Cryogenic Air Separation

For the Production of Nitrogen

CLEVELAND STATE UNIVERSITY

April 29, 2013

Authored by: Jaclyn Demyan, Todd Siwik
Table of Contents
Abstract ................................................................................................................................. 2

Introduction ........................................................................................................................... 3

Project Description .............................................................................................................. 3

Safety, Regulations and Codes ............................................................................................ 4

Technical Discussion .............................................................................................................. 6

Basis of Design ................................................................................................................... 6

Alternatives ......................................................................................................................... 6

Process Description ............................................................................................................. 7

Compressor ..................................................................................................................... 9

Removal of Impurities .................................................................................................... 10

Heat Exchanger .............................................................................................................. 11

Distillation Column ........................................................................................................ 11

Turbine .......................................................................................................................... 12

Scale-up .............................................................................................................................. 13

Process Description ........................................................................................................... 13

Compressors ................................................................................................................. 13

Removal of Impurities .................................................................................................... 14

Turbine .......................................................................................................................... 14

Cold Box ........................................................................................................................ 14

Control System .............................................................................................................. 15

Piping ............................................................................................................................ 17

Storage and Transportation of Liquid Nitrogen ............................................................... 19

Carbon Footprint ........................................................................................................... 20

Land and Utility Requirements........................................................................................ 20

Economic Analysis ................................................................................................................ 21

Conclusion and Recommendations ....................................................................................... 23

1
Abstract
Nitrogen gas is a very common requirement in several industries today. The purpose
of this report is to provide the design of a cryogenic air separation plant for the production of
nitrogen gas. First, a pilot plant must be constructed to provide all calculations and proof of
concept. Then, the pilot plant will be scaled up to a full production plant. The pilot plant
must produce 20,000 SCFH of nitrogen gas with a minimum purity of 99 volume percent. In
addition to the nitrogen gas, liquid nitrogen must be produced at a rate of 10% of the gas
production. After completion of the pilot plant design, it must be scaled up to a full size
production plant producing at least 600,000 SCFH of nitrogen gas with the same minimum
purity.

After design of the pilot plant, equipment was selected for the full production plant.
The system first compresses air from the atmosphere to about 11 bar with an Ingersoll Rand
model number C3000 centrifugal air compressor. After compression, the feed stream enters
a temperature swing adsorber (TSA) to remove remaining water, carbon dioxide, and
contaminants in order to prevent damage to cryogenic equipment. 13X and F-1 alumina
zeolites will be used in the TSA. The feed stream proceeds to the multi-cell heat exchanger
to reduce the temperature to 110 K by utilizing the waste and product streams from the
distillation column. After the feed stream is cooled, it enters the distillation column, with a
temperature of 110 K and a pressure of 10.1 bars, where nitrogen is separated from the
remaining components. The mostly pure nitrogen stream leaves the top of the column as the
oxygen rich waste stream is drained from the bottom. The waste stream is flashed to further
reduce its temperature and fed to the column condenser to liquefy some of the product gas.
After the condenser, the waste stream enters the heat exchanger, cooling the feed. The
nearly pure distillate leaves the column and is partially condensed in the column condenser.
The liquid nitrogen is sent to on-site storage tanks. This liquid nitrogen is stored to be
vaporized into nitrogen gas to be used during plant start-up as well as sold during plant
shut-downs. The remaining nitrogen gas, with a purity of 99vol%, is sent to the heat
exchanger to further cool the incoming feed air. A small portion of this gas is removed to
provide the nitrogen purge necessary for the coldboxes. The remaining nitrogen gas is
pumped through a pipeline to be sold to local customers.

After the design of the full production plant was complete, an economic analysis was
performed to ensure profitability. The process was found to be profitable and construction of
the plant is recommended.
2
Introduction
More than three fourths of the Earth’s atmosphere is made up of nitrogen gas. Just as
it is common within the atmosphere, nitrogen gas is also common in many industrial
processes. Nitrogen is an inert gas and limits oxidation when used in place of standard air.
Because of its properties, one of the highest industrial uses of nitrogen is within the drilling
industry. “Used both in onshore and offshore situations, applications for nitrogen include
well stimulation, injection and pressure testing, Enhanced Oil Recovery (EOR), reservoir
pressure maintenance, nitrogen floods and inert gas lift. Additionally, nitrogen can be used
to help prevent flammable gases from igniting and protect tubulars from downhole (sic)
corrosion.” (Generon IGS, 2010) In addition to its use within the drilling industry, nitrogen is
vital to the production of electronics, polymers, and within fuel systems on military aircrafts.

There are several options for companies who require nitrogen gas. When large
quantities of nitrogen are required at a plant, the nitrogen can be delivered as a liquid or gas
and stored on-site in storage tanks. Nitrogen gas can also be delivered by local pipeline, as
with this case study. The final option is to separate air on-site to obtain the required
nitrogen. For this case study, a plant will be designed for the purpose of providing nitrogen
gas to local companies via a pipeline. Additional profits can also be made by transporting
liquid nitrogen to customers. A detailed description of the project specifications can be
found below.

Project Description
Company A has requested the design of a nitrogen plant within the Akron/Canton,
Ohio. The production requirements of the plant are 600,000 SCFH of nitrogen with a
minimum purity of 99 volume percent. The design must also allow for the production and
storage of liquid nitrogen at about 10% of the gas production. This liquid nitrogen shall be
available such that it can be vaporized into gaseous nitrogen to off-set high peaks in demand
as well as plant shutdowns. Company A requires the construction of a pilot plant with the
ability to produce 20,000 SCFH of nitrogen at the above stated specifications. This will be the
basis of the plant design. This pilot plant will then be scaled to the required 600,000 SCFH.
Below you will find the results of the pilot plant study as well as the recommendations for
scaling to the required full plant specifications.

One thing must be noted in regards to measurements within this report. Standard
cubic feet per hour (SCFH) are a volumetric flow rate of gas corrected to “standardized”

3
temperature and pressure. However, there is no universal definition of what this standard
temperature and pressure should be. (SCFM versus ACFM and ICFM) For the purpose of this
paper, the standard temperature and pressure will be 60 degrees Fahrenheit ( 289 K) and
14.696 pounds per square inch (1.01 bar), respectively.

Safety, Regulations and Codes

Cryogenic materials are very cold substances. Hazards associated with cryogenic fluids
include personnel exposure, high pressure gases, material and construction compatibility,
and asphyxiation.

Cryogenics can present physiological hazards such as severe cold burns or frostbite
which may be inflicted if the cryogenic material or cooled materials comes into contact with
the human body.

Consideration must be taken in the selection of materials due to the effects of low
temperatures on the properties of those material. Thermal stresses, over pressurization of
equipment, and brittle fracture are all hazards which can occur due to the cryogenic process.
ASME codes B31.1 through B31.7 contain relevant information regarding materials compatible
with the products and temperatures they encounter.

Potential hazards exist in highly compressed gases because of the stored energy.
Cryogenics liquids vaporize with a change ration of volume up to 900, this can cause violent
changes in pressure especially if in confined areas. All cryogenic systems are equipped with
pressure relief devices to prevent excessive pressure buildup.

The most significant risk of cryogenic liquids is death by asphyxiation where a spill or
leakage depletes the atmospheric oxygen. If the oxygen concentration falls below 18%
adverse effects will occur resulting in loss of mental alertness and performance combined
with distortion of judgment. In atmospheres containing less than 10% oxygen death by
asphyxiation is rapid: just two breaths of oxygen-free air kills.

Transportation of cryogenic substances is covered in the US Department of

Transportation (DOT) 49 CFR 173, which covers mass/volume of goods that may be
transported, correct packaging and labeling as well as vehicle usage, driver training and
duties of responsibility.

4
 Training should be given in all aspects of the handling of cryogenic materials. It is
important that personnel have an understanding of the risks involved and where to obtain
information. Proper personal protective equipment (PPE) should be worn during the normal
handling of cryogenic materials.

Some major environmental laws which were taken into consideration were the Clean
Air Act regulates sources of air pollution such as manufacturing plants and the Clean Water
ACT (CWA) is an amendment to the Federal Water Pollution Act in 1977 which regulates the
discharges of pollutants to waters.

5
Technical Discussion

Basis of Design
The design of this nitrogen production plant is based on the production of 20,000
SCFH of nitrogen with a minimum purity of 99 volume percent. For simplification purposes,
the feed air is assumed to be at 283 K and 1.01325 bars. Air contains nitrogen, oxygen,
carbon dioxide, argon, water, and trace amounts of various other components. The pie graph
below shows the makeup of these components by volume percent. The water content of air is
dependent on the temperature and will vary from day to day operation of the plant.

Composition of Air by Volume

0.03% 0.93%

20.95%
Nitrogen

Oxygen
78.09% Carbon dioxide

Argon

Graph 1: Composition of Air (Air Composition, 2011)

Alternatives
Although cryogenically separating air was suggested for this plant, time must be taken
to fully eliminate other options. There are two widely used processes to separate air:
adsorption and membrane separation. Within adsorption processes, there are three methods
to divide air into pure gases. These include pressure swing adsorption (PSA), vacuum swing
adsorption (VSA) and a combination of the two, known as vacuum pressure swing adsorption
(VPSA). All of these adsorption methods utilize aluminosilicate minerals, also known as
zeolites, to separate the product gas from the remaining air. Generally, multiple beds of
zeolites are used so that one bed filters the air while the other bed is regenerating. Pressure
swing systems operate at near-ambient temperatures and rely on the properties of the
zeolites and specific pressures to adsorb the unwanted gaseous components. While under
high pressure, the unwanted gases are adsorbed by the packed bed and the product gas

6
continues out of the system. The pressure between the beds is then switched and the first
bed releases the waste gas from the zeolite under lower pressure. This swing between
pressures allows for continuous production of the target gas. Although vacuum swing
adsorption systems are similar to pressure swing, they allow for greater efficiency, reduction
in maintenance, as well as cost savings. A vacuum swing system operates at near ambient
temperature and pressure. The feed gas is drawn into the system over the zeolite bed to
separate the gases. When the system switches to the second bed, the initial zeolite is
regenerated by subjecting it to a vacuum. The lower pressure allows for the waste gas to be
released and removed from the system. Maintenance costs are reduced on this system
because the difference in pressure between the two stages is lower than the difference in a
pressure swing system, limiting the deterioration of the zeolite beds and reducing the
amount of dust particles that leave the system. By combining these two types into a vacuum
pressure swing adsorption (VPSA) offers the best efficiency. In VPSA systems, the feed gas is
drawn into the system at a higher pressure and regenerates the waste bed under a vacuum.
Although any three of these systems are capable of providing the purities required for the
case study, they are unable to produce gaseous nitrogen in the required amounts.

The last possible alternative is membrane separation of air. Membrane separation is

based on the difference of permeation components of the feed gas. Depending on the
required product gas, a membrane is selected. The driving force for the separation is
provided by the difference of partial pressures on each side of the membrane. The air is
pressurized and then fed over the hollow-fiber membrane where the product gas diffuses
through the membrane while the waste gases exit the system. Membrane separation
produces lower purity gases compared to the other alternatives discussed.

Each of these alternatives is not suitable for this case study because they are unable to
produce nitrogen at the required purities at the necessary production needs. An extremely
simplified illustration depicting the cryogenic separation of air can be found in the appendix.

Process Description
In cryogenic distillation, air is drawn into the system from the atmosphere and
liquefied by compressing and cooling the air. This liquefied air can then be distilled to
separate nitrogen from the remaining components of air. First, the air is compressed to
about 10 bar. Then the high pressure air is fed to a temperature swing adsorber where
carbon dioxide, contaminants, and remaining water are removed. The “clean” air is then

7
cooled to cryogenic temperatures by utilizing the waste and product streams within a four
chamber heat exchanger. The feed stream is then sent to a distillation column that produces
a distillate of nearly pure nitrogen gas and a bottom product of oxygen rich liquid. The liquid
is flashed to reduce the temperature to provide refrigeration for the condenser. After the
condenser, the bottoms product goes to the heat exchanger to cool the incoming feed. To
recoup some energy to power the compressor, the waste stream is expanded through a
turbine. It is then fed through the heat exchanger a second time. The waste stream is then
released to the atmosphere. The nearly pure nitrogen product stream is fed to the heat
exchanger to cool the feed stream. The product stream is then split. Nitrogen gas is
required for the coldbox surrounding the heat exchanger and distillation column and
additional nitrogen gas is liquefied for storage. The remaining product stream is pumped
through pipelines to local customers. Figure 1 below shows the process flow diagram. This
is followed by a detailed analysis of each piece of equipment for the design of the pilot plant.

Figure 1: Process Flow Diagram for Cryogenic Distillation of Nitrogen

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Compressor
To compress the air, a few variables must be taken into consideration including
required flow and required pressure. The necessary outlet pressure is about 10 atm with a
flow rate of about 55,000 SCFH. The correct type of compressor must be chosen to achieve
these specifications.

There are three different types of compressors; reciprocating, rotary screw, and
centrifugal. Reciprocating and rotary screw compressors are both positive displacement
compressors. Positive displacement compressors increase the pressure by decreasing the
volume of the gas. Reciprocating compressors contain a piston within a cylinder to reduce
the volume of the gas. These compressors are simple in design and have lower installation
costs but are not designed to run at full capacity 24 hours a day, 7 days a week. Rotary screw
compressors decrease the volume of air with the use of two or more rotors, or screws. Rotary
screw compressors are designed to run 100% of the time and are the most popular type of
compressor within plants. The last type of compressor, a centrifugal compressor, is
considered dynamic because it relies on a transfer of energy to increase the pressure of a gas.
Angular momentum from a rotating impeller spinning at high speeds is transferred to the
gas, producing a higher pressure. These compressors can be designed to reach flows of over
20,000 cfm at 125 psig. (Types of Air Compressors)

For the design of the pilot plant, the best selection would be a rotary screw
compressor. This compressor can be either oil free or oil flooded to reduce the heat created
by compressing air as well as lubricate the internal mechanisms. A comparison of these
methods is listed below in Table 1.

9
 Comparison of Oil Free and Oil Flooded Rotary Screw Compressors

Oil Free Oil Flooded

Rotors turn at high speeds
High compression temperatures
Higher maintenance requirements and
cost
Requires larger HP motor
Water cooling required
No additional filtration needed
Table 1: Oil Free vs. Oil Flooded Compressors (Air Systems International, 2011)
Rotors turn at lower speeds
Low compression temperatures
Lower maintenance requirements and
costs
Smaller HP motor and more energy
efficient
Air cooling
Additional filtration required to remove oil
from product

Although using an oil flooded compressor will introduce contaminants to the feed gas,
full package filter systems built into the compressor are available that are guaranteed to
remove all contamination. The higher cost of a filtration system will be offset by the savings
in maintenance costs and energy efficiency. With a smaller motor, less energy is required.
Theoretically, 170 HP is required to produce air flow of 55,000 cfh at a pressure of 10 bar. By
adding an additional 20% to compensate for friction and real life conditions, the required HP
is a little over 200. (Horsepower required to Compress Air, 2011) This cost of energy is one
of the biggest concerns when selecting a compressor. To reduce this energy need, the
process will also contain a turbine to recoup some energy from the waste stream to power the
compressor.

Removal of Impurities
Air quality is critical to cryogenic processes. Because of the extremely low
temperatures of the main components within the system, it is critical to remove all water and
contaminants from the incoming air stream. If water is allowed to enter the cryogenic
equipment, it will freeze, damage equipment, and reduce the flow of the feed stream.
Contaminants, especially hydrocarbons, can damage cryogenic equipment as well as reduce
the ability of the system to effectively separate nitrogen.

To remove contaminants from the air before it is cooled, a temperature swing adsorber
(TSA) will be used. This TSA functions much like the pressure swing adsorbers described in
the alternatives section of this report. Two separate zeolite beds are used to remove water,
carbon dioxide, and other contaminants. The feed air flows through the first bed where

10
contaminants are removed. This stream continues on to the heat exchanger. When
breakthrough, the point when the zeolites are near full capacity, is about to occur, the first
bed is taken off-line, and the feed stream is directed to the second, fresh bed. While the
second bed removes contaminants, the first bed is regenerated with hot purge gas at about
520 K. This purge gas is released to the atmosphere. When all contaminants are removed
from the first bed, a cool down period begins to return the bed to operating temperatures. At
this time, the feed stream is switched back to the first bed and the cycle begins again.

F-200 Alumina and 13X will be used to remove water, carbon dioxides, and other
contaminants. From an incoming feed rate of 18,670 lb/hr and assumed cycle length of 12
hours, 890 cubic feet of alumina is necessary to remove water within the feed air and 14
cubic foot of 13X is necessary to remove carbon dioxide and any remaining water. This will
require a tower with working dimensions of about 11.4 feet high with a diameter of 5 feet for
alumina and about 0.2 feet high with the same diameter for the 13X. It is assumed that all
contaminants are removed by this TSA system and the feed stream that leaves the packed bed
is composed of nitrogen, oxygen, and argon. Using the Ergun Equation, the pressure drop
across the tower can be calculated. The pressure drop must be determined to ensure that the
feed stream enters the distillation column at the correct pressure to produce the specified
product. Using this equation, it was determined that the pressure drop across the packed
tower is negligible.

Heat Exchanger
The compressed dry air is cooled to cryogenic temperatures in a series of four
consecutive heat exchangers which are combined as one main heat exchanger unit in the cold
box. This main heat exchanger utilizes the product and waste stream thermal properties to
cool the air to near its liquefaction temperature (around 110 K) before it enters the distillation
column. The distillate product stream minus the 10% which is liquefied, and the bottoms
product from the distillation column will be used to cool the air process stream.

Distillation Column
The main piece of equipment in the process is the distillation tower which is the
largest unit of equipment and allows for the separation of nitrogen to take place. The
distillation column will have a feed of compressed cooled air at 10 atm and – 163 oC. The
column contains 25 stages and the feed is introduced into the column above tray 17. The
column will be several stories high. The column produces distillate product of nitrogen at

11
99.5% purity which comes out as a gas at -169° C. The bottoms waste product, which will be
recycled for cooling contains less than 3% nitrogen and exits the column at a temperature of
-153° C. This bottoms stream which comes out as a liquid will be used to condense part of
the distillate stream to produce liquid nitrogen.

Turbine
Energy can be recovered from the waste stream to offset the cost of running the
compressors. Gas expansion turbines are often used for this purpose. A turbine is used to
convert internal energy of a high pressure stream into shaft work. An expansion turbine is
considered a reaction turbine that produces torque by “reacting” to the pressure of the
incoming gas stream. The outlet pressure from the turbine will be 1 atm in order to recover
the most energy. The incoming pressure to the turbine is about 5.7 atm at a temperature of
130 K. Knowing the incoming pressure, desired outlet pressure, and incoming temperature,
the outlet temperature and recovered power can be calculated. Assuming a turbine efficiency
of 95%, the outlet temperature is 81.6 K with about 18 kW of energy recovered. Although this
does not seem like a substantial amount of energy recovered compared to the 140 kW
requirement of the compressor, using a turbine will reduce energy needs as well as reduce
the overall carbon footprint.

12
Scale-up

Process Description
When a pilot plant is scaled up, the designing engineers face many challenges. Scaling
up from a pilot plant to a full production plant is not a linear transformation. Pilot plants are
used to establish a basis for designing a full production plant and offer a “proof of concept.”
Within pilot-scale equipment, certain aspects of a process can be examined and optimized to
provide a better foundation for the full production plant. By using the previously discussed
analysis of the pilot plant, a solid design for the full production plant can be made. Each
piece of equipment is reanalyzed to ensure the product specifications are reached.

Compressors
In the pilot plant, a rotary screw oil filled compressor was used to compress the air to
about 10 bars. When scaling up, a larger flow of air is needed. There are two different ways
to achieve a larger flow of air. Rotary screw compressors are limited to about 150,000 cfh.
Seven compressors would need to be run in parallel to reach the required 900,000 cfh flow
required for the process. The other option is to purchase a centrifugal air compressor which
is capable of producing higher flow rates at the required pressure. A brand new 250 hp
Chicago Pneumatic Rotary Screw Air Compressor, model number CPF-250, will cost about
$98,500. Seven of these units will cost $689,500. One multistage centrifugal air
compressor, manufactured by Ingersoll Rand, will cost $124,300. In addition to the cost
difference between the two options, energy requirements, noise production, and footprint are
substantially less for the centrifugal air compressor. For these reasons, the Ingersoll Rand
model number C3000 air compressor will be purchased for the plant. Table 2 below lists
some standard features and benefits to purchasing this air compressor.

Ingersoll Rand Centac C3000

Standard Features Benefits

Compact package on rigid baseplate No special foundation required
Mounted intercoolers and aftercooler Compact efficient design
Baseplate mounted control panel Pre-wired and factory tested
Fewest electrical hook-ups Minimal installation time and cost
Table 2: Standard Features and Benefits of Ingersoll Rand Centac C3000 (Ingersoll Rand, 2011)

13
Removal of Impurities
To scale up the TSA for use on a 600,000 SCFH plant, the increased air flow must be
considered. The incoming air flow for the full size plant is 68,682 pounds per hour. This will
require a tower with working dimensions of about 29 feet high with a diameter of 6 feet for
the alumina and 0.5 feet high with the same diameter for the 13X. Again, the pressure drop
is calculated to ensure the desired specifications are met. The pressure drop in the larger
column is larger, as expected, but can still be considered neglible. The pressure drop is
about 0.3 bar.

The TSA can be constructed or purchased. Parker’s Finite Airtek Filtration Division
sells a heat reactivated desiccant dryer, model number TWB9000, which can be loaded with
the 13x and F-200 alumina. When purchasing a pre-fabricated unit for TSA, the working
volume for each zeolite must remain the same regardless of design. At the time of this
report, financial data and necessary design required was not available. From known
specifications of the TWB9000, required flow and output requirements can be met. (Parker
Hannifin Corporation, 2012) For a constructed TSA, the Guthrie method was used to
determine the cost of construction. Both the cost of the vertical vessels and the cost of the
adsorbents must be accounted for. Because the TSA is before the process streams are at
cryogenic temperatures, carbon steel can be used for construction. The vessels will cost
about $56,500. The adsorbents will cost about $200,000 and can be purchased from BASF.
(BASF Catalysts LCC, 2007) The adsorbents will have to be replaced on a regular basis.

Turbine
Although the incoming temperatures and pressures will remain about the same for the
scaled up plant, the amount of air flow will increase, increasing the energy produced by the
turbine. With preliminary calculations, the turbine will produce about 100 kW of energy. The
selected compressor requires over 2,000 kW of energy. The cost of purchasing and installing
a turbine to expand the waste stream is more expensive than the amount of energy
produced.

Cold Box
Insulation must surround several pieces of process equipment in order to ensure they
are able to perform at cryogenic conditions. The heat exchanger, distillation column, and
piping must be enclosed in what is commonly known as a “cold box” to reduce heat gain.
Cold boxes generally consist of a carbon steel casing and insulation material in an inert

14
atmosphere. The most common type of insulation is perlite. Perlite is a siliceous volcanic
rock that expands when heated. Although the design of a cold box is extremely complex, the
full design is not within the scope of this project. Cold boxes can be purchased with all of
the necessary connectors, valves, monitoring equipment, as well as ladders and platforms.

Two separate cold boxes will be purchased. One will surround the heat exchanger
while the other will contain the distillation column. Two boxes will be used to reduce damage
to the perlite insulation and equipment in the case of an emergency. The cold boxes can be
purchased from Chart Industries. Chart can provide a BAHX (brazed aluminum plate-fin heat
exchanger) with the cold box as one unit ideal for air separation. A specific volume of perlite
will be necessary for the BAHX. Chart Industries can also manufacture a cold box for the
distillation column.

The cold box must also contain a nitrogen purge system that will provide a continuous
nitrogen supply during operation to eliminate moisture and air from the interior. If air comes
into contact with the process equipment, it will liquefy and create oxygen-rich pools that if
warmed, can vaporize and destroy the perlite insulation. The nitrogen purge also prevents
moisture from entering the area. Moisture within the cold box can also destroy the
insulation. (Asia Industrial Gases Association, 2005) Industry standards call for the
continuous purge to be set at a rate of one volume change of the cold box every 24 hours.
This nitrogen purge can come from the product stream of the system. (Chart Energy and
Chemicals, Inc. , 2009) The foundation for the coldboxes must be monolithic. This means
that the foundation must be one continuous slab of concrete with no seams or joints. The
area directly underneath the walls of the coldbox must also be reinforced.

Control System
Controls for the system will be purchased from ABB Inc. Their Symphony Plus™ system
is a distributed control system that targets key focus areas of the plant including plant
productivity, energy efficiency, operation security, plant safety, and cost of ownership. The
system will include all require hardware, software, training, and installation. Sensors are
needed to measure conditions and provide output information to the control system. The
control system then uses this information to provide feedback to the input actuators that will
make necessary changes to ensure that the process remains within control and producing the
product at the required specifications. Figure 2 below depicts the basic piping and
instrumentation drawing.

15
 Figure 2: Control System

In this process, there are very few actuators that can be adjusted to correct process
control. Although this is true, almost every stream within the process must be measured to
ensure proper equipment operation. There are several critical areas within the process that
must be under constant surveillance. These include the entrance to the heat exchanger, the
cold boxes, and the product stream. The stream entering the heat exchanger must be free of
water and contaminants in order to eliminate damage to sensitive cryogenic equipment. If
water is allowed to enter the extremely low temperature areas, it could freeze and ruin the
most expensive pieces of equipment. The same is true for the cold boxes. A constant
nitrogen purge is fed to the cold boxes to eliminate moisture that could damage the
insulation. Damage to the insulation would require a full plant shut-down that would be
detrimental to plant profits. The product stream must be watched carefully as well to
guarantee the correct product specifications are available for customers. Negative public
relations caused by the delivery of inferior products to customers could easily shut down
plant operations.
16
 By installing a continuous control system, such as the Symphony Plus controls, the
process can be observed and necessary changes be made in real time to safeguard the
equipment and products. The controllers provided are a high performance and high capacity
process controller. The controllers contain the control algorithms and user configurations to
provide input to the actuators throughout the system. The controllers and most
communication lines within the system are “hot stand-by” redundant. The purpose of this
redundancy is to provide a constant back-up in the case of failure within the primary module.
Another benefit of using the Symphony Plus system is the capability to interface with third-
party devices. ABB systems have the ability to communicate with a variety of communication
protocols and communication media. Several pieces of equipment, such as the air
compressor, can be purchased with standalone controls. ABB’s system can connect to these
built in systems to reduce the cost of hardware and provide central control of the process.

This system also includes “S+ Operations,” a human machine interface that provides
information integration and user navigation within a Windows environment. S+ Operations
provides the users with detailed process overview displays, flexible reports, performance
monitoring, and streamlined maintenance. Data from the system is stored in a “historian” to
allow for archival of system collected data. This data can be accessed instantaneously to and
can be used to analyze disturbances, compare trend data, and compile reports. S+
Operations also provides an emergency shut-off protocol that when instructed, will halt
production. This emergency shut-off is in addition to programed shut-off procedures that
would be activated under specified unsafe process conditions. (ABB, 2013)

The complete turnkey control system, including control room furnishings, necessary
training, and installation, can be purchased from ABB for about $476,400.

Piping
Piping, as simple as it sounds, requires additional attention when designing a
cryogenic process. The materials used in this process are exposed to a wide range of
temperatures and pressures. Common construction materials such as standard carbon steel
and aluminum are not suitable for all areas of the plant. Common piping solutions for
cryogenic processes include insulating with foam or vacuum. Figure 3 below shows a
comparison of foam insulated piping, dynamic vacuum insulation, and static vacuum piping.
(Weiler, 2004) Although there are several piping systems in existence, the most efficient
systems utilize vacuums. There are two main types of vacuum systems. The first utilizes a

17
pipe within a pipe design and is known as the dynamic vacuum system. The inner pipe is
constructed of copper and is insulated by a vacuum produced by a continuously running
pump. Although the vacuum decreases heat loss, the cost of such system due to installation
and maintenance requirements makes this option ineffective. This type of system would be
more effective for small scale plants. The second option is a static vacuum jacketed system.
Similar to the dynamic system, a pipe within a pipe is used to insulate the process streams
with a vacuum. The difference is in how this vacuum is applied. In a static system, the piping
is constructed in sections, with each section independently sealed. The piping is installed
with bayonet style fittings that provide very low energy loss. Although the initial construction
and installation costs are more expensive for a static vacuum system, the cost savings from
drastically reduced energy usage and maintenance make this the best selection for cryogenic
piping.

Chart Industries can provide a full “Modular Vacuum Insulated Pipe System constructed
of T304 Stainless steel inner pipe and outer jacket. The system utilizes vacuum insulated
bayonets for quick and flexible installation without welding and cutting.

Figure 3: Comparison of Common Cryogenic Piping

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Storage and Transportation of Liquid Nitrogen
Storage tanks are required on-site to house the liquefied nitrogen. As discussed
earlier, this liquid nitrogen can be sold as production allows as well as vaporized into
nitrogen gas during plant maintenance, unforeseen shut-downs, and increases in market
demand. The storage tanks for the proposed facility will be purchased from Universal
Industrial Gases, Inc. based out of Pennsylvania. The cryogenic tanks contain perlite
insulation between an ASME U rated inner vessel and an SA-36 carbon steel outer vessel. The
capacity of the selected tanks, model 80000, is 78,406 gallons. If 14 of these tanks are
stored on-site, they will house enough liquid nitrogen to provide about 1 week of nitrogen
gas at standard production rates to the plant. It will take approximately 70 days for these
tanks to be filled at regular production rates. The fill rate of the storage tanks is also affected
by the rate of transporting liquid nitrogen off-site.

Transportation of liquid nitrogen requires specialized equipment. Universal Industrial

Gases, Inc. can also provide ASME U rated transportation trucks. These trucks contain all
necessary piping and pumping drives necessary to deliver liquid nitrogen to customers. The
trucks contain 3 transverse baffles within the inner vessel, surrounded by composite
insulation and a high strength carbon steel outer jacket. The evaporation rate of the vessels
is less than 0.6%. UIG can provide trucks ranging from 6,000 gallons to 8,600 gallons,
depending on transportation needs.

One truck with a capacity of 8,600 gallons is capable of transporting half of the daily
produced liquid nitrogen. If this liquid nitrogen is transported on a daily basis from the
beginning of production, it will take a little over five months to completely fill the 14 storage
tanks on-site under ideal conditions. If it is assumed that one week of planned maintenance
will be completed every six months, this scheme of 14 storage tanks and one transportation
truck will be sufficient. Additional research should be done to verify the needs of the current
liquid nitrogen market within the Akron/Canton area.

The design of the tank farm is very elaborate and must take many things including
safety and hazard potential into consideration. This design is not within the scope of this
project. Estimates can be made however to determine the area needed for the tank farm.
According to industry standards, a three foot buffer zone is needed between the tanks. The
tank model selected has dimensions of 125 feet long by 12 feet wide with a height of 12.4
feet. With the need of 14 tanks, the tank farm will be about 0.6 acres. To account for the

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necessary area of the concrete pad as well as a containment system, this value will be
estimated as 0.8 acre.

Carbon Footprint
Climate change is a major challenge facing the global population and the natural
environment. A carbon footprint measures the total greenhouse gas emissions caused by an
organization. Causes of these emissions include electricity production in power plants,
heating with fossil fuels, transportation operations and other industrial processes. A carbon
footprint can be quantified using indicators like the Global Warming Potential (GWP). A GWP
as defined by the Intergovernmental Panel on Climate Change (IPCC) , is an indicator that
reflects the relative effect of a greenhouse gas in terms of climate change. The GWP’s for
different emissions can be added together for an overall contribution to climate change from
the emissions.

Although the cryogenic air separation plant will release some carbon dioxide back into
the atmosphere the main carbon footprint will be due to the energy consumption of the plant.
All of the processes for air separation are very power intensive. Accounting for the energy
which the ASU consumes and the carbon dioxide that will be released the ___ . This is below
the nessasary amount to even require a permit which under ___ is needed for __

This noted a company should know their carbon footprint.

Land and Utility Requirements

The footprint of the proposed 600,000 SCFH plant is about 5 acres. When determining
a suitable location for the construction of the plant available utilities, correct zoning
requirements, as well as vicinity to major transportation should be considered. A possible
location was located on Kropf Ave in Canton, Ohio. This location is zoned I-1 and I-2
(industrial) and is 14.5 acres. The property has access to water and sewer and is within 2
miles of Interstate Highway 77. This particular location contains a 4,500 square foot metal
building that can be converted into office space. The advertised price is currently at
$699,000 but because this lot has been on the market for over 6 months, and considering
the current economy, the reduction of this price is expected. The other benefit to purchasing
this large plot of land is the ability to sell or lease unused acreage and also have the
capability to expand.

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Economic Analysis

Estimating the cost of equipment and capital investment can play a crucial role in
selecting the design of a process. Attempt was made to procure an estimate for each of the
units in the process, land, materials, and utility requirements. Where a quote was not
obtained the pricing was calculated through other means. The cost of the heat exchanger was
estimated from the heat transfer area required, the purchase cost of the distillation column
was estimated from the height and diameter of the tower using the method of Mulet,
Corripio, and Evans which is a method based on the weight of the shell. The method includes
an allowance for platforms, ladders, and a nominal number of nozzles. (Seider et al) The
purchase cost of each of the units can be viewed in the chart below.

Initial investment Cost per year

Heat Exchanger $594,641.22 Labor $1,518,458.40
Distillation column $2,363,517.69 Power/Utility $4,922,126.10
TSA $2,389,739.89
Storage Tanks $359,471.36
Cold box $2,769,137.59
turbine $33,636.01 Nitrogen Sales per year $11,592,000.00
pumps $700,000.00
filter $73,803.94
Land $699,000.00
Table 3: Purchase Cost of Equipment

Taking the initial investment, the cost per year on labor and power and utilities, and
the sale of nitrogen per year the following chart shows the net profit per year and return on
investment.

Year Net profit per year Return on Investment

0 -$9,982,947.69 -$9,982,947.69
1 $5,151,415.50 -$4,831,532.20
2 $5,151,415.50 $319,883.30
3 $5,151,415.50 $5,471,298.79
4 $5,151,415.50 $10,622,714.29
5 $5,151,415.50 $15,774,129.79
6 $5,151,415.50 $20,925,545.28
7 $5,151,415.50 $26,076,960.78
8 $5,151,415.50 $31,228,376.28
9 $5,151,415.50 $36,379,791.77
10 $5,151,415.50 $41,531,207.27
Table 4: Net Profit per Year and Return on Investment

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 The following two graphs show the net profit per year and the return on investment. As
you can see from the second graph and the table above the ASU will take only two years to
return on the initial investment. From this analysis the ASU proves to be a good investment
with a short term return. It should be noted that this analysis is done for a ten years however
replacing material such as the packing in the TSA and perlite was not taken into account
which will lower the net profit in the 5-10 year period.

Cost/profit per year

$10,000,000.00

$5,000,000.00

$0.00
0 1 2 3 4 5 6 7 8 9 10
-$5,000,000.00

-$10,000,000.00

-$15,000,000.00

Graph 2: Cost/Profit per Year

Return on Investment
$50,000,000.00

$40,000,000.00

$30,000,000.00

$20,000,000.00

$10,000,000.00

$0.00

-$10,000,000.00 0 2 4 6 8 10 12

-$20,000,000.00
Year

Graph 3: Return on Investment

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Conclusion and Recommendations
o In conclusion, the proposed design of construction for the 600,000 SCFH
nitrogen production plant will be profitable.
o Additional profits can be realized with the sale of liquid nitrogen. The local
market within the Akron/Canton area should be analyzed to correctly regulate
the production and sale of the liquid nitrogen.
o Other alternatives to the temperature swing adsorber should be researched
further.
o The production of additional pure components is possible with the addition of
multiple columns. The available market for pure oxygen and argon, as well as
the cost of additional equipment should be analyzed.
o It is also possible to expand the waste stream as discussed in the paper to
recover energy. Expansion of the product stream is also an option. An analysis
of expanding multiple streams should be done to determine if energy recovery
is profitable.

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