Production of medium pressure nitrogen

by cryogenic air separation*

Rakesh Agrawal and Robert M. Thorogood

$rrducts and Chemicals, inc., 7201 Hamilton Boulevard, Allentown, PA 18195-l 501,

This paper concentrates on cryogenic process cycles for producing medium pressure nitrogen
(pressure over 5.5 bar (abs.)) at relatively high purity (oxygen concentration under 5 ppm). The major
inefficiencies of the conventional waste-expander cycle in a single distillation column were identified as
a starting point. These were removed by synthesizing a series of novel cryogenic nitrogen generators in
which the expander bypass flow was reduced and converted to a recycle flow to the distillation column.
The novel generators retain the convenient and efficient features of the conventional waste-expander
cycle while achieving applicability over a much wider range of production rates and product
pressures.

Keywords: cryogenic air separation; nitrogen; waste-expander cycle

Introduction remained the workhorse of the cryogenic air separation

industry’.‘. Several variations of this double-column
Nitrogen produced by cryogenic separation of air
process can easily be used for the production of nitrogen3.
(composition of air: 78.1% N,; 21.0% OI and 0.9% Ar) has
Even though many of the double-column processes are
been widely used in many industrial applications. It is
energy efficient, they are fairly capital intensive4. They use
used as an inert gas for purging equipment and for
two distillation columns rather than one and most of the
performing operations on materials that require an
nitrogen is produced at a pressure signiticantlylowerthan
oxygen-free atmosphere. Typical industries that use
that of the feed air. This usually requires that a compressor
nitrogen are chemicals. metal, glass. textile, electronics,
be used to compress the product nitrogen. For the
etc. Nitrogen product requirements vary significantly
majority of users requiring less than 200 t d-’ of nitrogen,
between various industries: some need nitrogen with
at pressures in the range 5-10 bar (abs.), it has been
fairly high purity (0, concentration less than 5 ppm),
attractive to reduce capital cost by minimizing the
while others can operate with percentage O2 impurity
number of distillation columns and eliminating the
levels. The pressure of the nitrogen product required also
nitrogen compressor.
varies with the type of industry. For example, the
As a result, a process cycle that is widely used in the
electronics industry requires that extremely pure nitrogen
industry to produce MP nitrogen is the single-distillation-
be supplied at a pressure of about 7-10 bar (abs.).
column waste-expander process shown in Figure 15-‘. This
This paperwill concentrate on cryogenic process cycles
process is preferred for its flexibility to produce nitrogen at
for producing medium pressure (MP) nitrogen (pressure
different pressures (5.5 to 9.6 bar (abs.)) without product
over 5.5 bar (abs.)) at relatively high purity (oxygen
compression. This is particularly attractive for the
concentration less than or equal to 5 ppm). A typical
electronics industry, where it is desirable to avoid the
process cycle currently being used to produce this MP
possibility of contaminating the final nitrogen product in
nitrogen will be described first. Its benefits and short-
a compressor. Significant quantities of liquid nitrogen can
comings will be discussed. followed by a description of the
also be recovered by this process.
evolution of more energy-efficient process cycles which
In this process cycle, atmospheric air is filtered and
still retain the operating and capital advantages of the
compressed to about 1 bar above the nitrogen product
current process.
delivery pressure. The compressed air is cooled and the
condensed moisture is removed in a condensate separator.
A typical cryogenic process cycle to Air enters a molecular sieve system where the water
produce MP nitrogen vapour, carbon dioxide and most hydrocarbon con-
taminants contained in the air feed are adsorbed. The
A double-column arrangement to produce oxygen was
clean air then enters the insulated cold box, which
proposed by Carl Von Linde in 1910 and since then it has
contains all the cryogenic equipment.
The clean feed air enters the main heat exchanger
*Paper presented at GAS Separation International, Austin, TX, USA,
22-24 April 1991 where it is cooled to near its dewpoint by the product
Please note this work is the copyright of Air Products and Chemicals, Inc. nitrogen and oxygen-rich waste streams. The cooled air

0950-42 14/9 l/040203-07

0 199 1 Butterworth-Heinemann Ltd Gas Separation Et Purification 1991 Vol 5 December 203
Medium pressure nitrogen generation: R. Agrawal and R.M. Thorogood

as an oxygen-rich stream at a moderate pressure. Since

this oxygen-rich waste stream is typically not a desired
product, the efficient recovery of energy from this stream
is a major challenge. Some of this energy is constructively
used to provide the refrigeration for the process by the
near-isentropic expansion of the waste stream. However,
the flowrate and pressure of the waste stream are usually
such that an expansion of all the waste stream would
provide excess refrigeration. This problem of excess
refrigeration has been overcome in two ways: (1) producing
excess liquid product from the cold box and vaporizing it
Figure 1 Nitrogen generator: conventional waste-expander
process outside the cold box, or (2) bypassing a fraction of the
waste flow around the expander and letting its pressure
down across a Joule-Thompson (JT) valve as shown in
stream is fed to the bottom of a single distillation column Figure 1. Both of these methods waste a fraction of
where it is distilled to nroduce a nure nitrogen stream at pressure energy contained in the pressurized feed air.
the top and an oxygen-rich liquid stream ycalled crude resulting in process inefficiency. ‘\
LOX) at the bottom of the distillation column. A portion The magnitude of this problem increases as the
of the nitrogen stream from the top of the distillation pressure of the nitrogen product stream (and hence of the
column is warmed in the main heat exchanger to provide distillation column) is increased. An increase in the
the desired pressurized nitrogen product stream. The product nitrogen pressure generates the waste stream
other portion of this nitrogen stream is condensed at the from the vaporizer-condenser at increased pressure.
top of the distillation column and is used as reflux. A Furthermore, increase in the column pressure decreases
small portion of the condensed nitrogen can be collected the relative volatility of nitrogen with respect to oxygen
as liquid nitrogen product. The crude LOX from the and argon and leads to more nitrogen being lost in
bottom of the distillation column is let down in pressure the crude LOX. This also increases the waste flow.
and vaporized in heat exchange with the condensing The increasing inefficiency of this process is a major
nitrogen stream to provide the vaporized waste stream. handicap in its utilization for the production of large
The vaporized oxygen-rich waste stream is partially quantities of nitrogen at higher pressures.
heated in the main heat exchanger, then expanded in a In order to quantify this inefficiency, as a function of
turbo-expander. The near-isentropic expansion of the nitrogen product pressure, an all-gas product plant
waste stream provides the refrigeration needed for the (Figure I) was simulated (no liquid nitrogen is produced
process. The expanded cold waste stream is rewarmed in from this plant). The nitrogen product contained 5 ppm
the main heat exchanger and exits the cold box. A portion oxygen. Calculations were first done for the case where the
of the waste stream is used to regenerate the molecular nitrogen product is produced at the lowest possible
sieve system. The other portion of the waste stream is pressure. This pressure is defined as the pressure of
vented-directly to the atmosphere. nitrogen that results in a waste stream with the right flow
Although the waste expander cycle has been widely and pressure combination from the vaporizer-condenser
used for nearly three decades, it has some deficiencies, to provide exactly the quantity of refrigeration needed
which have occasionally limited its use. Since the from the expander. No waste flow is bypassed around the
distillation column does not have a stripping section expander and no liquid product is produced. For the
below the air feed, the minimum nitrogen content of the chosen process parameters the minimum pressure of the
liquid (crude LOX) leaving the bottom of the distillation nitrogen product is about 4.5 bar (abs.). (It should be
column is that which is in equilibrium with the feed air at noted that in actual plants some liquid products are
column pressure. This relationship limits the recovery of always produced. This requires more refrigeration. which
the nitrogen product to 35-45% of the air feed for the invariably results in the nitrogen product pressure being
typical column pressures in the range 6-10 bar (abs.). So greater than 4.5 bar (abs.).)
the crude LOX/waste stream flow is about 55-65% of the For the all-gas plant under consideration, the waste-
air feed. As the pressure of the column is increased, the expander cycle of Figure 1 can be used in two ways to
recovery of nitrogen decreases. supply a nitrogen product at pressures greater than 4.5 bar
The pressure at the top of the distillation column sets (abs.). In method 1, nitrogen is directly produced from the
the temperature of the condensing nitrogen stream. For a cold box at the desired pressure (and the surplus
given vaporizer-condenser design, the temperature refrigeration capacity is wasted). In method 2. nitrogen is
difference (AT) between the condensing and the boiling produced at 4.5 bar (abs.) from the cold box and is then
fluid is set by: the required heat transfer duty. the fluid compressed in a nitrogen compressor to the desired
dynamics of the fluid flows involved, and by their heat pressure. Power consumption by method 2 is the lowest
transfer coefficients. Typical ATs are in the range 1.5-3°C. power to produce nitrogen at high pressures using this
The composition ofthe crude LOX and the temperature at waste-expander cycle. Figure 2 compares relative power
which it boils determines the pressure at which the waste consumed by method 1 with that of method 2. for different
stream must be vaporized. So, as the pressure of the product pressures. As the pressure of the nitrogen product
column is increased, the pressure of the vaporized waste is increased, the energy penalty associated with the direct
stream can also be increased. For a column pressure of 5.5 production of pressurized nitrogen from the cold box
to 10 bar (abs.), the pressure of the vaporized waste stream increases sharply. At a product pressure of 7.8 bar (abs.).
is in the range of 2.5 to 6.0 bar (abs.). method 1 consumes 24% more power than method 2.
The distillation column and its overhead condenser The severe energy penalty associated with the pro-
thus permit the recovery of a large fraction of the feed air duction of the pressurized nitrogen directly from the cold

204 Gas Separation & Purification 1991 Vol 5 December

 Medium pressure nitrogen generation: R. Agrawal and R.M. Thorogood

1.5 alternative solutions that do not require any nitrogen heat

pump. These flowsheets will now be described in the
balance of this paper. Exergy analyses leading to some
1.4 of these process cycles can be found elsewhere’*.

Development of novel processes

1.3
It is clear from the discussion that the major source of
inefficiency in Figure 1 arises from bypassing a fraction of
k the waste flow around the expander and letting down its
g 1.2
P pressure across a JT valve. Indeed, it has been shown that
F
for a nitrogen product pressure of 7.9 bar (abs.), about 41%
._
5 1.1
of the total cold-box exergy loss is due to this expander
d bypass”. An objective of all the solutions discussed in this
paper was to eliminate this loss by eliminating the
expander bypass flow. These solutions can be divided into
1.0
two broad categories: those that require no changes to the
distillation column configuration and those that do.
0.9
Solutions with no changes to the distillation column
The most obvious way to reduce loss across the expander
L I I I I I
bypass valve is to expand only that portion of the oxygen-
4.5 5.5 6.5 7.5 8.5 9.5 10.5
rich waste stream that is needed for the cold-box
N2 Product pressure (bar Cabs.11 refrigeration. The balance of the oxygen-rich waste flow is
warmed through the main exchanger, providing a
Figure 2 Power consumption by method 1 as compared to
pressurized stream. The challenge is economically to
method 2 for the conventional waste-expander process as a function
of the nitrogen product pressure: method 1, pressurized nitrogen recover energy from this pressurized oxygen-rich stream.
directly from the cold box; method 2, nitrogen at 4.5 bar (abs.) from A trivial solution is to expand this stream at ambient or
the cold box and then compressed to the desired pressure higher temperature in a turbine and recover energy.
However, for sizes up to 200 t d-’ of nitrogen production,
the flowrate of this stream is so small that the cost of a
box led Ruhemann and Limb5 to conclude that plants turbine cannot be justified; so. alternative more efficient
using the waste-expander cycle are best used for column solutions were sought. To facilitate comparison of alter-
pressures around 8 bar (abs.) and for quantities less than native process cycles, it is useful to hold certain parameters
3000 Nm3 h-‘. Ayres ef al.’ describe its use for nitrogen fixed, so that differences in cyclescan be clearly identified.
production up to 10 000 Nm3 h-’ and pressures up to For the work reported here: nitrogen product pressure was
9.5 bar (abs.). fixed at 7.9 bar (abs.): no liquid nitrogen was produced;
the number of theoretical stages of distillation was fixed,
Alternative processes for production of as were the vaporizer/condenser AT and the heat leak
MP nitrogen from the ambient to the cold box. The oxygen concentra-
tion in nitrogen was 5 ppm. The relevant process para-
Studies have been made in the past to improve the meters are summarized in Table 1.
efficiency of the waste-expander cycle to enhance its In the first solution. the pressurized oxygen-rich stream
applicability over a much wider range of plant sizes and is recycled by mixing it with the feed air providing a new
nitrogen pressures. It is fairly well known that overhead feed stream for the cold box (Figure.?). In the preferred
vapour can be used as a heat-pump fluid in certain mode, this stream is fed at an intermediate stage of the
instances to increase the efficiency of a distillation main air compressor”. Mixing the oxygen-rich waste
columnx-‘. For the waste-expander nitrogen generator of stream with air feed increases the concentration ofoxygen
Figure 1, it has been suggested that addition of a stripping in the feed to the cold box and. at first. might seem to be
section at the bottom of the distillation column with
nitrogen as a heat-pump fluid increases its efficiency
substantially”“‘. In these solutions. a high pressure
Table 1 Process specifications for computer simulations
nitrogen stream is recycled to provide the boil-up at the
bottom of the distillation column and the condensed Distillation section
nitrogen is fed at the top of this column as part of the Column tray count 50
reflux fluid. In another variation, a part of the feed air is Heat exchanger sections
boosted to a pressure higher than the column pressure Main exchanger NTU count 60-70
Overhead reboilerkondenser A.T (“F) [“Cl 4.35[- 15.361
and is used to provide some boil-up at the bottom of the
distillation column. The condensed liquid air is fed as Compressor/expander sections
Air feed temperature (“F)[“C] and 70[21 .l] and
impure reflux to the distillation column. These methods relative humidity (%) 50
increase the recovery of nitrogen to 75-90% of the nitrogen Isothermal efficiency (%) 70
present in the feed air, resulting in improved process Motor efficiency (%) 95
efficiency. Air compressor suction pressure 14.5
As stated earlier. there is always a finite possibility of (psi (abs.))
Expander efficiency (%) 85
contaminating a nitrogen stream in a compressor with No power credit for expander
trace impuritities. As a result. it was decided to explore

Gas Separation & Purification 1991 Vol 5 December 205

Medium pressure nitrogen generation: R. Agrawal and R.M. Thorogood

capital investment and thus make the suggested solution

quite attractive.
The biggest disadvantage of the WEWR-1 process is
that it is unable to fully exploit the benefit of the pressure
energy in the oxygen-rich pressurized stream from the
cold box due to losses associated with the mixing of this
stream with the feed air. In order to avoid the losses due to
mixing, two solutions were studied. In one ofthe solutions,
a separation device outside the cold box is used to perform
some separation on the oxygen-rich pressurized stream
such that the composition of the recycle stream is now
closer to air. For this purpose separation devices such as
Figure 3 Nitrogen generator: WEWR-1 membranes or adsorption units can be easily employed’4.
Even though more efficient process configurations using
membranes are discussed in reference 14, the simplest
undesirable for the production of nitrogen. However, it scheme used for the current study is shown in Figure4.
was found that the irreversible losses due to the expansion The only difference between this process and the one in
of the gas across the JT valve are greater than the Figure3 is that the oxygen-rich waste stream prior to
irreversible losses associated with mixing the oxygen-rich recycle is passed through a membrane unit. This mem-
stream with air; the result is an overall reduction in brane is more permeable to oxygen, and pressure on the
the power requirement. Some relevant results for the permeate side is maintained close to atmospheric. The
Waste Expander Waste Recycle-l (WEWR-1) process of nitrogen content of the non-permeate stream from the
Figure 3 are listed in Table 2. It can be seen from the results membrane is higher than the feed and this stream is fed to
that as the recycle flow to the main air compressor is an intermediate stage of the main air compressor.
increased, the concentration of oxygen in the main air Calculations were made for the process of Figure 4 by
compressor discharge stream is increased; and the flow using the standard conditions listed in Table 1. A
through the expander bypass JT valve is decreased. With membrane unit with oxygen: nitrogen selectivity of 8.3 was
the increase of oxygen in the feed to the cold box, the used. Argon was assumed to have the same permeability
concentration of oxygen in the waste stream increases as nitrogen. Feed to the membrane unit contained 35.6%
from 35.6% to 46.4%; and the recovery of nitrogen based on oxygen and its flow was 0.95 mol mall’ of nitrogen
fresh feed-air flow also increases. i.e. the fresh air feed product. Its pressure was 3.7 bar (abs.). About 64% of the
decreases. feed to the membrane was recovered as non-permeate
The most interesting finding is that the power consumed
by the proposed WEWR-1 process can be about 8-9%
lower than that required by the base case. As the recycle
flow is increased, the energy saving also increases, but it
quickly reaches a point of diminishing returns, i.e. the
energy difference between case I and the base case is large.
but the further reduction in going to cases II and III are
modest. This implies that as the concentration of oxygen
in the recycle stream is increased, the resulting increased
work of separation decreases the net benefit derived from
the utilization of its pressure energy.
By examining the processes shown in Figures 1 and 3, it
is clear that employing the present suggestion requires
some additional passages in the warm end of the main
heat exchanger and some piping to feed the recycle stream
to an intermediate stage of the main air compressor. These Figure 4 Nitrogen generator: waste expander with a membrane
changes should be minimal in terms of any additional

Table 2 Relevant results for WEWR-1 process (figure 3)

WEWR-1
Base case
(figure 7) Case I Case II Case Ill

Oxygen in feed to cold box (%) 21 24 26 29

Oxygen in waste stream (%) 35.6 40.1 42.6 46.4
Recycle stream flow - 0.41 0.59 0.84
Recycle stream pressure exit cold box (bar (abs.)) - 3.6 3.5 3.3
Expander bypass flow 0.97 0.60 0.48 0.35
Feed air flow 2.42 2.09 1.96 1.82
N2 recovery from air feed (96) 52.8 61.3 65.2 70.3
Specific power (kWh Nme3 N2) 0.256 0.240 0.236 0.234
Relative power 1 .o 0.94 0.92 0.91

aN, recovery is defined as a percentage of the total nitrogen in the feed air stream
Nitrogen product pressure, 7.9 bar (abs.). All flows are in mol mol-’ of nitrogen product

206 Gas Separation Et Purification 1991 Vol 5 December

 Medium pressure nitrogen generation: R. Agrawal and R.M. Thorogood

stream with nitrogen concentration similar to air. This is higher than that for the WEWR-1 process in Table2.
stream was then fed to the intermediate stage of the main The specific power for this process is about 20% lower than
air compressor. The power consumption for this case to that for the base case process of Fi&zueI and is more
produce nitrogen product at 7.9 bar (abs.) was efficient than the processes shown in Figures 3 and 4. For
0.218 kWh Nrne3 of nitrogen. This power is 14.9% lower comparison, when 7.9 bar (abs.) nitrogen is produced by
than the base case of F@re 1. Depending on the cost and method 2, described earlier, using the conventional
availability of such a membrane, the suggested solution process of Figure 1. the specific power consumption is
can be quite attractive economically. However, alternative 0.205 kWh Nmm3 of nitrogen. This power is similar to that
solutions without any membrane units, but requiring consumed by case II in Tuble3. The solution proposed
changes to the distillation column, were explored. allows the efficient production of pressurized nitrogen
without the use of a product nitrogen compressor and
Solutions with modifications to the distillation thereby eliminates the possibility of contaminating the
column gaseous nitrogen product.
One potential drawback of the WEWR-2 process is that
Figure 5 shows a second solution, which avoids the mixing
it requires a separate recycle compressor machine and
loss of the waste recycle flow15. In this WEWR-2 process,
reduces the possible benefit that can be derived by the use
rather than mixing the oxygen-rich pressurized stream
of one single compression machine as shown for the
from the cold boxwith the feed air stream, it is compressed
processes in Figures 3 and 4. Alternative schemes where
in a separate compressor and recycled as an additional
the pressurized recycle stream from the cold box is
feed stream to the bottom of the distillation column. A few
generated at a composition close to air were, therefore,
distillation trays (three to six) are used between the air feed
explored. For this purpose, separation by distillation was
and the recycle feed locations. The use of this recycle
performed on the crude LOX stream from the bottom of
stream allows the addition of a stripping section to the
the distillation column to yield two streams: one for
distillation column and reduces the nitrogen content of
recycle and the other for expansion to provide
the waste stream. This leads to increased nitrogen
refrigeration.
recovery and enhanced energy efficiency.
Figure6 shows one such solution”. In this process,
Table 3 lists some ofthe relevant results for the WEWR-
rather than adding a stripping section below the air feed in
2 process. The total number of trays in the distillation
the main distillation column, a stripping section at a lower
column were kept constant at 50, as shown in Table 1.
pressure is used above the vaporizer-condenser. This
Similar to the WEWR-1 process, the amount of the recycle
crude LOX from the high pressure rectifying column is let
stream can be controlled. Two cases were simulated for
down in pressure and fed at the top of a lower pressure
different recycle flows and results are compared with the
stripping column. This stripping column is a short
conventional waste-expander process of Figure I. As the
column with two to live theoretical trays for distillation.
expander bypass flow is decreased, the recycle stream flow
The boiling duty at the bottom of this column is, of course,
and its oxygen content is increased. As expected. the
oxygen concentration in the waste stream for this process

Figure 5 Nitrogen generator: WEWR-2 Figure 6 Nitrogen generator: WEDC

Table 3 Relevant results for WEWR-2 process (Figure 5)

WEWR-2
Base case
(Figure 1) Case I Case II

Oxygen in waste stream (%) 35.6 50.5 56.3

Recycle stream flow - 0.66 0.77
Recycle stream pressure exit cold box (bar (abs.)) - 3.2 2.9
Expander bypass flow 0.97 0.23 0.06
Feed air flow 2.42 1.71 1.60
N, recovery from air feed (%) 52.8 75.5 80.6
Specific power (kWh Nm-3 N2) 0.256 0.210 0.206
Relative power 1 .o 0.82 0.80

aN, recovery is defined as a percentage of the total nitrogen in the feed air stream
Nitrogen product pressure, 7.9 bar (abs.). All flows are in mol mol-’ of nitrogen product

Gas Separation & Purification 1991 Vol 5 December 207

Medium pressure nitrogen generation: R. Agrawal and R. M. Thorogood

Table 4 Relevant results for WEDC process (Figure 6)

Case I Case II Case III Case IV

Number of trays in short column 1 2

Nitrogen in recycle stream (%) 75.2 78.9 8?2 8z.l
Recycle stream flow 0.57 0.70 0:74 0.73
Recycle stream pressure exit cold box (bar (abs.)) 3.0 3.0
Expander bypass flow i.338 GO 0.15 0.15
Feed air flow I:81 1:ss 1.61 1.61
N, recovery from air feed (%)” 70.1 77.6 80.3 80.3
Specific power (kWh Nme3 NJ 0.220 0.213 0.2 1 1 0.21 1
Relative power to base case 0.86 0.83 0.82 0.82

aN, recovery is defined as a percentage of the total nitrogen in the feed air stream
Nitrogen product pressure, 7.9 bar (abs.). All flows are in mol mol-’ of nitrogen product

provided by the vaporizer-condenser located at the top of

the main rectifying column. The oxygen-rich stream from
the bottom of the short column provides the waste stream
to be expanded for refrigeration. The vapour stream from
the top of this column has nitrogen concentration similar
to air and is recycled by feeding it to an intermediate stage
of the main air compressor. It is worth mentioning that a
generalized distillation scheme with vapour recompression
from the stripping column such that the rectifying section
operates at a pressure higher than the stripping section
has been reported by Mah et al. “. Is. Celar er al. I9have used
a similar concept for the production of pressurized
nitrogen and low pressure pure oxygen products from air. Figure 7 Nitrogen generator: DCDR
Table4 lists some relevant calculation results for the
Waste Expander Double Column (WEDC) process of
Figure 6. The nitrogen concentration of the recycle stream bottom of this column. The pressure of this stream is
is very close to air and therefore it may be appropriate to further reduced and it is fed to another vaporizer-
name the recycle stream as ‘synthetic air’. This stream is condenser. The vapour from this vaporizer-condenser is
easily fed to an intermediate stage of the main air treated as a waste stream and is used to supply refrigeration.
compressor without much mixing loss due to difference in The vapour from the top of the short column is recycled as
compositions. It is clear from the table that three to four usual. Since nitrogen from the top of the main distillation
trays are sufficient for the short column. The nitrogen column is condensed in both the vaporizer-condensers.
recoveries and power consumptions for this process are for the same minimum temperature difference between
similar to the WEWR-2 process listed in Table_?. The the condensing and boiling fluids in each vaporizer-
additional capital cost incurred due to the addition of condenser. the pressure of the short stripping column in
about four trays above the vaporizer-condenser would be Figure 7 would be higher than the corresponding pressure
minimal. in Figure 6. As a result. the pressure of the recycle stream
Even though the above results are extremely for the waste expander Double-Column Dual Reboiler
encouraging, an exergy analysis was made to identify (DCDR) process of Figure 7 would be higher, leading to
further inefficiencies that could potentially be improved. more energy savings.
The methodology and results are reported elsewhere”. It Calculations similar to case III of Table 4 were made
was determined that a major source of inefficiency exists for the proposed DCDR process and the results are
in the vaporizer-condenser. This is due to the changes in summarized in Table 5. The only difference is that rather
composition and temperature of the boiling fluid along than three trays in the short column, four trays were used
the length of the heat exchanger. Since nitrogen is nearly in this column. As the pressure in the short column is
pure, its temperature does not change as it condenses. increased to 4.0 bar (abs.) from 3.0 bar (abs.) for the
However, the boiling fluid is an impure stream and it is WEDC process, the relative volatility of nitrogen with
coldest at the entrance to the heat exchanger and warmest respect to oxygen and argon drops and the number of
at the exit. The pinch or the lowest temperature difference trays has to be increased to maintain a similar nitrogen
between the condensing and the boiling fluid is at the exit concentration in the recycle stream. The specific power for
of the boiling fluid from the heat exchanger. In order to this case is 0.200 kWh Nm-’ of nitrogen; the lowest power
have a smaller mean temperature difference along the of all the processes discussed in the paper. A more
length of this heat exchanger, it is proposed that rather interesting observation is that the specific power for this
than boiling all the fluid in one heat exchanger it is boiled process is even lower than the corresponding value of
sequentially in two exchangers at different pressures. The 0.205 kWh Nrn-j of nitrogen when nitrogen is produced
solution based on this concept is shown in Figure 7’“.Thus by method 2 using the conventional process of Figure 1.
the crude LOX from the bottom of the main distillation This was also found to be true with calculations of
column is let down in pressure and fed at the top of the nitrogen production at 10 bar (abs.). It seems that the
short stripping column. Unlike the WEDC process of DCDR process is efficient even at much higher nitrogen
Figure6, now a liquid stream is withdrawn from the product pressures. This will allow high pressure nitrogen

208 Gas Separation 8 Purification 1991 Vol 5 December

 Medium pressure nitrogen generation: R. Agrawal and R.M. Thorogood

Table 5 Comparison of the two double-column processes

WEDC
Base case (Figure 6) DCDR
(Figure 1) Case III (Figure 7)

Number of trays in short column -

Nitrogen in recycle stream (%) - 872 8T.l
Recycle stream flow - 0:74 0.74
Recycle stream pressure exit cold box (bar (abs.)) - 4.0
Expander bypass flow 0.97 :.?5 0.15
Feed air flow 2.42 1:Sl 1.61
N, recovery from air feed (%) 52.8 80.3 80.3
Specific power (kWh Nmm3 N,) 0.256 0.21 1 0.200
Relative power 1 .o 0.82 0.78

‘N, recovery is defined as a percentage of the total nitrogen in the feed air stream to the compressor
Nitrogen product pressure, 7.9 bar (abs.). All flows are in mol mol-’ of nitrogen product

product to be obtained directly from the cold box without Drs K. B. Wilson and S. R. Auvil. Permission from Air
using a product nitrogen compressor. Products to publish this work is gratefully acknowledged.
It should be pointed out that even though two vaporizer-
condensers are used in the DCDR process, the total heat References
transfer duty for this process is no different from the
Ruhemann, M. TheSeparation ofGases Oxford University Press,
conventional waste-expander process of Figure 1.
2nd Edn (1952)
Therefore, the difference between the total heat exchanger Latimer, R.E. Distillation of air Chem EngngProg (1967) 63(2)
area is also small. Addition of a short column with a few 35
trays does not require much capital. The recycle stream is Tborogood, R.M. Large gas separation and liquefaction
compressed using the main air compressor. The total feed plants Cr?/ogenicEngineering (Ed. B.A. Hands) Academic Press.
London (1986) ch 16
flow to the cold box remains virtually unchanged. In 4 Agrawal, R. and Woodward, D.W. Efficient cryogenic
short, the additional costs associated with the DCDR nitrogen generators: An exergyanalysisGasSepBtrif(1991)5 (3)
process are minimal. As a result, the DCDR process can 139
be used at higher product pressures, where the conventional 5 Ruhemann, M. and Limb, D.I. Recent developments in the
waste-expander cycle becomes impractical due to its production of pure nitrogen IChemE Symp Ser No 79 (1983)
320
extremely low energy efficiency. The DCDR process 6 Ayres, C.L., Abrardo, J.M. and Himmelberger, L.M.
meets most of the objectives set for this development: a Developments in nitrogen generators Cryogenic Process and
relatively efficient process cycle has been synthesized Equipment (Ed. P.J. Kerney, N. Chatterjee. D.B. Crawford and
from the conventional waste-expander nitrogen generator M. El-Masri) ASME I55
I Isalski, W.H. Air separation processes Separation of Gases
in which the good features of the conventional process are Clarendon Press, Oxford (1989) ch 3, 51
retained, and its major inefficiencies are substantially 8 Flower, J.R. and Jackson, R. Energy requirements in the
decreased. separation of mixtures by distillation Trans Instn Chem Engrs
( 1964) 42 T249
9 Danziger, R. and Baumer, W. Distillation columns with
Conclusion vapor recompression Distillation ‘79; IChemE Symp Ser No 56
(1979) 4.1/15
An evolution of more- efficient cryogenic nitrogen IO Patel, S.U., Corrnier, T.E. and Wilson, K.B. Nitrogen
generators to produce pressurized nitrogen has been generator cycle US Patent 4400,188 (1983)
described. A widely used waste-expander single- II Agrawal, R. and Cormier, T.E. Process and apparatus for the
separation of air US Patenr 4.464.188 (1984)
distillation-column cycle was chosen as the starting point. I2 Agrawal, R., Woodward, D.W., Kleinberg, W.T. and Wilson,
Major inefficiencies of the conventional waste-expander K.B. Efficient processes to produce nitrogen by cryogenic air
cycle were identified: the expander bypass flow and the separation Proc Low Temp Engng Cnogen Conf 1990
boiling of an impure fluid in the vaporizer-condenser. Southampton. UK (17-19 July 1990) 04.1
I3 Agrawal, R. and Auvil, S.R. Process for the production of high
These inefficiencies were removed by synthesizing a series
pressure nitrogen US Patent 4872,893 (1989)
of novel cryogenic nitrogen generators. In all of these 14 Agrawal, R. and Auvil, S.R. Process for the generation of
solutions, the expander bypass flow was reduced and gaseous and/or liquid nitrogen US Patent 4.595.435 (1986)
converted to a recycle flow to the distillation column. Use I5 Thorogood. R.M.. Roden. T.M. and Houkins. J.A. Crvoeenic
of a small stripping section was found to be beneficial. process for &J, prdduction’with O2 enri&ed recycle Ui &$
4.867.773 (1989)
These nitrogen generators retain the convenient and 16 Thorogood, R.M. and Roden, T.M. N, generator with waste
efficient features of the conventional waste expander distillation and’recycle of waste distillation overhead US Parent
cycle. By decreasing major losses, applicability over a 4.848.996 (1989)
much wider range of nitrogen production rates and I? Mah, R.S.H.,Nicholas, Jr, J.J. and Wodnik, R.B. Distillation
product pressures has been achieved. with secondary reflux and vaporization: A comparative
evaluation AIChE J (1977) 23 (5) 651
18 Fitzmorris, R.E. and Mah, R.S.H. Improving distillation
column design using thermodynamic availability analysis
Acknowledgements AIChE J (1980) 26 (2) 265
The authors are grateful to Messrs T. L. Ratzell and T. M. I9 Celar, L., Sikora, J. and Chrz, V. Flexible process of oressure
nitrogen and low pressure oxygen production hoc XbIIth Int
Roden for providing computer simulations for the Congr Reji-ig Vienna. Austria (1987) 220
flowsheets. Rakesh Agrawal would like to acknowledge 20 Agrawal, R. High pressure nitrogen production cryogenic
the encouragement and technical discussions provided by process US Patent 4.927.441 (1990)

Gas Separation & Purification 1991 Vol 5 December 209