BOOK3.

MAIN PROCESS DESCRIPTION REVISION HISTORY

REVISION DATE REVISION DETAIL DESCRIPTION

A 11 2020 REVISION B OF THE OPERATIONS AND MAINTENANCE MANUAL

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BOOK 3 - MAIN PROCESS DESCRIPTION
SUBJECTS COVERED
 Introduction
 Process Air
 Air Chiller
 Adsorption
 Air Cycle Refrigeration
 Nitrogen Separation
 Oxygen Separation

INTRODUCTION

The Spruce7 series plants produce liquid Nitrogen and/or liquid Oxygen by the
cryogenic distillation of ambient air. This book provides a general description of
the process.
The support processes such as the lube oil and seal gas systems are described
in BOOK 4 of this manual.
The process description is best understood by following the flow schematics on
the Piping and Instrument Diagrams (P&IDs). Where applicable, equipment tag
numbers are provided.

Basic process description:

Process air is used both as a source of refrigeration and as a feed source for
the cryogenic distillation process in the columns.
REFRIGERATION
The Turboexpander generates a cold stream that provides the refrigeration
which is necessary to achieve cryogenic temperatures. This cold stream is used
in the Main Heat Exchanger (HE-501) to cool the incoming process streams
destined for the columns. Waste streams from the columns are also directed
through heat exchangers to cool feed streams.

PROCESS AIR

Process air enters the plant through the Air Compressor inlet filter. The
compressor is an electrical motor driven, three stage centrifugal compressor,
complete with accessories, piped, wired and baseplate mounted.
After the first and second stages are water-cooled intercoolers, and after the final
stage is a water-cooled aftercooler. Safety of operation is provided for as the

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compressor will shut down if excessive temperature, electrical overload
conditions, or system over pressure should occur.

AIR CHILLER
The first stage of the “warm end module” (air treatment module) is a mechanical
refrigeration chiller (R-600) that cools the compressed air to about 4 0C. As the
air is cooled most of its moisture is condensed in the evaporator and then
removed in the water separator/coalescer. This coalescer incorporates a
coalescing filter and an automatic drain valve. The automatic drain valve
minimizes air loss while facilitating water removal.

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ADSORPTION

The cool air then flows from the water separator into the “online” adsorption bed
that removes impurities such as water-vapor and CO2. The “regen” bed
undergoes regeneration while the active bed is “online”. Regeneration involves
heating the adsorber material with a low pressure stream of waste nitrogen from
the top column, to free and expel contaminants from the bed.

AIR CYCLE and REFRIGERATION

The dry, purified air leaving the online bed flows through the process air
particulate filter (removing any particulate matter that may have been introduced
from the molecular sieve) before branching into 2 streams:
 One stream joins the Turboexpander Loop (at the booster compressor
suction) as a refrigeration source.
 The other branch stream passes through a portion of the Main Heat
Exchanger (HE-501) and enters the Nitrogen Column (C-530) as high
pressure gas.
 The Turboexpander loop (the liquefaction portion of the plant) is
supplemented by the Turboexpander/Booster Compressor assembly
(TBX-401). The other principal components of the Turboexpander Loop
are the plate-fin Main Heat Exchanger (HE-501) including a Product Sub
Cooler and a JT (Joule-Thompson) valve (TCV-580).

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The stream flows to the Booster Compressor driven by the Turboexpander. It
leaves the Booster at 1300 kpag and is cooled to 38C in the air-cooled Booster
After-Cooler (HE-433).
The boosted air then flows to the Coldbox and into the Main Heat Exchanger,
where it is cooled further by exchanging heat with the counter-flow cold streams
from the Turboexpander exhaust and distillation waste gasses. The medium
pressure air (4.1 -5.5 bar) from the feed air valve to the column is also cooled in
the main heat exchanger in the same way.
The boosted high pressure air splits ¾ of the way down the Main Heat
Exchanger at a temperature of -124C. One stream of this HP Air enters the
turbine at -124C and 1300Kpa and is expanded down to -190.4C at near
atmospheric pressure. The expansion process (combined with the kinetic work
extracted by driving the Booster Compressor) cools the turbine exhaust air,

providing the refrigeration source for the column distillation process. This very
cold, low pressure air flows back through the Main Heat Exchanger, absorbing
heat from incoming counter streams and venting to the atmosphere..
The other branch of the high pressure stream continues down the remaining
length of the Main Heat Exchanger where it condenses and emerges as high
pressure, sub-cooled air at -188.6C. This stream expands to 0.24barg through
the JT expansion valve (TCV-580) into the Oxygen Column (C-531) as 3.5%
vapor and 96.5% liquid. This liquid provides the “reflux” for the distillation
process in the upper (Oxygen) Column.
The above description indicates that there are two air feeds to the distillation
columns:

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  One is the cold saturated vapor (410-550 kpag) that originated from the
Main Air Compressor. This stream moves through the online bed at 8.25
bar(g) but is expanded down to 4.10-5.50bar (equivalent to the high
pressure column) via FCV-495. The operating pressure of the lower
column is governed by back pressure of the upper column waste pressure
control valves and the amount of feed air required. The air feed to the
column enters the Main Heat Exchanger and is cooled against counter-
current low pressure streams to saturation temperature before entering
the high pressure Nitrogen column. This gaseous stream is the driving
force for distillation.
 The other feed is the boosted high pressure (1300kpa), sub-cooled (-
188.6C) air stream that is expanded into the low pressure Oxygen Column
via the JT valve. This liquefied stream enters the column at tray 10 at a
pressure of 23kpag and represents the main source of liquid in the upper
column.

In Oxygen mode 62.6% of the Main Air Compressor flow goes to the high
pressure column. 19.8% of the Main Air Compressor flow goes to the low
pressure column (via the booster) as the liquid source. 17.4% is used to boost
the turbine flow. In Nitrogen mode 45% of the Main Air Compressor flow goes to
the high pressure column. 19.5% of the Main Air Compressor flow goes to the
low pressure column through the JT expansion valve. 35.4% is used to boost the
turbine flow.

NITROGEN DISTILLATION COLUMN (Medium Pressure Column)

Only Gas enters the high pressure (4.1- 5.3barg) Nitrogen column and only liquid
leaves this column (as the Rich Liquid and Pure Nitrogen Liquid flow).
The air stream feeding the Nitrogen column enters the base of the column as
saturated vapor. This air feed flows up the column through the 30 trays until it is
condensed by the Condenser Re-boiler (HE-530) at the top of the column. As
the vapor raises towards the top of this column the distillation process increases
its Nitrogen concentration. The accumulating condensed liquid is then split
between a product (Nitrogen) stream and a reflux stream.
The product stream leaves the column and is sub cooled against the column
waste streams and turbine exhaust in the sub-cooler section at the bottom of the
Main Heat Exchanger. The reflux stream is fed to the top of the Oxygen column
and flows back down the trays by gravity, it mixes with the gas rising from the
bottom of this column and creates a foam of liquid and gaseous air which
facilitates a high surface area for gas/liquid contact, which increases the potential
for evaporation and condensation (the distillation process).

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There is a pressure drop between each successive tray as gas moves from the
base of the N2 column up towards the Condenser Re-boiler. The pressure at the
top tray of the N2 column is 5.01barg and at the bottom tray it is 5.34Barg. As
the pressure drops up the column so the temperature drops. Nitrogen has a
lower boiling point (Nitrogen = −196 °C, Oxygen = −183 °C) than oxygen (is more
volatile) and therefore, given equivalent pressure, will remain a gas at lower
temperatures than oxygen. The oxygen in the saturated vapor moving up the
column has a higher tendency to condense than the Nitrogen and so, as the gas
moves upwards into zones of lower pressure and temperature, it becomes
increasingly rich in Nitrogen. The Nitrogen gas that reaches the top of the
column has reached final purity. Oxygen that condenses out of the rising gas
joins the reflux and flows back down through the trays.
As the liquid reflux falls through the trays and mixes with the rising gas it
becomes richer in oxygen (as Nitrogen evaporates out of the foam on the trays).
At each tray pressure an equilibrium purity concentration is achieved, with a
different oxygen, argon and nitrogen purity profile in the liquid and vapor.
The oxygen rich liquid that reaches the bottom (sump) of the Nitrogen column is
called “Rich Liquid” or “Crude”. Its purity is normally 38% oxygen. The sump level
is controlled by the Level Control Valve LCV-520 that regulates the flow of rich
liquid to reflux the top column.
A portion of the condensed and sub-cooled liquid Nitrogen after the Main Heat
Exchanger is returned to the top tray of the Oxygen column to provide reflux to
the upper levels of the column. This Nitrogen creates a low concentration O2
reflux at the top of the column, this reflux “washes” the Oxygen vapor out the

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waste stream. This flow is controlled by HIC-550. The remaining liquid is sent to
the LIN product storage tank via the product valve V-556.
The purity at the top of the high pressure column is between 99.6% Nitrogen
(0.19% O2) and 5 ppm Oxygen, depending on the amount of reflux diverted
down the column. In Nitrogen mode 100% of the product comes from this
column via HIC-556.

C-531 OXYGEN COLUMN (Low Pressure Column)

The top column has 47 trays and three feed sources: the Pure Liquid up flow
(from the bottom column) at the top of the column at tray 1(valve HIC-550), the
JT valve at tray 10 (TIC-580) and the rich liquid at tray 20 (LCV-520).
Distillation in the top column follows the same principles as that of the bottom
column: as the liquid falls through the trays it releases Nitrogen vapor, leaving
the reflux liquid richer in the less volatile Oxygen. Liquid that reaches the sump
of this column is normally 99.6% Oxygen and can be drawn off as product.
The Reboiler Condenser heat exchanger is physically located in this sump of
Oxygen liquid at the bottom of the column. The sump liquid level is controlled by
continually draining a small portion of liquid Oxygen from the column using
LCV531. The sump is known as the “Oxygen Bath” and the liquid level must be
maintained so that Reboiler Condenser is fully submerged. This will prevent "dry
boiling" of the Oxygen liquid, which could trap hydrocarbons and cause an
ignition hazard. The amount of liquid drained from the sump needs to be
balanced so that the level is maintained.

THE REBOILER CONDENSER (HE 530)

The Reboiler Condenser is a plate fin heat exchanger that provides the thermal
connection between the two columns.
The refrigeration required to condense the Nitrogen gas in the Condenser is
provided by the liquid Oxygen that is boiling at a lower pressure and temperature
(0.55barg and -178.77C) on the other side of the heat exchanger. The nitrogen
gas is warmer (-176.4C) and at a higher pressure, which allows it to condense in
the passages when cooled by the lower temperature liquid Oxygen boiling on the
0.55 barg side of the heat-exchanger.
This boiled Oxygen vapor is the driving force for the Oxygen column. The vapor
rises up the column, becoming enriched with nitrogen as Oxygen is condensed
to join the reflux. Waste gas very rich in Nitrogen and low in Oxygen is vented
above tray 1. This waste gas flows through the Main Heat exchanger as a
refrigeration source before leaving the coldbox to be used as both a heating and
cooling medium for bed regeneration.

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In Oxygen mode the waste gas from tray 1 will have 1.1 % Oxygen purity
when the system is operated efficiently. If the Waste purity is too high in
Oxygen, this is a sign that the plant is being run inefficiently (there is not enough
refrigeration to the system or the air feed flow to the HP column is too high). If
the waste purity is low or falling it indicates that there is not enough air flow to the
system and the purities will be compromised. This waste gas leaves the column
and provides refrigeration to the sub cooler and the Main Heat exchanger HE-
501.The waste gas then flows to the warm end module (WEM) where it is used
as regeneration gas for the beds.

The Gaseous Oxygen (GO) vent is vented above the re-boiler bath at tray 47.
When running in Nitrogen mode the Oxygen bath purities would become high
enough to create an ignition risk. The GO vent removes Oxygen molecules from
the system to control the liquid Oxygen and gaseous Oxygen purity. This vent
also limits the amount of Oxygen molecules leaving in the waste stream. If the
waste contains too much Oxygen (a safety risk as waste gas is heated for
regeneration) then the GO vent can be opened to reduce the purity. Waste
purities of 21-30% are acceptable, as long as the liquid Oxygen bath purity does
not go above 99.8%.
Thus there is an operator split of air flow to Distillation through valve FCV-495
(HIC-495) which sets the purity of the cryogenic products. Production quantity is
maximized by the maximum air flow to the refrigeration system and the split to
TEV-580. Production purity is maximized by the air flow to the column system. It
is the operator’s duty to achieve an optimal balance between these two flows.
Too high an air flow to the columns will result in high purity product but low liquid
yield. Low air flow to the column and high flow to refrigeration will result in a high
liquid yield but with a low purity.

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