Asut 09 01 08 Pap

ASUT-09-01-08
About Pre-Purification Units
Purpose and Scope 2

Air Preparation and Purification 2
Contaminants in Air 2
Air Filters 3
Water Vapour in the Air 3
Vapour Content Dependency on Temperature 4
Vapour Content Dependency on Air Pressure 6
Condensate Separator 7
Dryers - mole sieves 8
Mole Sieves in Combination with Other Drying Media 11
Risks with Hydrocarbons 12
The Function of Mole Sieve Batteries 14
1.0 November 2007 Uncontrolled Copy - do not use after date of printing Page 1 of 16
ASUT-09-01-08
Purpose and Scope
Purpose This chapter describes the pre-purification unit, explains how it works and outlines how it is used in
the air separation process.
Scope All relevant Linde employees who are to be trained in ASU operating techniques.
Air Preparation and Purification
Contaminants in Air
Contaminants The air which is used is contaminated with:

• Dust
• Water vapour, the amount of which depends on the weather conditions
• Carbon dioxide, approx 0,04%
• Hydrocarbons, eg. acetylene, in ppm quantities and less
The contaminants are found in normal fresh air. There are also other contaminants, but in smaller
quantities, eg. sulphur dioxide and nitrogen dioxide, which occur from combustion.
In areas around industrial chemical plants or steel works, there can be other contaminants as well.
ASUT-09-01-08
Air Filters
Air filter An air filter removes dust particles. Normally they comprise two parts:
description
• a course filter for the large particles and
• a fine filter which takes out particles with a size down to a micrometer (=1 millionth of a meter
= 1 thousandth of a millimetre).
Dust removal Dust must be removed or else it accumulates and clogs the process equipment, therefore increasing
resistance and can lead to undesired stoppages.
This particularly applies to turbo compressors that are very sensitive to dust as they have parts which
rotate at very high speeds and have very small clearances with stationary parts.
The dust increases wear, and gas leaks through the clearances in the compressor reduce its operating
efficiency.
Course filter A course filter normally comprises a screen which is rolled on automatically. More dust in the filter
increases the pressure drop over the filter, by measuring the pressure drop new screen can be
automatically brought into use.
One must always check that the roll is not empty and that the screen is not damaged, which will
indicate that the pressure drop has increased or decreased respectively by too much.
Fine filter A fine filter comprises a textile mesh in a cassette. There is a pressure meter which measures the
pressure drop and when a pre-determined value is exceeded, for example 60mm wc 6 mbar, the
filter must be changed. This can be viewed as an insignificant drop but its importance is in the air
compressor energy consumption, (see Change of Capacity Due to Altered Suction Conditions (in
ASUT-05-01-09)).
Water Vapour in the Air
Water vapour Water vapour must be removed from the air as we have a cryogenic process which means that the
removal vapour freezes to ice, even if there is as little as 1 ppm vapour in the air.
Atmospheric air will always contain water vapour, the quantity being dependent on temperature,
weather and wind conditions. This is because that over water, even when it is cold, there is always
evaporation taking place with the water vapour rising into the atmosphere.
Air saturation At the same time condensation occurs in the form of very small drops that return to the water. If
there is dry air standing still over water, then in the beginning there will be more evaporation than
condensation. The vapour content increase and therefore condensation increases.
Finally, the maximum vapour content is reached, this is known as the air being saturated with water
vapour. Evaporation and condensation continue but in exactly equal proportions. Equilibrium has
been reached. This is one of natures many recycles.
ASUT-09-01-08
Vapour Content Dependency on Temperature
Vapour content The vapour content in air which is saturated depends on the temperature. The following table shows
and air how much vapour there is at different temperatures. The table also shows the vapour pressure,
temperature which shows how much pressure that vapour alone has.
Temperature Vapour Content Vapour Pressure

(°C) (g/m3) (mbar)
-10 2,3 2,9

0 4,8 6,1
5 6,8 8,7
10 9,4 12,3
20 17,3 23,4
30 30,3 42,4
40 51,0 123
100 598 1013
ASUT-09-01-08
We can see that at 100°C/ (212°F) the vapour pressure is 1,013 bar, which is identical to atmospheric
pressure. Therefore, when we boil water, the vapour content rises so much that it displaces the air.
Sub zero It is important to note that the vapour is not lost when the temperature is less than 0°C/ (32°F).
temperatures Vapour content reduces gradually with temperature. This explains why it is possible to dry laundry
outdoors in the winter time.
ASUT-09-01-08
Relative humidity When air is saturated with vapour, we say that it has 100% relative humidity. When it rains the
relative humidity is 100% and on a sunny day it can be 70%.
Despite this there can be more water vapour in the air on a sunny day than on a rainy day, if it is
warmer on the sunny day.
For example, if it is 20° and 70% there will be 0.7 • 17,1 = 11,9 g/m3 vapour, whereas at 10° C and
100 % there will be 9,3 g/m3 vapour.
If we cool down air at 20°C/ (68°F) and 70% relative humidity the possible vapour content is
reduced as we can see in the table. This implies that when the air becomes colder the relative
humidity increases. When this approaches 100% the air cannot hold off the vapour so condensation
begins. The dew point is reached.
In our example we had 11,9 g/m3 vapour, and this point is reached at approx. 14°C/ (57,2°F). This
means that air at 20°C/ (68°F) and 70% has the same dew point = 14°C/ (57,2°F), which can be read
off the tables that are more detailed than the one here.
If we continue to cool the air, more water will come out. At 10°C/ (50°F) the air will contain 9,3
g/m3 of water. We have cooled out 11,9-9,3 = 2,6 g/m3. If we had cooled air at 20°C/ (68°F) and
100% relative humidity to 10°C/ (50°F), then we would cool out 17,1-9,3 = 7,8 g/m3, while the
vapour content that remains in the air depends only on the final temperature.
Vapour Content Dependency on Air Pressure
The air pressure has almost no effect on the vapour quantity at saturation. In an air compressor, air
is compressed from atmospheric pressure to approx 5 bar g. If we convert the pressures to absolute
pressures: 1 and 6 bar abs we can calculate the volume ratio according to the ideal gas equation.
More details of this are given in Calculation of Gas Volume According to the Ideal Gas Equation
(in ASUT-05-01).
The final volume is 1/6 of the original volume. Therefore the final volume would contain six times
more water as the original volume, which means that a lot of water must condense out.
If we compress air at 20°C/ (68°F) and 70% relative humidity to 5 bar g and cool it to 20°C/ (68°F),
the water input vapour content is 11,9 g/m3.
However at the outlet the air can only contain 17,1 / 6 = 2,85 g/m3, therefore 11,9-2,85 = 9,05 g/m3
must condense out.
If we compress air at 20°C/ (68°F) and 100% relative humidity in the same way, then more vapour
goes in: 17,1 g/m3, but only the same amount of vapour can come out. Therefore more water must
be condensed out =17,1-2,85 = 14,25 g/m3.
ASUT-09-01-08
Condensate Separator
Condensate The air after the compressor is cooled with water and refrigeration machine to +5°C/ (41°F). Large
separator amounts of condensate are formed, which have to be separated.
description
A condensate separator is a container that has a much larger diameter than the pipe that it is
connected to. The larger diameters make the velocity of the air flow become lower, so that it is
possible that the water droplets are not blown away but fall to the bottom. The water is taken out via
a valve which is designed only to pass water.
To ensure that the very small droplets and mist are separated the container is filled with, many
metallic meshes which are fitted tightly together. The small droplets adhere to the meshes to form
larger droplets, which fall down and are separated. If water droplets enter the drier, then it will
become overloaded. Therefore it is important that the separator is in good working order. There is
an alarm and trip for high water level in the separator (LZAH).
Water Separator
ASUT-09-01-08
Dryers - mole sieves
Mole sieve Drying is nowadays carried out using mole sieves. These are manufactured from a man made
description mineral of aluminium silicate called zeolite. This comprises crystals which tie in a lot of water to
their molecular structure. When the zeolite is warmed-up, the water is evaporated, while the silicate
molecules remain tightly together and pore holes are formed which are all of equal size. The zeolite
is now ready for air drying. The water molecules bind very powerfully to the surface of the pores.
This is called adsorption.
Because of its special molecular structure with pores the mole sieve will pick up other contaminants
such as carbon dioxide, acetylene and most hydrocarbons. Mole sieves manufactured from zeolite
crystals are bound onto a ceramic material to become beads of around 5mm diameter. These are put
into a cylindrical vessel as a bed on a plate with small holes.
ASUT-09-01-08
Regeneration There are both standing and lying vessels. Air is fed into the bottom of the vessel, passes over the
mole sieve and goes out from the top. Heated impure nitrogen is fed in the opposite direction to
remove the water, which is called regeneration. Therefore two vessels are required, one for drying,
and the other for regeneration.
Mole Sieve Adsorber
Cooling air To avoid having large, expensive vessels and large electrical heaters for regeneration, the vapour
before drying quantity in the air is reduced before it goes into the mole sieve. This is done by cooling the air to
+5°C/ (41°F) with a refrigeration machine. This temperature is selected in order that there is no risk
of freezing the vapour to ice in the cooler. If the refrigeration is degraded and the temperature is
increased, then the vapour quantity and the load of the mole sieves are increased.
ASUT-09-01-08
Carbon dioxide If overloading occurs in the mole sieve, then carbon dioxide breaks through into the process. It then
break through freezes out to soft snow in the cold end of the main heat exchanger. This appears as an increased
temperature difference, which cannot be reduced by changing the gas streams, and as increased
pressure drop. Carbon dioxide will continue to be partly blown into the column and because it has a
higher boiling point it is washed down in the rich liquid. Then it will be fed to the LP column and
washed down to the LOX-reboiler and then form a layer on the reboiler surface. This degrades the
heat transfer which raises the pressure of the nitrogen part on the condenser side (see How a
Reboiler - Condenser Functions (in ASUT-12-01-06)).
Note: A break through of CO2 shall be avoided according to new rules, see Risks with
Hydrocarbons (Page 12).
ASUT-09-01-08
Mole Sieves in Combination with Other Drying Media
Drying media to Mole sieves are very sensitive to water droplets. When the water binds, energy is released and when
absorb water the water droplets come, the temperature rise is so large that there is a risk that the mole sieve beads
can split.
So in the bottom part of some mole sieves, where the air enters, there is a layer of alumina gel, which
is a common drying media, manufactured from aluminium oxide, see diagram below.
Mole Sieve Adsorber
The quantity of alumina gel used is designed for the amount of water and the quantity of mole sieve
to the amount of carbon dioxide and hydrocarbons.
An advantage with alumina gel is that it requires less energy to remove the water from it.
ASUT-09-01-08
Risks with Hydrocarbons
ASU incidents In 1997 powerful explosions occurred in two ASUs. As a consequence of this, the gas industry has
strengthened the rules of operation. The rules for Linde are available on Lotus Notes, SEQ service
(Safety, Environment, Quality).
The explosions were among others, caused by a big release of ethene in the neighbourhood in one
case, and by smoke from forest fires for months in the other case.
Adsorption levels Most of the hydrocarbons are completely adsorbed in the mole sieves, but ethene and propane partly,
and boiling and methane and ethane not at all. Their boiling points are higher than that of oxygen (see Air
points Gases Boiling Points (in ASUT-01-01)), so they will be washed down to the LOX reboiler and go
out to tank. Ethane, ethene and propane have much higher boiling points, so they will as a matter of
fact go down completely in the LOX. Methane, which has its boiling point closest to LOX, will to a
big part go down into the LOX, but a part goes out with the GOX.
As oxygen is 21% in air, the concentration of ethane, ethene and propane in LOX will be
approximately 5 times (1/0,21) that of their concentration in air, if all O2 is taken out as LOX. Their
presence in the atmosphere varies, but for methane it can be 1-2 ppm and for the others, less than 0,1
ppm each. The solubility of these hydrocarbons in LOX is several hundred ppm, which is much less
than the explosion limit, so it is normally a small risk. But a reduced production of LOX means an
increased concentration, so new rules of minimum allowed production must be followed.
Dry boiling Dry boiling of LOX is very dangerous, as in this case the hydrocarbons are enriched to a high
concentration. This can occur if you are operating with too low a level in the reboiler and a part is
coming up of the LOX bath. Splashes of LOX are then boiled off and the hydrocarbons remain.
Detailed instructions of the dimension of the reboiler in relation to the sample points of the level
indicator are necessary from the manufacturer.
Dry boiling can also occur in a passage in the reboiler block, if it is partly clogged by CO2. A well
operating CO2 analyser is necessary in all plants. The alarm limit shall be 1 ppm CO2 in the end of
an adsorption cycle. Continuous break through of CO2 below 1 ppm but above the detection limit of
the analyser is serious, as this could be an indication of damage or a leak inside the mole sieve.
Break through of CO2 also has the consequence that the partly adsorbed ethene and propane are
pushed out into the coldbox. A big break through, but not 1 ppm, even acetylene can be pushed out.
Acetylene is present in the atmosphere with approximately 0,1 ppm and is especially dangerous as it
is not soluble in LOX above 5 ppm. Above that are formed crystals (“ice”) which are very
explosive.
ASUT-09-01-08
Breakthrough Sequence of Impurities in a Mole Sieve
Special rules for Nitrous oxide (N2O or laughing gas) has appeared to be a risk factor in plants with an uncommon
Falling Film type of LOX reboiler, the falling film type.
Reboilers
Approximately 0,35 ppm of it is present in the atmosphere and it passes to a great extent through the
mole sieves. If there is a big GOX production, then it may crystallize in the falling film reboiler and
cause dry boiling in a spot.
For plants in risk areas, such as in the neighbourhood of oil refineries and petrochemical complexes
and having falling film reboilers, there are special rules.
ASUT-09-01-08
The Function of Mole Sieve Batteries
The pipe work and valves have been arranged so that the following steps will be carried out in each
mole sieve:
Adsorption Out of air at 5 bar from the refrigeration machine at +5°C/ 41°F
Parallel operation Of both vessels at 5 bar
Pressure reduction Of the vessel which was adsorbing
Heating With impure nitrogen at 0,2 bar
Cooling With impure nitrogen at +5°C/ 41°F
Pressure build up With air at 5 bar
Flow Schematic of a Mole Sieve Battery
Cycle time In a mole sieve the entire cycle takes 2-12 hours and the switch over of the vessels (adsorption -
regeneration) is automatic. The cycle times can be varied within certain limits, as this can be
necessary if the pre-cooling degrades. This increases the water quantity in air and mole sieve bed, so
the cycle time must be decreased. If this is not sufficient, then the air flow must be reduced or else
carbon dioxide is pushed out to the cold box. The difficulty is that shorter drying time gives shorter
time for regeneration of the other vessel. If the refrigeration machine completely fails and there is no
reserve machine, then the whole plant must be stopped.
ASUT-09-01-08
Pressure Mole sieves can be damaged by too rapid pressure drops or rises. They rub against each other and
reduction to powder is formed. Their distribution can be irregular and the bead level uneven, which will increase
avoid damage the risk of carbon dioxide break through.
Therefore a pressure reduction is carried out in steps: First through a small pipe with a small valve
and then through a large pipe with a large valve.
In newer plants there is a Pressure Differential Switch (PDISH), which does not allow the large
valves to open if pressure differential is over a certain limit. In a few plants there is a mechanism for
making the bed level even during operation.
Controlling The impure nitrogen used for regeneration is warmed in an electric or steam heater to approx 200°C/
nitrogen flow for 392°F. The temperature is controlled by a control (TISH), which shuts off the heater if the
regeneration temperature is too high.
The flow of impure nitrogen must be set according to the manufacturer's instructions otherwise the
regeneration may not be sufficient even if the temperature is correct. Normally, there is a flow meter
with an alarm (FISL), because if there is too little flow the electric heater can be damaged through
the risk of over heating.
Heating to Heating continues until the temperature at the outlet is at a level, that it can be ensured that all water
remove water is removed with the regeneration gas.
If this temperature is plotted on a printer (see diagram below), you can see when this happens as
there will be a "notch" in the curve. Please note that there is always some rest water remaining in the
mole sieve and it could slowly increase. If a capacity reduction has occurred and CO2 is breaking
through, it may help to increase the flow of the regeneration gas or to regenerate at maximum
possible temperature for a couple of hours during a plant stop.
Mole Sieve Regeneration Gas Curve (Cryoss, Hungary)
ASUT-09-01-08
In mole sieves where there is no alumina-gel in the bottom and where part of the mole sieve has
pulverised, the powder can be baked together in clumps with the help of water. These clumps allow
less gas to pass through, so that regeneration takes a longer time. This can be seen on the
temperature plot by the curve being more "drawn out". The pressure differential in the mole sieve
can be measured which will increase when there is dust in it.
Third vessel type In certain plants there is a 3rd vessel with a stone bed acting as a heat accumulator. The heater is on
continuously and hot regeneration gas is passed through the stone bed. During the regeneration
cycle, part of the cold regeneration gas can be heated in the bed.
By the heat accumulation the heater kW capacity can be reduced. This can be important depending
on the electricity tariffs, because the discontinuous heater creates a higher peak power to the whole
plant.

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ASUT-09-01-08

About Pre-Purification Units

About Pre-Purification Units

Purpose and Scope 2

Purpose and Scope

Air Preparation and Purification

Contaminants The air which is used is contaminated with:

Water Vapour in the Air

Vapour Content Dependency on Temperature

Temperature Vapour Content Vapour Pressure

-10 2,3 2,9

Vapour Content Dependency on Air Pressure

Dryers - mole sieves

Mole Sieve Adsorber

Mole Sieves in Combination with Other Drying Media

Mole Sieve Adsorber

Risks with Hydrocarbons

Breakthrough Sequence of Impurities in a Mole Sieve

The Function of Mole Sieve Batteries

Flow Schematic of a Mole Sieve Battery

Mole Sieve Regeneration Gas Curve (Cryoss, Hungary)

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