UOP AIR PRE-PURIFICATION UNIT (APPU) ADSORBENTS (MOLECULAR SIEVES AND

ACTIVATED ALUMINA) RELOADING AND START-UP GUIDELINES

December 2020

BY HUGO LI
ADSORBENT STS MANAGER IN SHANGHAI UOP OF HONEYWELL

Content：

BRIEF OF MOLECULAR SIEVE ACTIVATED ALUMINA IN AIR PRE-PURIFICATION UNIT

ONSITE HSE AND KEY POINT DURING MOLECULAR SIEVE RLOADING
EQUIPMENT, TOOLS AND STUFFING
MAJOR ONSITE RELOADING PROCEDURE
HIGHLIGHTED DETAILS OF KEY STEP

APPENDIX：

LIST OF SCREEN MESH AND SIZE

BOTTOM GRID TYPES
APPU STARTUP GUIDE IN GENERAL

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1 BRIEF OF APPU

Feed gas：Air
Regeneration Gas：Waste N2 in normal running, dried air in activation
Target impurities：H2O, CO2
Other harmful but not specified impurities：CO, N2O, C2H2
Temperature: normal range 7-18 Deg. C
Pressure: 500-800 Kpa, A

2 ONSITE HSE AND MOLECULAR SIEVE RELATED REMINDING

HSE

1. In-vessel suffocation：Molecular sieve, especially fresh goods, can quickly adsorb oxygen
from air, causing oxygen – insufficiency inside the vessels. So onsite operational workers
need to pay attention to the high risk of suffocation. The O2-analyzer and pump-type Long
tube air breathing apparatus are all required for anyone working inside the vessel.

2. Fine powder hazard ： Inflammation of the eye, long-term inhalation can cause
pneumoconiosis. Pay attention to that and always wear a breathing mask at the scene, at
least wear a dust mask.

3. Falling risk of high-altitude operation: The operating point is basically more than 5 meters from
the ground, even reaching 10 meters or higher. If workers onsite need to climb, it is necessary
to be careful to wear a safety rope always to prevent the risk of falling. When climbing the
ladder, don't follow, make sure to have one person climb and then next one. Work is prohibited
on strong windy days. Anyone working on top of the vessel should always safety belt. When
entering vertical vessel from the top, anti-sink equipment/system is required.

4. Risk of slipping: Molecular sieves or alumina pellets/beads scattered on the ground should
be supervised and promptly cleaned, to avoid slipping.

5. Other external force injuries: Cuts, scratches, crushes by tanks, tool falls and knocks head,
lifting rings broken when lifting big bags, etc. Always wear safety helmets, safety shoes, and
cut-proof gloves on site. It is strictly forbidden to stand under the crane and any irrelevant
person should stay outside the safety yellow line.

About Molecular Sieves and Activated Alumina：

1. It is strictly required to keep the molecular sieve or alumina away from liquid water. It is
strictly forbidden to bring the water bottle/water cup into the tank.

2. It is strictly forbidden to open the barrel in advance of loading molecular sieve or alumina
and forbidden to expose it to the air for a long time.

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 3. Forbidden to load in rainy days

4. It is strictly forbidden to prevent the molecular sieve from being broken by the
mechanical/external force. Generally, it is forbidden to use the pump to fill. When loading
the molecular sieve, the vertical drop height should not exceed 3-5 meters. Otherwise, a
canvas speed reducer should be used.

5. Molecular sieve or alumina is strictly prohibited from contacting any organic compounds,
including oils and various solvents.

6. Molecular sieves are strictly prohibited from contacting any unknown chemical products
and avoiding any possible contamination. For example, when the molecular sieve is
poured from drums into a big bag, the big bag must be a clean and new. Do not use any
used large bags in order to prevent the introduction of other impurities. For example: It is
strictly forbidden to use urea bags, resin powder sacks, etc.

7. It is forbidden to forget any tools and objects in the tank.

3 EQUIPMENT, TOOLS AND STAFFING

Large equipment: crane, unloading vacuum pump, forklift, scaffold

Tools and materials: new big-bags, steel-wire screen, hopper, canvas speed reducing bag with
enough length, sling, cross-hanging shelf, ventilation, rope ladder or lifting pulley,

Preparation of other gadgets: plastic/wooden rabbles for flattening the surface (lightweight wood
planks are also available), a number of planks on which people stand (preventing the footstep on
the surface from collapsing, avoid pits appearing or causing unevenness). Flashlight, interphone,
rope ladder, safety belt, tape ruler for measurement, plastic shovel, stone pen, asbestos rope, tin,
iron wire, fine steel wire

Basic PPE: face mask respirator, long tube pump oxygen breathing apparatus, dust mask, dust
glasses, safety shoes and gloves, flame retardant clothing, safety rope,

Staffing: 1-2 forklift truck driver, 1 crane driver, ground cranes coordinators 1-2 people, dumping
MS from drums to big-sack needs 3-4, 2-3 people on the vessel top, 2-3 people inside vessel, 1
ground supervisor, another 1 person as supervisor on the top, 1 person in charge of gas analysis.
Total: 13-18 people.

4 MAJOR ONSITE RELOADING PROCEDURE

1. Discharge
- There are not special requirements for the unloading process. It is recommended to use a
vacuum pump to remove the used adsorbent, that is more efficient.
- If discharging manually, mechanical damage to the any inner parts of the vessels, including
distributors, grid, screen etc., should be avoided.

2. Check
- Check and confirm the number of drums or bags of molecular sieves and alumina

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- Check and verify that the molecular sieve and alumina packaging are in good condition,
whether the product is correct, whether the warehouse storage conditions are ideal, if not ideal
(such as leakage of rain, water seen on ground, leakage of broken bag, barrel deformation),
then take photos in time for evidence.
- Remove the bottom valve or a flange to facilitate access to the bottom of the tank. If the
conditions are not available, it is necessary to weld-cut a 400-500mm diameter manhole on the
pipe.
- After determining the oxygen content, works enter the pipeline. Check the inlet and outlet
valves, check the internal corrosion of the pipeline, check the inner wall of the pipeline for salt
condensation, water, ice, molecular sieve particles / powder accumulation, etc.
- Inspection on internal pieces of vessel
- Measure to confirm the pore opening width and type of the bottom grid (Johnson type,
punched-board type, large-pore-opening type grid)
- Check the bottom part the vessel for damage and corrosion
- Check the bottom grid from the bottom of the vessel for damage and corrosion.
- Check the connection between the grid boards, at the joint between the grid and the wall,
whether there is de-soldering, corrosion, excessive gap, etc.
- Check the upper and lower airflow distributor filters for damage
- If any internal parts are damaged, repair it. Repair welding, asbestos rope filling may be
required, and if the damage is serious, it should be replaced.

3. Loading
- Generally, lift the goods in drums or bags by crane, by using sling or cross hanger. It is strictly
forbidden to directly hook the big bag’s hanger (hanging rings) to the crane hook, otherwise the
big bag will easily be teared and broken.
- The scaffolding should be set up before loading, and the loading hopper/funnel or pipe or
another groove should be well fixed. If you need to pour the drums to a large bag on the ground,
you need to set up a platform to facilitate the step. A water-proof shed is required to be installed
at filling hole of the vessel or at least prepared in case of storm.
- Confirm that all stuffs in place
- Wire screen, and other tools are ready
- For regular vertical and horizontal beds:
- load large ceramic balls (not necessarily)
- flatten then install screen (not necessarily)
- load large alumina ball (not necessarily)
- flatten then install screen (not necessarily)
- load small alumina balls
- flatten then install screen
- load Molecular sieve and flatten

Pay attention: if
4. Cleaning
- Unloading and charging will generate a large amount of molecular sieve particles passing
through the barrier and leak to the bottom of the tank, which needs to be cleaned manually.
- Personnel can enter from the bottom into the pipeline, manhole or tank bottom, and the inlet/
outlet valve sealing surfaces can be cleaned
- Check and unblock inlet and outlet drain valves of absorber for both feed air and regeneration
N2.
- check and confirm not blockage of the bottom thermal-couples.

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5. Recovery / Sealing
- The owner's personnel can seal the can and ventilate if necessary.

5 HIGHLIGHTED DETAILS OF KEY STEP

For horizontal bed, the manhole (also used as filling inlet during loading) is on the side instead
of the top of the vessel.

1. To discharge: most convenient way is to use vacuum pump (if the old adsorbent will not be
recycled). Unloading manually is less convenient but also possible and usually seen as
below fig. The hand-made white-iron (same material as used in external insulation of the
pipeline) groove, should be fixed with proper tilt angle degree, onto which workers can
manually dump the used adsorbents and let it flow outside of the tank, finally into the big
bags.

2. Check and confirm the bottom grid.

The grid is the support of the entire bed. The most basic requirements are three points: the
strength is enough and cannot be collapsed; the size of the pore is small enough to prevent the
particles from leaking; no blockage and no influence on the airflow distribution. Therefore, the
inspection of the bottom grille before loading is critical. Different types of barriers have different
requirements due to the splicing method, workmanship, and gap size.
For Johnson grille or perforated plate, simply confirm the size of the grille or orifice slit to ensure
that it does not leak.

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For any wide-opening grid, it is necessary to confirm whether it is necessary to add a screen to
increase the strength and prevent the leakage of the bed during operation. For some roughly-
wade grid, even two-three layers of mesh (3-5 mesh, 8-10 mesh and 12-20 mesh) are required.
The protruding part of the ribs should be even covered with a 3-5 or 8-12 mesh screen to reduce
the compressive stress on the bottom particles.

3. After grid and inside check, but before starting loading the alumina, it is suggested to mark
the design height of each layers on the inner of the vessel, just to help to check the flatness,
equal thickness of entire layer and to double confirm the loading amount of each layer of
product. Below fig shows the both good (top fig) and wrong (the two figs on bottom) examples
after loading alumina goods.

4. If product is packaged in big bag, simply hanging and dumping to directly load. If product is
packaged in steel less drums, user need to dump product into big filling hopper or solid and
clean big bags then hang them to the manhole to load in vessel. Don’t open the drums once
for too much, to avoid long time exposure to the moisture in air.

5. For vertical bed, the slow-down bag should be used, instead of dumping directly without any
control to avoid physical breakup of product particles. For horizontal bed, user can simply
refit the groove used for unloading, to a proper opposite tilt direction to let in the fresh
goods. Some users also can make a pipeline while connected on the filling hopper (fixed on
the top, not the one for transferring the good from drums) on one side, while another side is
extended into the vessel through the manhole.

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6. Screen of proper mesh should be installed after loading and flattening of alumina goods, just
to sperate it from molecular sieve, and to avoid mixture of bed. There are quite a lot of detailed
requirement and experience during preparation and installation of such separation screen.

7. In certain reloading case, the alumina layer thickness is possibly changed just due to different
designed weight or different density. In this case, the original fixed separation grid/screen (if
there was) should not be allowed to installed back, otherwise the gas can go through certain
uncovered area and causing the channel flow risk which in turn will cause startup failure.

8. The preparation of separation screen in detail:

Fig. cutting in proper length.

If the purchased screen is delivered in roll, then user should cut to the proper length.
For horizontal bed’s screen installation in transverse direction or normal vertical bed’s screen
installation: the cut length should be equal to diameter of the vessel + 300mm.
For horizontal bed’s screen installation in axial /lengthways direction: the cut length should be
equal to the entire length of the vessel (including the 2 heads) + 300mm.

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Fig. Overlap and connected different pieces to form the entire one. （overlapped width should
be 300mm, fixation is required every 200-300mm distance.）

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Fig. Any screen, no matter is bottom screen or separation screen between alumina and
molecular sieve layers, should be paved with side upward curve about 150mm height, to avoid
the side-bed-sink effect in long term.

Fig. Two kinds of screen installation way for horizontal bed: in lengthways (right hand) or in
transverse (left hand). Works should put inside some long wood board and step always on it to
avoid unflattening of the bed or breaking the screen.
Pay attention: for normal vertical vessel, the connected screen should be cut to a round shape
with diameter equal to vessel’s diameter plus 300mm, in order to keep 150mm edge-upward-
curve height.

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Fig Cut the screen at any hopper-liked shape’s position, especially at two heads of the
horizontal vessel.

9. To load alumina or molecular sieve on the installed screen, always remember to pave the
edge firstly, so that the weight of the goods can press the screen edge to well adhere to the
inner surface of the vessel. Then all the wood boards should be moved out of the vessel and
accounted to assure no omitting. After all user can continue to load.

10. In some Linde’s horizontal equipment, on the very top surface of the molecular sieve, user
can load a little bit more molecular sieve than in the middle, just as a weigh buffer to
compensate the possible edge-sink effect in future, while keep at least 100-200mm height
beneath to the top gas distributor.

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Page 11 of 17
 6 Appendix
Screen mesh and size:

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 3 types of grid

Johnson grid - equivalent：

Hole-board ：

-y

Wide-open board：

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UOP GUIDELINES FOR APPU START-UP AND ACTIVATION

Before startup/re-startup, user should check carefully all below items in cooperation with original
EPC, to make sure that:
1. The mist catcher of the air-cooling tower is not blocked or damaged, otherwise it needs to be
replaced or cleaned in time
2. The circulating water pressure has been relieved
3. The pressure holding test confirms that the system has no leakage
4. The valves at each position can switch normally
5. The drain valve on the molecular sieve inlet pipe (of feeding air) should be opened and
unblocked. If it is an automatic valve, ensure that it operates normally.
6. The condensate water drain valve of the regeneration gas outlet is open and unblocked.
7. The automatic drain valve on the bottom of the molecular sieve tank (if there is) can open
normally.
8. The steam heat exchanger has no corrosion or any leakage, and the outlet heated gas dew
point can reach the standard (<-75C)
9. All heating tubes of the electric heater are normal and can assure heating to the target
temperature.
10. The valves on the air pipeline after the molecular sieve unit, to the downstream expander and
cold box, should be closed or blinded.
11. Other sensors and meters are tested normally.

Below are usually recommended by UOP for startup step:

1. Activating medium gas: the molecular sieve bed can be activated by continuous purging
heated wasted nitrogen, or it can be activated with heated dried air. However, if there is not
those pipeline gas source, end-user can also choose to take the self-circulation mode for
activation step.

2. Activation temperature: It is recommended that the heating temperature be around 200-220C,

and the temperature at the entrance of the molecular sieve should be controlled at 180-200
degrees, and the peak temperature of the outlet of absorber is preferably at 140-160 degrees.
When the fresh product is just installed for the first time, it generally does not need to be
heated to above 250C for activation, unless there is significant moisture absorption during
storage or loading.

3. Activation cycle time (time for heating-then-cooling one bed): This time should match the air
flow rate. If the feed air flow rate is 20-25% of the designed full charging(20-25% of full charge
is the usually recommended flowrate of air during the activation step), the cycle time is
controlled within 5-6 hours (that is to assure the bed utilization ratio is controlled less than
30%, to avoid moisture breakthrough and assure the dewpoint of the dried air ), heating time
is about 2-3 hours, cooling time is about 3 hours, the rest time can be distributed into de-
pressure (about 15 minutes) and re-pressure (20-25 minutes). For example, when tank A is
running in adsorption, then the dried air after tank A goes through the heater and will be heated
to target temperature 200°C for instance. Then the heated dried air is passed into the second
tank B as the regeneration gas. After at least 4 cycles (that means, each tank will be activated
at least 2 times. It is better to be 3-4 times for each tank, if time allows), user can go to the
next step. After confirming that the outlet carbon dioxide and moisture concentration meet the

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 standards (normally CO2< 0.5ppmv, Dewpoint <-70C), user can pass the purified air to
downstream expander and the cold box.

4. Start introducing more air to the system, and gradually adjust the air flow rate to 50%-75% of
designed full charge, meantime the adsorption time(per bed) should be shortened to about 4-
5 hours/bed (i.e. one full cycle time of 8-10 hours for 2 beds), and the heating time is 90-110
minutes, Cooling time is set to about 140-170 minutes. If there is no liquid in the cold box
(namely cold box had once been heated to remove hydrocarbon), user can use the purified
air to purge the cold box (driving out CO2&H2O). Both CO2 and moisture should be analyzed
in the cold box. When bottom cold-box temperature decreased to target temperature, the liquid
air will be gradually formed. Once the level of liquid air in the cold box reaches to the designed
value, the cold box can be started. About 2-4 cycles after purging cold box, the returned gas
is heated by the heater and used as regeneration gas. At this time the cold box begins to cool
down. Regenerative gas flow rate now can be controlled to about1/5 to 1/4 of the full
charge/feeding air flowrate. System now is very close to normal running.

5. When the temperature of the cold box drops below -180 degrees, the feeding air flowrate
should be close to 90%. User should make sure now that the adsorption time per bed should
be about 4-4.5 hours, not higher than that. Then user continue to wait for 2 cycles and observe
the peak temperature of N2 at outlet of each bed in each cycle. Since the APPU is running
with the thermal pulse regeneration mode, the peak temperature during N2-Cooling-purge is
an evidence showing whether the bed is regenerated enough or not and should be controlled
above 120-130 degrees or as much as possible. In addition, the cooling N2 temperature at
outlet of absorber should be controlled as lower as possible. At such beginning stage startup,
it is highly recommended that all the regeneration condition is controlled to the very
advantageous level, including the N2 flowrate, the heater outlet temperature, as well as the
heating and cooling times need to be refined to achieve the best regeneration effect in each
cycle, assuring the lowest residue impurity level in the bed. After the system becomes stable,
user can enter next step.

6. Meanwhile, the cold box should normally work in standard mode, the regeneration gas
becomes pure nitrogen. Enter the next step after confirming the entire system is stable.
7. Judging from the real entrance impurity concentration, the adsorption time readjusted within
4 to 4.5 hours, and then wait for the system to stabilize. According to the peak temperature
value and the cooling effect, user can determine how to refine the heating and cooling time
distribution.

Note:

1. Each set of air separation system can be different from another. As an experienced user
or for EPC contracting project, the user can develop a more reasonable activation-start-
up-commissioning process or follow the EPC guidance. The above operational suggestion
may not be adopted completely to certain equipment. And some specific conditions need
to be adjusted according to real onsite working conditions. During the debugging process,
pay attention to the following parameters:

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 Usually the following key parameters are checked:

Parameter Recommended value

Adsorption temperature < 10-16°C
Reg. heating temperature > 180°C
Reg. cooling temperature < 20-25°C
Peak temperature during 140-160°C （ during activation and
cooling purge
startup）
> 120°C（during normal running）

2. During the activation process, the specific operating parameters, temperature program
and other settings can be adjusted appropriately in consideration of the special
requirements of the original equipment provider.

3. Since UOP molecular sieve is a highly porous material with good diffusibility, it does not
need to be heated to a very high temperature even during activation. Instead UOP
recommends no more than 220 degrees. If user need to ensure a lower moisture residue
rate, user can extend the heating time to achieve the same effect (the premise is that the
regeneration medium gas itself must be dry and the dew point must be low enough <-70-
75C).

Assuming that the filling process is quite different for A/B tanks (there is a difference in exposure
or pre-absorption): B is loaded first, and the humidity may be higher after rain, while A bed is
loaded faster, so the amount of water and carbon dioxide of the air pre-adsorbed in the bed A
should be relatively smaller than B. So, the adsorption starts from A. The following table is an
estimated schedule only for reference only.

time/ A/B bed Feeding air Ads temperature/reg. note

hours status or reg. gas heating or cooling
flowrate % temperature / C
of designed
full charge
A B A B A B
0-6 Ads. Act. 20- 20- <11 >180/<22 Time set in mins:
25% 25% 10+150+180+20(depress+heat+cool+repress)
，air inlet of bed A about 25% of designed full
charge，ads. time per bed: 6h, dried air 100%
recycled through heater then to bed B
6-12 Act. Ads. 20- 20- >180/<22 <11
25% 25%
12- Ads. Act. 20- 20- <11 >180/<22 1.5 cycles to observe, if peak shape is normal
18 25% 25% then can increase air flowrate in advance。
18- Act. Ads. 20- 75% >180/<22 <11 Time set in mins: 10+95+145+20 ， air feed
22.5 25%
flowrate 75% of designed full charge ， ads.

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 time: 4.5h, if CO2 and moisture tested to OK,
then purified air can be let into downstream cold
box to purge from next cycle.
22.5- Ads. Act. 75% 20- <11 >180/<22 Normal running now, reg. gas is waste N2.
27 25%
27- Act. Ads. 100% 20- >180/25 <11 Continue increasing feeding air flowrate,
51.5 25% keeping another parameter the same.
51.5 Observation, stabilization, make sure no
之后 continue decrease of peak temperature.

Pay attention to the following suggestions in your normal running:

1. Adsorption air temperature: The recommended value is controlled below 12°C, and the
ideal value is below 10°C. Higher temperature means that more saturated water will enter
the adsorbent bed, which will increase the heat load of regeneration, and will also inhibit
the adsorption performance of CO2 (due to competitive adsorption).
2. Regeneration heating temperature (heater setting temperature): It is recommended to
control at 200°C, but it does not need to be higher than 220°C. If the regeneration heating
temperature is low, the heating time can be appropriately extended during commissioning.
3. If the original equipment manufacturer has requirements for the temperature gap between
the inlet and outlet of the equipment, the temperature can be increased manually in two
steps. The first step is to set to 140 degrees, and when the outlet temperature reaches 40
degrees, set it again to 180-200 degrees. The total heating time can be basically
unchanged.
4. The lowest temperature at the end of regenerative cooling: the lower the better, and it is
recommended to control it below 20 degrees.
5. All the operational time set value should adjusted to meet the above key parameters as
the premise.
6. Peak value of regeneration N2 during cooling purge step: the best range is 140-160C. If
energy-saving operation is considered, it can be appropriately reduced to the range of
120-140C. However, this operation generally corresponds to the adsorption time.
Therefore, it is recommended to consult UOP technicians before adjusting.
7. Any adjustment of operational time set, or adjustment of regeneration heating temperature
should be adjusted gradually in several steps, and sufficient observation time should be
taken always between each adjustment/change.
8. Pay attention to the drain valves on the air inlet/outlet pipes of the equipment and make
sure to normally open it to exhaust liquid water. In winter, pay attention to possible freezing
and blockage of those valves.
9. In order to deal with water flush accidents, ensure that the T-shaped connection at the
bottom of the adsorption air intake pipeline is unblocked (if it is an automatic valve, ensure
that it operates normally), and there is no unloading small particles residue caused
blockage.
10. Run from 2-3 weeks to 1 month and observe whether there is bed sink. If there is,
appropriate supplementation can be carried out at the appropriate time to ensure that the
height.
11. For any other operations, please communicate with UOP technicians in advance. It is
necessary to strengthen the monitoring of DCS in daily operation, and regularly pull out
the trend line to determine whether it is operating in a steady state.

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