5 ft
Length 5 ft
The sump and reflux drum diameters and lengths were rounded to a common tank size as they would be
ordered.

7.3 Vessels
7.3.1 Raw Material Storage
The raw materials propylene glycol (PG), diethyl glycol (DEG), and dimethyl terephthalate (DMT)
are stored in two tanks each. The reason for using two tanks for storage of each raw material instead of
one larger tank is because it allows more flexibility in scheduling for shipments and maintenance in
emergencies. This will reduce any downtime in the process which is essential for profitability. Sizing and
specifications are provided in table 16 below.
Table 16: Sizing and specification for raw material storage tanks [10] [11]

Storage Vessels
Dimethyl
Propylene Glycol Diethyl Glycol Terephthalate
TK-101A TK-101B TK-102A TK-102B TK-103A TK-104B
Tank Type Vertical Fixed Roof Horizontal Tank Vertical Fixed Roof
Material Carbon Steel Carbon Steel Stainless Steel
Capacity 25,000 galls 7,500 galls 30,000 galls
Diameter (ft) 16 9 12
Height (ft) 26 - 47.5
Side Length (ft) - 14 -
Total Length (ft) - 16.6 -
Storage Time (days) 15 15 15
Heating Surface (ft2) - - 1252
Agitator Motor (hp) - - 7.5
Agitator Height (ft) - - 1.5

21
DMT is stored in molten liquid form above its melting temperature of 140 0C in heated and
insulated storage tanks at 165 0C. Due to the high temperature and the possibility of corrosion, the tank
is to be made of stainless steel. The two tanks have 6-inch fiberglass insulation all around, two heating
coils with hot oil flowing through them, and an agitator shaft with two impellers running at 40 rpm for
uniform temperature [11]. Caution should be used when handling the molten DMT as it can cause
thermal burns. PG presents no unusual problems and with a low melting point, heating is not necessary.
DEG however has a melting point of -10 0C and in the cold winters, there is a risk for DEG to solidify.
Therefore, the tank will have 6-inch fiber glass insulation all around it to keep it from reaching the
melting point. The diagram below shows the DMT tank design schematic.

Figure 7: Storage tank design schematic for our molten DMT [11]

The sizing of the tanks was done by calculating the amount of raw material required in 30 days
(60 batches) in gallons which is then divided by two since we’re using a two tank system. A third of the
tank space is left empty for the nitrogen blanket. When the raw materials shipment arrives, the tank will
be filled to two-thirds of its capacity and the remainder will be filled into the second tank. The
shipments arrive in intervals of 15 days (twice a month) so by the time the next shipment of raw
materials arrive, there will be enough space in the tanks for storage. The table below shows the
scheduling of the shipments with the amount ordered.
Table 17: Shipping and storage schedule for proposed plant

29st (last 12th (current 14th (current 14th (current 29th (current
month) month) month) month) month)
DMT 31,500 galls 30,000 galls 31,500 galls
DEG 5,000 galls 5,000 galls 5,000 galls
PG 25,000 galls 25,000 galls 25,000 galls

22
The tank dimensions were determined by using an online calculator [10] with a length to
diameter ratio of about 1.5. All vessel dimensions in the plant were determined this way except for DMT
and the product storage silos which were determined from capacity charts. A sample calculation for
storage tank sizing is shown below for DMT.

𝑘𝑔 𝑏𝑎𝑡𝑐𝑕
5156 ×2 × 30 𝑑𝑎𝑦𝑠
𝑏𝑎𝑡𝑐𝑕 𝑑𝑎𝑦
𝐶𝑎𝑝𝑎𝑐𝑖𝑡𝑦 = ÷ 2 𝑡𝑎𝑛𝑘𝑠 = 30,270 𝑔𝑎𝑙𝑙𝑜𝑛𝑠
𝑘𝑔
5.11
𝑔𝑎𝑙𝑙𝑜𝑛𝑠

7.3.2 Receivers
During transesterification, once the methanol is separated from the glycols it is completely
condensed into a liquid and held in a receiver tank before being sent to the storage tank. Since all the
methanol has been condensed, we do not require cooling water for the receiver and there will be two in
total for each of the two reactors. Sizing was done by calculating the volumetric flow of methanol per
batch and multiplying it by a factor of 1.25 for extra space. Calculations for this are shown below.
𝑘𝑔
1674
𝐶𝑎𝑝𝑎𝑐𝑖𝑡𝑦 = 𝑏𝑎𝑡𝑐𝑕 × 1.25 = 698 𝑔𝑎𝑙𝑙𝑜𝑛𝑠
𝑘𝑔
3.0
𝑔𝑎𝑙𝑙𝑜𝑛𝑠

During polycondensation, the glycol vapours are condensed to a liquid (95%) by a condenser,
which is further condensed afterwards, in two condensate receivers (refer to Figure 3: P&ID) for the
remaining 5% vapour. Service water from the cooling tower at ambient temperature will be used as the
cold water supply for condensing. Sizing for the primary receiver was done by taking 95% of the take-off
condenser glycol over 2 hours since most of the glycols are pulled within that time while the secondary
receiver is 5%. They are sized for two batches in case of any downtime in the process. Calculations for
this are shown below with a table under it showing the specifications of the receivers.

𝑘𝑔
0.95 × 2014
𝑏𝑎𝑡𝑐𝑕
2 𝑕𝑟 × 2 𝑏𝑎𝑡𝑐𝑕 × 1.25 = 600 𝑔𝑎𝑙𝑙𝑜𝑛𝑠
𝑘𝑔
0.8 × 4.23 + 0.2 × 3.22
𝑔𝑎𝑙𝑙𝑜𝑛𝑠
𝑘𝑔
0.05 × 2014
𝑏𝑎𝑡𝑐𝑕
2 𝑕𝑟 × 2 𝑏𝑎𝑡𝑐𝑕 × 1.25 = 28 𝑔𝑎𝑙𝑙𝑜𝑛𝑠
𝑘𝑔
0.8 × 4.23 + 0.2 × 3.22
𝑔𝑎𝑙𝑙𝑜𝑛𝑠

23
Table 18: Sizing and specification for all receivers

Receivers (Glycols - PC Stage) Receivers (MeOH - TC Stage)


Secondary
Primary Receivers Receivers Primary Receivers
V-202A V-202B V-203A V-203B V-201A V-201B
Material Stainless Steel Stainless Steel Stainless Steel
Capacity (galls) 600 30 700
Height (ft) 6 2.4 7
Diameter (ft) 4.5 1.6 4.5

7.3.3 Methanol Storage and Glycol Recycle


Methanol from the two receivers (V-201A/B) will be stored in a single tank rather than in two
tanks like everything else. Methanol is a flammable liquid so storage is to be kept away from sources of
ignition or sparks. The storage tank is sized for 30 days of storage with a third of the tank space allowed
for the nitrogen blanket. Sizing calculations for the methanol tank is shown below.

𝑘𝑔
1674 𝑏𝑎𝑡𝑐𝑕
𝐶𝑎𝑝𝑎𝑐𝑖𝑡𝑦 = 𝑏𝑎𝑡𝑐𝑕 ×2 × 30 𝑑𝑎𝑦 × 1.5 = 50,220 𝑔𝑎𝑙𝑙𝑜𝑛𝑠
𝑘𝑔 𝑑𝑎𝑦
3.0
𝑔𝑎𝑙𝑙𝑜𝑛

During polycondensation when the glycols go through the primary and secondary receivers, they
will be sent to a glycol recycle tank which will recycle the glycols back into the process for the next
batch. This glycol recycle tank is sized for 3 days. This seems like a lot but in case anything goes wrong in
the process, we don’t have to worry about the tank overflowing. Sizing calculations for the glycol recycle
tank is shown below with a table under it showing the specifications.

𝑘𝑔
2014 2 𝑏𝑎𝑡𝑐𝑕
𝐶𝑎𝑝𝑎𝑐𝑖𝑡𝑦 = 𝑏𝑎𝑡𝑐𝑕 × × 3 𝑑𝑎𝑦 × 1.15 = 3450 𝑔𝑎𝑙𝑙𝑜𝑛𝑠
𝑘𝑔 𝑑𝑎𝑦
0.8 × 4.23 + 0.2 × 3.22
𝑔𝑎𝑙𝑙𝑜𝑛
Table 19: Sizing and specifications for methanol storage and glycol recycle tanks

Methanol Glycol Recycle


TK-201 V-204
Tank Type Vertical Fixed Roof Horizontal Tank
Material Carbon Steel Carbon Steel
Capacity 50,000 galls 3,500 galls
Diameter (ft) 20 7
Height (ft) 33 -
Side Length (ft) - 11
Total Length (ft) - 13.13
Storage Time
(days) 30 3

24
7.3.4 Product Storage Silos
The polyester resin product will be collected in welded carbon steel silos. There will be two silos
sized to store two weeks of product each, this will allow one silo to be filled while the other can be used
to fill super sacks for shipping. Also, there will be a third silo that will be used to store any off-
specification product (deviation from our target molecular weight) which is sized assuming 10% of our
resins produced in a month will be off-specification. Later on, the off-specification products will be
mixed in with the rest of marketable products in order to homogenize them so that they can be sold.
Calculations for sizing of the two main silos (TK-301A/B) are shown below with a table under it showing
the specifications of all silos. The silo capacities in the table are a little higher than calculated because
they were taken from a capacity chart and it is beneficial to have the extra space.

𝑘𝑔 2 𝑏𝑎𝑡𝑐𝑕
5669 × × 30 𝑑𝑎𝑦
𝑏𝑎𝑡𝑐𝑕 𝑑𝑎𝑦
𝐶𝑎𝑝𝑎𝑐𝑖𝑡𝑦 = ÷ 2 = 38,477𝑔𝑎𝑙𝑙𝑜𝑛𝑠 = 5985 𝑓𝑡 2
5.11 + 4.23 + 3.92 𝑘𝑔
3 𝑔𝑎𝑙𝑙𝑜𝑛

Table 20: Sizing and specifications for polyester resin storage silos [12]

Polyester Resin Product


TK-301A TK-301B TK-302
Tank Type Shop Welded Silo (45o hopper)
Material Carbon Steel
Capacity 6,426 ft3 2,396 ft3
Diameter (ft) 14 12
Height (ft) 48 28
Storage Time (days) 15 30

25
7.4 Downstream Equipment
7.4.1Cooling belt system
The Sandvik double roll feed cooling belt [13] is used after the reactors to transport and
cool the polymer. The Polymer is discharged from the bottom of the reactor, between two rollers,
that flatten the polymer to a thickness of 2 mm. The polymer is then pulled by the steel cooling belt
of width 1.02 m and 8 m length as water is sprayed on the underside of the belt to cool the melt. To
cool the polymer to ambient temperature of 25 oC, approximately 16,300 kg of water is required.
The average velocity would be around 0.031 m/s for the cooling belt. The flakes will then be
removed from the belt by a scraper and broken by a breaker roller before going to the pulveriser.

Figure 8: Double roll feeder cooling belt [13]

26
7.4.2 Disintegration equipment
The broken flakes will deposit into the feed bag of a Hammer-Mill pulveriser to be further
broken down to smaller particulates. The pulveriser can take 1200 to 3000 kg/hr of the polymer which is
within our parameters [14]. After the polymer is broken further down, the particulates will fall onto a
conveyer belt. The pulveriser contains a recycling and filter unit so that when particles are not of a pre-
determined size the filter would stop them from leaving the system and would be recycled back into the
hammer mill to be broken down further.

Figure 9: Hammer Mill-30 Pulveriser [14]

After the pulveriser, the granules are deposited onto a cleated inclined conveyor belt angled at
60 degrees of approximately 55 meters (180 ft) in length to put the solid into a silo to be mixed with
different batches to create uniformity.
Table 21: Specifications of Selected Processing Equipment

Section Dimensions
Cooling belt 8 by 1.02 m (26 by 3 ft)
Pulveriser 1.45 by 0.93 by 1.69 m (4.75 by 2.8 by 5.5 ft)
Conveyor belt 31 by 1 m (102 by 3 ft)

27
7.5 Utility Equipment
7.5.1 Hot Oil Utility
In the plant, Fulton’s four pass vertical coil thermal fluid heater will be used to provide the
required heating by hot oil to the reactor and the two heated DMT storage tanks. From the heat
balance, a heat output of 1,700,000 Btu/h was calculated to be the maximum heat required at peak
demand and a suitable thermal fluid heater design was selected from the capacity chart.
Transesterification required more heat than polycondensation so the heat output was found by
summing the heat required for TE stage and the heat required for the raw DMT tanks since that will be
the maximum heat (capacity) required at once. Sizing calculations for this are shown below.

Heat in TE Reaction

𝑄𝑟𝑒𝑞 = 𝑀𝑚𝑒𝑡𝑎𝑙 𝐶𝑝𝑚𝑒𝑡𝑎𝑙 + 𝑀𝑐𝑕𝑒𝑚𝑖𝑐𝑎𝑙 𝐶𝑝𝑐𝑕𝑒𝑚𝑖𝑐𝑎𝑙 𝑇2 − 𝑇1


𝑘𝐽 𝑘𝐽
𝑄𝑟𝑒𝑞 = 5027.7 𝑘𝑔 × 0.15 + 10847.6 𝑘𝑔 × 2.2 160 − 100 ℃ = 1,477,133 𝑘𝐽
𝑘𝑔 ∙ ℃ 𝑘𝑔 ∙ ℃

 100oC was found to be the initial temperature because the DMT is already heated

𝑀𝑚𝑒𝑡𝑎𝑙 𝐶𝑝𝑚𝑒𝑡𝑎𝑙 + 𝑀𝑐𝑕𝑒𝑚𝑖𝑐𝑎𝑙 𝐶𝑝𝑐𝑕𝑒𝑚𝑖𝑐𝑎𝑙 𝑇 − 𝑇1


𝜏= 𝑙𝑛
𝑈𝐴 𝑇 − 𝑇2
𝑘𝐽 𝑘𝐽
5027.7 𝑘𝑔 × 0.15 + 10847.6 𝑘𝑔 × 2.2 175 − 100 ℃
𝑘𝑔 ∙ ℃ 𝑘𝑔 ∙ ℃
𝜏= 𝑙𝑛 = 0.818 𝑕𝑟𝑠
𝑘𝐽 175 − 160 ℃
1750 2 × 27.67𝑚2
𝑚 ∙𝑕∙℃

𝑄𝑟𝑒𝑞 1,477,133 𝑘𝐽
𝑄𝑇𝐸 𝑟𝑥𝑛 = = = 501.6 𝑘𝑊
𝜏 × 3600 0.818 𝑕𝑟 × 3600 𝑠
𝑕𝑟

Heat in DMT Storage Tanks

𝑄𝑙𝑜𝑠𝑠 = 𝑀𝐷𝑀𝑇 𝐶𝑝𝐷𝑀𝑇 0.05 × 𝑇 ∗ 5% 𝑕𝑒𝑎𝑡 𝑙𝑜𝑠𝑠 (𝑙𝑖𝑓𝑒𝑡𝑖𝑚𝑒 𝑖𝑛 𝑡𝑎𝑛𝑘)

𝑘𝐽
𝑄𝑙𝑜𝑠𝑠 = 143,088.6 𝑘𝑔 × 2.2 0.05 × 165℃ = 2,597,038 𝑘𝐽
𝑘𝑔 ∙ ℃

𝑄𝑙𝑜𝑠𝑠
𝑄𝐷𝑀𝑇 = ×2
𝑕 𝑠
𝑙𝑖𝑓𝑒𝑡𝑖𝑚𝑒 × 24 × 3600
𝑑𝑎𝑦 𝑕
2,587,038 𝑘𝐽
𝑄𝐷𝑀𝑇 = × 2 = 7.49 𝑘𝑊
𝑕 𝑠
8 𝑑𝑎𝑦 × 24 × 3600
𝑑𝑎𝑦 𝑕

Total Heat Capacity

𝑄𝑐𝑎𝑝𝑎𝑐𝑖𝑡𝑦 = 𝑄𝑇𝐸 𝑟𝑥𝑛 + 𝑄𝐷𝑀𝑇 = 501.6 𝑘𝑊 + 7.49 𝑘𝑊 = 509.1 𝑘𝑊

28
𝐵𝑡𝑢
𝑄𝑐𝑎𝑝𝑎𝑐𝑖𝑡𝑦 = 509.1 𝑘𝑊 = 1,737,121
𝑕𝑟

Natural gas will be used as fuel in the thermal fluid heater to heat the hot oil which runs through
the heating coils along the diameter of the heater. A schematic of the thermal fluid heater is provided
below showing how the heating happens in the interior.

(1) Top mounted burner Top mounted burner design with special cone design
produces a “narrow” long flame. By keeping the flame away
from the inner row of coils it avoids flame impingement on
the coils.
(2) Fluid inlet and outlet Fluid travels through a continuous closed loop system. The
fluid is pumped through the coils, to the fluid outlet, and
continues on through the entire system to the users.
(3) All safety and operating They are located in one central control panel.
controls
(4) Fan air inlet It is used for combustion

Figure 10: Fulton’s vertical coil thermal fluid heater design with descriptions [1]

29
The specifications for the thermal fluid heater is provided in the capacity charts shown in the
table below. We will use the 0240 model which has a heat output capacity of 2,400,000 Btu/h. This is
more than enough to provide for our heating.

Table22: Specifications for the four pass Fulton vertical coil thermal fluid heater [1]

7.5.2 Cooling Tower Utility


The use of a cooling tower in the plant will eliminate the need to rely solely on municipal water.
This requires the plant to only treat the make-up water instead of a constant treatment if only using the
municipal water. The cooling tower will be used for cooling the process water to 20 degrees C. This
water will be used by the following units as cooling water: E201AB, E202AB, E203AB, V201AB, V202AB
and V203AB as can be seen in the P&ID. It was determined that the cooling process can be
accomplished by using water, which prevents the usage of refrigerated water or refrigerated glycols
which will save money in operating costs. The parameters relating to the cooling tower can be seen
below. The cooling tower used will be an induced-draft tower utilizing a counterflow arrangement as
suggested in Perry’s Chapter 12 to be the most common and the most thermodynamically efficient. The

30
make-up water was calculated as a sum of the drift water, evaporated water, and the purge water; to
ensure the required water level is maintained

Table 23: Cooling tower specifications

Total Required Cooling Water 59.3 USGPM

Design Parameter 89.0 USGPM

Cooled Water 68 F

Process Water 118 F

Maximum Temperature for design 98 F

Make Up Water Neded 6.6 USGPM

Tower Radius 4.8 ft

Tower Height 21.0 ft

Fan Power 3.2 kW

* Design Parameters are calculated by using the guides and

graphs shown in Perrys Handbook Chapter 12

31
7.6 Pumps
Pumps were sized with respect to the required flow rate and net positive suction head, with
pump charts used as a reference to determine the power requirements. All pumps are centrifugal with
the exception of the vacuum pump, which is a rotary piston pump. Centrifugal pumps were selected
due their simplicity, capacity range, and ease of operation and maintenance [15].

Both piping and pumping are constructed with ANSI 304 grade stainless steel, except sections
handling propylene glycol, which is corrosive and requires more durable ANSI 316 grade steel. As DEG is
toxic, pumps handling any quantity of this fluid should be hermetically sealed to reduce the likelihood of
exposure. Pumps and lines handling molten DMT are heat traced to prevent solidification in the lines.
Table 24: Pump Specifications

Pump Function P & ID Capacity Power Additional Considerations


Reference per Pump per Pump
Name (m3/h) (kW)
To Feed Storage
To DEG stores P-101 34.0 19 Hermetically sealed
To PG stores P-103 37.9 19 Made of ANSI 316 grade steel
To DMT stores P-105 37.9 19 Heat-traced pump and line
To Reactor
DEG feed P-102 A & B 0.629 2 Hermetically sealed
PG feed P-104 A & B 3.43 2 Made of ANSI 316 grade steel
DMT feed P-106 A & B 4.29 2 Heat-traced pump and line
To Methanol Storage
Pumps methanol from P-201 A & B 1.13 2
TE stage to store
Vacuum Pump
Generates vacuum for P-202A & B 4 22 Rotary piston type pump
PC stage
To Glycol Storage
Pumps glycols from PC P-203 A & B 1.8 2 Hermetically sealed, made of ANSI
stage to store 316 grade steel
Glycol Recycle
Recycled glycol feed to P-204 1.71 2 Hermetically sealed, made of ANSI
reactor 316 grade steel
Cooling Tower
Cooling water pump P-401 A & B 20.2 30
Heater
Heating oil pump P-402 A & B 22.0 30 Insulated pump and line

32
8.0 Process Safety
8.1 Hazardous Conditions
There are several hazardous conditions that must be considered in the plant ranging from
operational, thermal process, and raw material hazards. The potential hazards in the plant include
ignition of flammable liquids causing fires or explosions, eye and skin irritation with the possibility of
causing blindness, inhalation of airborne vapours causing central nervous system depression, thermal
burns, etc. The majority of the hazards just mentioned come from contact with methanol as well as to a
lesser extent, molten dimethyl terephthalate (DMT), diethyl glycol (DEG), propylene glycol (PG), and the
hot oil.

8.2.1 Plant Classification (electrical safety)


The entire plant along with the control and lab room will be explosion proof. The facility will be able
to handle class I, division 2, groups C and D chemicals [22]. This will be done by the use of explosion and
static proof pumps for transporting of chemicals. All vessels/reactors in the plant will be well ventilated
with a nitrogen blanket on top in order to prevent airborne vapours which increase the risk of ignition,
especially for methanol with its low flash point. Class I refers to hazards through the presence of
flammable gases and vapours such as natural gas and methanol vapours in this case. Division 2 refers to
abnormal conditions and groups C and D chemicals include most of the usual class I chemical groups
[22].

8.2.2 Operational Safety


The required wearing of the proper personal protective equipment (PPE) such as safety glasses,
safety shoes, hard hats and leather gloves by the workers will greatly minimize the possibility of many of
the hazards mentioned previously. This mainly applies for transporting of chemicals and work related to
the hot oil unit. As mentioned previously, sufficient ventilation and nitrogen blanket will prevent any
inhalation hazards from airborne vapours for the operators. The supervisor will have a large
responsibility in ensuring safety protocols (handling procedures, PPE, etc) are followed by the workers.

The control instrumentation in the process will minimize any major hazards that can occur from
process failure and since the plant has two of everything due to using a two reactor system, it provides
redundancy and the process can still be ran efficiently while diagnosing any problems or hazards that
arise. There will be fire alarms around the facility with fire extinguishers and emergency exits in case a
fire breaks out. Eye wash stations will be placed near all chemical storage vessels and handling
areas/lab. MSDSes will be readily available in easily accessible areas for workers and weekly meetings on
operational safety will take place in order to ensure the staff is well informed of all hazards. The table
below lists important hazards and handling procedures for all materials used in the plant.

33
Table 25: Material hazards

Material Form Safe Handling Main Hazards


DMT Molten liquid  Do not handle near an  Exposure to powder or dusts
open flame, heat or may be irritating to eyes, nose
other sources of and throat
ignition.  May form explosive dust/air
 Use non-sparking tools mixtures if concentration of
when opening or closing product dust is suspended in
containers air
 Can cause thermal  May be ignited by heat,
burns, handle the sparks or flames
molten liquid with care
(wear PPE)

PG Colourless  Keep away from heat  Hazardous in case of ingestion


liquid and other sources of  May cause irritation if
ignition exposed to skin or eyes
 Ground all equipment  Flammable at high
containing material temperatures

DEG Colourless  Keep away from heat  Harmful if swallowed


liquid and other sources of  May cause irritation if
ignition exposed to skin or eyes
 Ground all equipment  Flammable at high
containing material temperatures
Methanol Colourless  No smoking or open  Inhalation of air-borne
liquid flame near handling vapours can cause headaches,
areas nausea, confusion, loss of
 Use explosion proof consciousness, disgestive and
electrical equipment visual disturbances and even
 Ensure proper death
grounding procedures  Moderately irritating to the
skin (effects similar to those
of inhalation)
 Swallowing small amounts
could potentially cause
blindness or death. Effects of
sub lethal dose are nausea,
headache, abdominal pain,
vomiting and visual
disturbances
 Easily ignitable (fire or
explosion), very low flash
point, keep away from
sources of ignition

34
8.2.3 Thermal Process Safety
Any hazards that arise from the thermal process units such as the thermal fluid heater, reactors
and DMT tanks are at a minimum. Temperature controls will ensure operations are within
bounds and the process reaction is an endothermic, equilibrium reaction so there are no issues
that can arise. In case of any leaks that occur within these units, the control room will pick this
up and appropriate action will be taken.

8.3 Waste Disposal


There is limited waste produced in the plant. The DEG and PG byproducts are recycled back into
the reactor for the next batch and the methanol byproduct is stored and sold. Service water
used for cooling is recycled back into the cooling tower and the hot oil is recycled back in the
hot oil unit. The purge for all these recycled loops will require some form of treatment or
disposal. The cooling water will be treated according to regulations and then disposed of; the
DEG, PG and methanol will be disposed of by means of a waste disposal company

35
9.0 Floor Plan

Rail Tracks

C T -4 0 1
54' 65' F -4 0 1

T K -1 0 1 A T K -1 0 1 A V- V-

E x p lo s io n
E -2 0 2 A 203B
202B

R -2 0 1 B 2 0T1- A E -2 0 1 A
V-
201A
P ro o f A re a

HM - T K -3 0 1 B T K -3 0 1 A
C B -3 0 1 C B -3 0 2
T K -1 0 2 B T K -1 0 2 A 301

52'
1 7 '-6 "

58'-6"
R -2 0 1 A 2 0T1- A E -2 0 1 B
V-
201A

V-
T K -3 0 2
V-
E -2 0 2 B 203A
202A
N itro g e n 4 7 ' -6 '’
T K -1 0 3 A T K -1 0 3 B

30'-0"
Lab

17' -6'’
T a n k F a rm A re a
C o n tro l R o o m N o n -E x p lo s io n
P ro o f A re a
N o n -E x p lo s io n P ro o f A re a

P a rk in g

Figure 101: Floor plan

36
The lot size of the plant layout seen in figure 8 is approximately 2 acres; however additional land will be
required to allow for acceptable commercial spacing. The explosion proof and non-explosion proof areas
have been indicated on the diagram with the exception of the hot oil unit containment area, F-401,
which will also be explosion proof.

Sarnia was chosen as the plant location since the area has housed large industrial ventures for decades
and is considered to be international leaders in chemical production with access to continental railways
and seaways. Consequentially, there is a large skilled industrial work force and the government is
providing incentives to promote new growth in the area including endorsing environmentally friendly
processes. The local government has provided several large business parks, including an additional 100
acres this year, to encourage new industrial growth. The price of land varies depending on several
variables including accessibility to water and railway. The cost of land for required property with railway
access is approximately $200,000 Canadian.

10.0 Economic Analysis


10.1 Capital Costs, Installation Costs and Expense/Fees

Table 26: Overall Capital Costs

Factor
Component Cost Used Cost
Direct Plant Cost
Equipment Cost 100 $5,831,367
Piping 0 0
Auxilary Systems &
Services 12 $699,764
Electrical 10 $583,137
Instrument and Control 10 $583,137
Civil Work 20 $1,166,273

Total Direct $8,863,678

Indirect Costs
Engineering and
Supervision 12 $699,764
Contingency 10 $583,137

Total Capital Costs $10,146,578

37
Table 27: Raw Material Prices & Costs

Propylene Glycol Diethyl Glycol Dimethyl Terephthalate


(PG) [16] (DEG) [17] (DMT) [18] Methanol Total
FOB Contract price (US$/ton) $1760.00 $1345.00 $1400.00 $350.00
Amount per batch
(ton/batch) 3.536 0.704 5.156 1.67

Cost per Batch (US$) $6223.36 $946.88 $7218.40 $584.50 $14,389


Cost per Batch (CAD) $6136.23 $933.62 $7117.34 $576.317 $14,187

Cost per Day (CAD) $12272.47 $1867.25 $14234.68 $1152.634 $28,374

Cost per Month (CAD) $368173.98 $56017.42 $427040.54 $34579.02 $851,232

Cost per year (CAD) $3608104.98 $548970.72 $4184997.33 $338874.396 $8,342,073


Revenue/ year (methanol) $338,874

38
Table 28: Equipment Capital Costs

Unit 1: Upstream Capital


Cost
per Number Capital
Tanks: Unit ($) of units Cost ($)
TK 101 A/B 108796 2 217592
TK 102 A/B 44496 2 88993
TK 103 A/B 255121 2 510243

Pumps: P 101 85600 1 85600


P 102 A/B 28600 2 57200
P 103 74600 1 74600
P 104 A/B 19000 2 38000
P 105 85600 1 85600
P106 A/B 24900 2 49800

Unit 2: Processing
Reactor: R 201 A/B 462407 2 924814

Exchanger: E 201 A/B 46996 2 93992


E202 A/B 35825 2 71649

Column: T 201 A/B 373389 2 746778

Tanks: V 201 A/B 45007 2 90015


V 202 A/B 41476 2 82953
V-203 A/B 8477 2 16954
V 204 16992 1 16992
TK 201 135813 1 135813

Pumps: P 201A/B 19000 2 38000


P 202 A/B 79400 2 158800
P 203 A/B 22500 2 45000
P 204 A/B 22500 2 45000

Unit 3: Downstream
Equipment: CB 301 376601 1 376601
HM 301 56287 1 56287

39
Silos: TK 301 A/B 485538 2 971076
TK 302 185830 1 185830

Transport: CB 302 17600 1 17600

Unit 4: Utilities
Equipment: F 401 183650 1 183650
CT 401 89334 1 89334

Pumps: P 401 A/B 61700 2 123400


P 402 A/B 76600 2 153200

Capital Cost
(equipment) $5,831,367
*All capital costs for the equipment were calculated using Don Woods’s Bare Modulus Method, except
where noted in Section 6. This method allows for considerations for piping, material, pressure,
installation and any other major considerations specific to each case.

10.2 Operating Costs

Table 29: Plant Operating Costs

Water
Total Cost (Hourly, after first 6000
m^3) $2.007 $/h
Total Cost (Daily, after first 6000 m^3) $48.163 $/day
Total Cost (Annually) $24148.46 $/yr
Oil
Total Cost (Annually) $41571.66 $/yr
Natural Gas
Total Cost (Hourly) $12.332 $/h
Total Cost (Daily) $295.959 $/day
Total Cost (Annually) $87011.91 $/yr
Electricity
Total Cost (Daily) $769.158 $/day
Total Cost (Annually) $226067.50 $/yr
Labour
Total Cost (Hourly) $132.38 $/h
Total Cost (Daily) $3177.12 $/day
Total Cost (Annually) $934073.3 $/yr
Total Operating Cost
Annual $1312873 $/yr

40
The electricity and natural gas rates used for this estimate were the 2009 rates for the city of
Toronto. Water rates used were the 2010 rates for the city of Toronto [19]. Labour costs were estimated
using an online database of national salaries [20]. Lighting cost was estimated by comparing the size of
our plant to a lighting cost estimate for another industrial manufacturing plant [21].

10.3 Income statement over 12 years accounting period


An analysis was completed on the financials for the proposed plant and the data in the following
table are the major conclusions.

1. The project will produce an estimated 25 million dollars (Net Present Value) over 12 year plant
life according to the profit loss statement seen in figure 11
2. The minimum to charge for the product for the project to break even; covering the cost of the
loan, interest (5%; Prime +2%), and operating costs is $3.58/kg, see figure 13.
3. If the resin is sold at $5/kg, the lower end of the market value for a high quality polymer resin,
the project will produce a 36% rate of return.
4. Varying the selling price from $5/kg to $7/kg changes the payback time from 3.5 to 1.5 years,
see figure 12. A selling price of $5/kg allows for a reasonable payback time of 3 years and yields
a NPV of $25M (using 5% interest) see figure 14.
5. Raw feed prices are the major expenditure for the plant; An increase of 20% in the raw feed
prices increases the payback time from 3 years to 5 years at the recommended selling price,
based on the conclusions above, see figure 15.
6. The breakdown of the selling price is shown in figure 17.

This is an income statement over 12 years for the proposed plant. The inputs for the income
statement are based on the previously calculated values for capital costs, operating costs, and material
costs. The tax rate is from the generally accepted accounting principles (GAAP).

41
Figure 11: Accounting statement for the plant based on a 5% and $5/kg selling price

42
100

80

60
NPV ($Millions) 40

20

0
1.5 2.5 3.5 4.5 5.5 6.5 7.5 8.5
-20

-40

-60
Selling Price ($/kg)

Figure 12: Sensitivity Analysis on the selling price NPV vs selling price ($/kg) for a 5% interest rate for borrowing after 12 year
plant life

10.3.1 Sensitivity Analysis on the selling price

70
60
50
40
30 $5/kg
NPV

20 $6/kg
10 $7/kg
0
-10 0 2 4 6 8 10 12
-20
Period (Years)

Figure 15: NPV vs year for varying selling prices

43
10.3.2 Sensitivity Analysis on the raw feed prices
15

10
NPV ($Millions)
5
Raw Price (100%)
0
Raw Price (105%)
-5 0 2 4 6 8 10 12
Raw Prices (110%)
-10

-15
Period (years)

Figure 136: NPV vs year for increasing raws cost

10.4 Acid Route Alternative Analysis


The acid route alternative was also analysed to determine the impact that it would have on the
bottom line. Main considerations when determining the alternative route analysis were:

 Only slightly less capital than in the DMT route. The acid route does not require methanol
condensers, a packed column, glycol condenser, or methanol storage tanks. However, the acid
route will be run under pressure, which will require the equipment used to be pressure rated,
increasing the cost.
 The cost of acid route raw materials is less expensive which is the major difference between the
two methods
 The product produced is the exact same quality and is therefore sold for the same price in the
market.

A comparison between the two routes based on NPV and selling-point breakdown are available in
Figures 17 and 18, respectively.

44
50

40

30
NPV ($ millions)

Transesterification
20 Route
10 Direct Esterification

-10 0 5 10

-20 Period (years)

Figure 14: A comparison of the acid route vs the DMT route, based on NPV.

5
4.5
4
3.5
3
$/kg sold

Profit
2.5
Unit costs
2
1.5 Raw costs

1
0.5
0
Acid Route (Alternative) DMT Route (Proposed)

Figure 15: Selling price breakdown; showing profit, unit cost of manufacturing, and raw costs

45
11.0 Conclusions/Recommendations

The plant design outlined in this report includes several unique aspects such as use of two
reactors running off-cycle, and the use of molten DMT. Using selling price of 5 $/kg, which is at the low
end of the market price, the plant design in this report yields a net present value of $25,400,000 over 12
years. Adjusting the selling price of the product towards 7 $/kg at the high end of the market yields a net
present value of nearly $60,000,000. Due to the profitability of the plant in its current state and the
flexibility of the outlined plant design, notably the ability to run two different products off-cycle should
the market change significantly in the near future; it is recommended that further development of this
project be approved.

46
12.0 Acknowledgments

We wish to thank Dr M. Saban for his continued support throughout this term. Without the support and
extensive knowledge in scale up design this report would have been significantly different. Thanks for a
great term.

We also wish to thank Y. Sanchez for his support with Aspen to size specific equipment needed to
complete the report.

Lastly, thanks to the team at XRCC for the tour of the Pilot Plant to help us gain some practical
knowledge that helped greatly in determining the practicality of out suggestions.

Team Magenta

4W4 Poly, 2011

47
13.0 References
[1] Polyesters, Vol 12, Chemical Engineering 4W04 2010-2011. Provided by Dr. Saban

[2] Dynatrol (2008) Viscosity Mesurement and Control Equipment [Online]. Available:
http://dynatrolusa.com/products/dynatrol-viscosity-probe.htm

*3+ “High efficiency hydrofoil agitators”; ProChem Inc. Mississauga, Ontario; Chemineer HT agitators

*4+ “Baffle Sizing”, Hayward Gordon Ltd; Section TG6, page 6.01-6.12, July 2000.

*5+ “Chemical process equipment: selection and design”; James R. Couper, W. Roy Penney, James R. Fair;
Chapter 10: Mixing and Agitation; Elsevier Inc, 2010

[6] ITT Standard (2011). SSCF – stainless steel shell & tube heat exchangers. Standard Shell & Tube.
Available:
http://www.ittstandard.com/Tools/Portfolio/frontend/item.asp?type=9&size=0&lngDisplay=4&jPageNu
mber=5&strMetaTag=
[7]Couper, J., Penny, W., Fair, J., Walas, S. (2010). Chemical Process Engineering. Burlington, M.A.,
United States: Elsevier Inc.

[8] Hoon, C., Ling, A. (2007). Distillation Column Selection and Sizing. Taman Tampio Utama, Malaysia:
KLM Technology Group.

[9] Geankoplis, C. (2003). Transportation Processes and Separation Process Principles. Upper Saddles
River, N.J., United State: Pearson Education Inc.

[10] Tank Connection, Tank Capacity Calculators, Water and Wastewater, 2004.
http://www.waterandwastewater.com/resources/capacity_calculators/index.php

[11] CEI Enterprises. Vertical Tanks for Modified Asphalt. Astec Industries, Inc. 2011
http://www.ceienterprises.com/downloads/cei_tankline.pdf

[12] Lemanco. Lemanco Welded Silo Capacity Chart. Chief Industries, Inc. 2008
http://www.lemanco.com/html/silo_capacity_chart.html

[13] Sandvik – your partners in melt granulation systems, Sandvik, 2007.


http://www.sandvik.com/sandvik/0140/internet/s001664.nsf/3aa39d675f7cc278c12569b900513b28/c3
9993f6c144db58c12577c90035f40c/$FILE/PS-442-ENG-07.pdf

[14] Mill Power Tech, Mill pulveriser, http://www.mill.com.tw/products-hammer-mill_english.htm

[15] Girdhar, P., Moniz, O. (2004). Practical Centrifugal Pumps. Burlington, M.A., United States: Elsevier
Inc.

[16] ICIS Pricing. Propylene Glycol (PG) Prices and Pricing Information. Reed Business Information Ltd.
2011.
http://www.icis.com/v2/chemicals/9076442/propylene-glycol/pricing.html

[17] CMAI. Ethylene Glycol, Oxide & Derivatives Market Report. CMAI Global. 2010

48
www.cmaiglobal.com/Marketing/Samples/EOEG.pdf

[18] ICIS Pricing. Dimethyl Terephthalate (DMT) Prices and Pricing Information. Reed Business
Information Ltd. 2011
http://www.icis.com/v2/chemicals/9075278/dimethyl-terephthalate/pricing.html

[19] City of Toronto Website, http://www.toronto.ca/invest-in-toronto/utilities.htm

[20] Payscale for Employers, http://www.payscale.com/hr/default?cmpid=70140000000Xsa6

[21] ReliablePlant Website, http://www.reliableplant.com/Read/28285/How-must-costs-run-equipment

[22] United States Department of Labor. Hazardous (Classified) Locations, Osha.

http://www.osha.gov/doc/outreachtraining/htmlfiles/hazloc.html

49

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