SYLOBEAD® Adsorbents Handling

Brochure
Precautions and Safe Practices in Working
with Process Adsorbents

1. Basic Understanding of Adsorbents and Their

Operation..............................................................................Page 1

2. Loading of Adsorbents...................................................... Page 1

3. Start-Up and Commissioning............................................ Page 6

4. Unloading Activities and Handling Spent Adsorbent......Page 7

5. Storage of Adsorbents...................................................... Page 9

The information contained herein is based on our testing and experience and is offered
for the user’s consideration, investigation and verification. GRACE DISCLAIMS ALL
WARRANTIES EXPRESSED OR IMPLIED, regarding the advice and instructions provided
herein and all results obtained from the use of our products, since customer operating and
use conditions vary and are beyond Grace’s control.

W. R. Grace & Co. is a global supplier of adsorbent materials

for dynamic processes under the trade name SYLOBEAD®.
The adsorbent products vary from Activated Alumina to
Molecular Sieves and Silica Gel type products. This brochure
aims to give guidance to our customers in handling, installing,
operating and unloading our adsorbent materials in their
process units.

Grace intends to give general recommendations in this

document that will help our customers and their engineering
partners take decisions during engineering phase. The
ultimate responsibility and liability for a good engineered
unit lies with the end-user and engineering partner.
W. R. GRACE & CO. ­— SYLOBEAD® Adsorbents Handling Brochure
1) Basic Understanding
of Adsorbents and Their
Operation
Adsorbents remove contaminants from
process streams by physical interactions
at the molecular level between the
contaminant itself and the adsorbent
surface. Adsorbents therefore are
materials with a high internal surface area.
To access the surface area, pores play a
critical role and thus adsorbents are as well
highly porous materials.
Thermodynamically, adsorption is
an exothermic process. The heat
of adsorption is released during the
adsorption steps. The heat of adsorption
can be relatively high, like for water
adsorption on zeolites, or hardly noticeable
like CO2 adsorption on activated alumina.
The heat of adsorption can be seen as a
parameter for selectivity of contaminants
on a specific adsorbent: the higher the
heat of adsorption, the more selective the
component is attracted by the surface.
Once the adsorbent material has been
completely saturated with the contaminant,
i.e. its total capacity is occupied, it can be
regenerated to recover its initial capacity.
Regeneration can be done by reducing
the pressure – so-called pressure swing
adsorption units (PSA) – or by heating the
material up – so-called thermal swing units
(TSA) – or by displacement steps. The
most common practices are TSA and PSA.
For more detailed descriptions on
adsorbent materials and their specific
characteristics, and the specifics of
adsorption processes, refer to the Grace
SYLOBEAD® adsorbents brochure.
2) Loading of Adsorbents
This chapter describes the steps related
to the loading of the adsorbents in
chronological order. Please read through
carefully and make sure all steps have
been completed before proceeding to the
next steps.
Page 1
2.1) Preparation
Prior to the loading operations, a set of
preparational steps are needed to make
sure the following steps in the loading
operations will be executed in a safe and
efficient way.
2.1.1) Safety considerations
Grace’s SYLOBEAD® adsorbents are
supplied as beaded or granulated
materials. In their freshly delivered
state, they impose little risk to operators
provided the correct PPE is used. The
personnel involved in adsorbent handling
procedures should be equipped, as
a minimum, with the following PPE:
helmet, gloves, fire-retardant coverall
(for example Nomex®), dust mask
(minimum FFP-3), safety boots with steel
tip, and safety glasses or face shields.
Respiratory equipment is required for all
personnel doing vessel entry (see below).
Adsorbents react exothermic when
contacted with humidity and therefore
direct contact with moist skin, eyes and
mucous membranes should be avoided.
The MSDS sheets of the involved products
should be available and reviewed prior to
executing handling procedures. Contact
your Grace representative if the MSDS
sheets are missing.
If vessel entry is necessary, confined
space practices should be followed. Prior
to work starting, personnel must review
and implement confined space practices.
Grace recommends the use of respiratory
equipment when operators enter the
vessel to execute adsorbent levelling or
when sock loading method is used.
Since loading operations typically involve
lifting operations, safe practices for
lifting operations should be reviewed
and established by the operators. The
minimum required personnel for crane
operations is 2: the crane operator
executing the lifting work; and the rigger
foreman making sure the area is kept
free of people and waste, attaching the
big bags or cat bins (loading containers)
to the crane and supervising safe lifting
operations. Personnel should have the
required trainings and accreditations
to execute lifting works. Typically,
forklifts are also involved during loading
operations. The necessary safety training
and procedures should be established
before forklift operation begins. Before
work begins, forklift operators should
be trained and approved to execute
operating a forklift.
2.1.2) Equipment and loading
preparations
Prior to the loading operations, the
necessary equipment should be on-site
and readily available.
The necessary mesh screens should be
available on-site, cut at the right diameter,
and delivered with the correct mesh
opening. For guidelines on mesh screen
size, refer to paragraphs 2.2 and 2.4.
The required ceramic ball and adsorbent
materials per vessel should be lined
up before loading procedures, so that
there is little margin for error. Operators
should be briefed regarding the required
amounts of products per vessel and
maintain track-records of the drums and
big bags of material that are loaded for
each vessel. Each installed layer should
be noted down with its installed mass and
layer height measured from a fixed point,
for example, the top flange. If further
assistance is required, contact your Grace
representative. Grace can provide loading
sheets for tracking the loading operations.
Free-fall loading and sock loading are the
loading methods that should be followed.
If using free-fall loading, the maximum
free-fall height should not exceed
10 meters (32.8 ft). The necessary
equipment required to execute free-fall
loading includes a lifting crane, loading
hopper or funnel to be installed at the
top of the vessel, availability of cat bins
(loading containers) in case the adsorbent
is delivered in drums, and a device to
level each adsorbent layer. If using the
sock loading method, a sock is connected
to the loading hopper or funnel at the
top of the vessel. The sock is at the right
length (close to bottom of the vessel) at
the start of loading and is shortened as
the loading works continue to minimize

the fall length of the adsorbent to roughly
1 meter (3 ft) resulting in less dust
formation and abrasion.
If Grace® adsorbents are delivered
in drums, they should be opened
and emptied into the cat bin (loading
container). Loading containers can usually
contain up to 4 drums. To empty the
drums safely into the loading containers,
scaffolding with a plateau at height
should be constructed. The height of
the plateau should be slightly above
the loading container height. A forklift is
used to put the drums on the scaffolding
plateau from where operators can empty
the bins into the empty loading container
placed at ground level. Prior to working
with scaffolding, safe practices should be
implemented and reviewed. Operators
working on the scaffolding should be
provided with fall protection equipment in
addition to the already required PPE. A
loading crew should have several loading
containers (cat bins) at their disposal
during the transfer of adsorbent from
drums to the loading container, which
should be a continuous process beginning
Figure 1: Handling practices for sock loading of adsorbent material supplied in drums
W. R. GRACE & CO. ­— SYLOBEAD® Adsorbents Handling Brochure
in the preparation stage. A minimum of
six (6) cat bins should be available to
continue operations uninterrupted. The
above practices are demonstrated in
Figure 1. Grace adsorbents delivered in
big bags can be lifted directly by crane as
represented in Figure 3.
Prior to progressing to step 2.2, the
vessels should be fully isolated from
process lines, the vessel bottom head
should be clean and free of dust and
debris, the vessel is at atmospheric
conditions, and the vessel should be dry.
If the vessel cleaning involved water,
necessary steps should be established
to dry out the vessel prior to loading
operations. Grace’s SYLOBEAD®
adsorbents do not require inert
atmosphere for loading operations.
Loading operations can only be executed
in dry weather. Loading during rainy or
snowy conditions is prohibited due to the
exothermic nature of adsorbents when in
contact with humidity.
For loading activities, the following
amount of personnel is required:
• Crane crew for lifting operations:
• 1 crane operator
• 1 rigger foreman
• Loading crew:
• 1 forklift operator transporting cat
bins or big bags back and forth
• 2 operators to fill cat bins
• 2 operators on top of the vessel
to handle cat bins or big bags
• 1 operator for vessel entry in
case of sock loading
• 1 shift supervisor
It is at the discretion of the customer
to decide to dedicate a number of their
operators to assist the loading crew, for
example, with filling of the cat bins. In
such case, loading crews may contain
less operators. This is a matter of
agreeing on the work distribution between
end-user & loading crew.
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 W. R. GRACE & CO. ­— SYLOBEAD® Adsorbents Handling Brochure

Bottom Manhole

20 US mesh

Hold-down ring 4 US mesh

Rope packing

Support grid

Support ring I-beam

Figure 2: Grid Support System

2.2) Loading of ceramic ball support
layers
With the installation of ceramic ball
support layers, the loading operations
begin. One final check of the correct
installation of the bed support system
should be made. There are two (2)
bed support systems: full bottom head
ceramic ball support system and a
grid support system, the latter being
represented in Figure 2.
Grid support system: The grid should
be placed on a non-interrupted support
ring that goes with the circumference
of the vessel. The grid is to be placed
perpendicular to the I-beams. Between
the grid and the vessel wall, sufficient
space should be provided for thermal
expansion during heating steps in a
TSA unit. The space should be filled
with ceramic rope packing or rock wool
packing to prevent ceramic balls falling
into the gap. The grid should be covered
with two (2) mesh screens, cut to the
same diameter as the vessel internal
diameter. Typically, a 4 US mesh is
placed directly on the grid, covered by a
20 US mesh on top. The mesh screens
are kept in place by a hold-down ring. If
V-wire profile Johnson screens are used,
no extra mesh screens are needed. On
top of the 20 US mesh screen come the
ceramic ball support layers.
For the loading of the ceramic ball
support layers on top of the support
grid, Grace follows the “double size
philosophy”. This means that every
layer should be supported by a layer
consisting of particles that are double
in size. As a minimum, two (2) layers
of ceramic balls should be used, each
75 mm (3 inch) in height. For vessels
with an internal diameter larger than 4
m (13.12 ft), we recommend the use of
an extended support ball configuration.
Refer to Table 1 to determine which
ceramic ball size to install.

ID < 4 m ID > 4 m ID < 4 m ID > 4 m

Last adsorbent layer Small beads (1.6 – 2.5 mm) Large beads (2.5 – 5 mm)
1/8” balls 1/8” balls 1/8” balls 1/8” balls
CB layer 3
75 mm / 3” layer 75 mm / 3” layer 75 mm / 3” layer 100 mm / 4” layer
¼” balls ¼” balls ¼” balls ¼” balls
CB layer 2
75 mm / 3” layer 75 mm / 3” layer 75 mm / 3” layer 100 mm / 4” layer
½” balls
CB layer 1 - - -
75 mm / 3” layer
GRID + Mesh screens

Table 1

Page 3

ID < 4 m
Last adsorbent layer Small beads (1.6 – 2.5 mm)
1/8” balls
CB layer 4
75 mm / 3” layer
¼” balls
CB layer 3
75 mm / 3” layer
½” balls
CB layer 2
75 mm / 3” layer
1” balls till 75 mm
CB layer 1
from TL
Full bottom head ceramic ball
support system: A full bottom head
ceramic ball filled support system
indicates there is no support grid
system, and only ceramic balls are used
to ensure the necessary mechanical
strength and support for the adsorbent
layers. For the filling of the bottom head,
we recommend maintaining the same
“double size philosophy”. Therefore,
typically 1 inch ceramic balls are used
to fill the bottom head till 75 mm (3 inch)
from the bottom tangent line, followed
by the layers of smaller ceramic balls as
represented in Table 2.
The loading of the ceramic balls can
be executed via the bottom manway
or the top manway. The recommended
easiest and safest way to perform the
loading of the ceramic ball is t from the
top manway as the bottom manway
can already be closed. If closed, there
will be no big bag or loading container
hanging next to the vessel.
Ceramic balls are usually loaded via
sock loading. The required amount
of balls is transferred from drums to
loading containers which are lifted to the
vessel top, or if delivered in big bags,
the bags can be lifted directly. On top
of the vessel, a loading hopper (funnel)
is positioned with a sock inserted into
the vessel. The lifted loading container
or big bag is emptied into the hopper.
Typically, an operator enters the vessel
to manipulate the sock reducing the
speed and evenly distributing the
W. R. GRACE & CO. ­— SYLOBEAD® Adsorbents Handling Brochure
ID > 4 m
1/8” balls
75 mm / 3” layer
¼” balls
75 mm / 3” layer 75 mm / 3” layer
½” balls
75 mm / 3” layer 75 mm / 3” layer
1” balls till 75 mm 1” balls till 75 mm
from TL
Table 2
balls over the vessel surface area,
additionally leveling the different
layers after loading. For all scenarios,
each layer should be levelled prior to
beginning the loading of the next layer.
A mesh screen should not need to be
installed between the top ceramic ball
layer in the bottom support set-up and
the adsorbent, or between the adsorbent
layers itself. The extra mesh screen
installation complicates the loading
operations and subsequent unloading
operations later. It is the customers’
discretion to install intermediate mesh
screens or not, in mutual agreement with
the vessel mechanical design contractor.
2.3) Loading of adsorbent
After installation of the bed support and
ceramic ball support layers, the loading
of the adsorbent layer(s) can begin. As
previously indicated, the adsorbent can
be loaded by sock loading or by free-
fall loading.
If the material is delivered in drums,
the adsorbent is typically transferred
to loading containers (cat bins) which
are lifted to the top of the vessel (see
Figure 1). If the material is delivered
in big bags, those can be lifted
themselves (see Figure 3). The loading
container or big bag respectively, are
emptied into the loading hopper on
top of the vessel. The adsorbent then
flows into the vessel by either free-
fall loading or by sock loading. With
sock-loading, an operator should be
ID < 4 m ID > 4 m
Large beads (2.5 – 5 mm)
- -
¼” balls ¼” balls
100 mm / 4” layer
¼” balls ½” balls
100 mm / 4” layer
1” balls till 75 mm
from TL from TL
present in the vessel, manipulating the
sock to reduce speed and distribute the
adsorbent over the vessel area.
Each separate adsorbent layer should be
levelled after being completely loaded and
before beginning the loading of the next
layer. For large vessels, where different
layers of adsorbent can be larger than 40
ton, we recommend to level every 20 ton
in case of using sock loading. To enhance
the natural distribution of the adsorbent
and engage in less leveling efforts, free
fall loading should be conducted.
If loading operations need to be interrupted,
due to bad weather or shift changes,
the top manway should be closed by a
plastic flange or plastic foil to prevent
moisture ingress onto the adsorbent.
Adsorbent volume is irrelevant
for guaranteed performance.
Adsorbent mass is the key parameter
for performance. As a consequence,
deviations in adsorbent layer heights
might exist between the initially provided
estimated loading diagram, and the
actual loading diagram due to differences
in estimated and actual density of the
adsorbents. This is normal and has no
influence on performance, for as long as
the required adsorbent weight is installed.
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W. R. GRACE & CO. ­— SYLOBEAD® Adsorbents Handling Brochure
Figure 3: Handling practices for sock loading of adsorbent material supplied in big bags
2.4) Installation of floating mesh
screen
We recommend the installation of a
floating mesh screen in the top of the
vessel, between the top adsorbent layer
and the hold-down layer of ceramic balls
on top. This mesh screen is typically a 20
US mesh screen. This is a floating mesh,
and thus not fixed onto the vessel. The
adsorbent should settle during operation,
causing the installed ceramic ball hold-
down layer on top to settle. This floating
mesh serves as a basket to maintain the
ceramic balls in place with allowance for
bed settling. We recommend a 150 mm
(6 inch) layer of ceramic balls to serve as
a basket and the floating mesh should be
folded upwards against the vessel wall
for 200 mm (8 inch); the diameter of the
floating mesh in the top should equal the
vessel ID plus 400 mm (16 inch).
2.5) Loading of hold-down layer of
ceramic balls
After loading of the adsorbent and the
floating mesh screen has been installed
correctly, the loading of the hold-down
Page 5
layer of ceramic balls should begin and is
generally performed by sock loading. This
is usually a 150 mm (6 inch) layer of ½
inch balls. The ceramic balls are loaded
into the loading container, which is lifted
to the top of the vessel and emptied into
the loading hopper, from where they flow
into the sock for equal distribution into the
vessel. The layer should be levelled at the
end of the loading.
2.6) Completion of loading procedures
Once the loading is finished, the
vessel needs to be closed as soon as
possible. The required flanges should
be installed and the vessel prepared
for N2 purging. The vessel needs to be
purged until O2 levels are below 0.5
vol%. If you do not have sufficient N2
available on site for purging, repeated
re- and depressurization steps with
N2 can also support reduction of O2
levels. Once the required O2 levels
are achieved, the vessel should be
kept under positive N2 pressure until
process piping is connected.
It is strictly prohibited to maintain
a vessel loaded with adsorbents,
pressurized and stagnant with a
hydrocarbon containing gas. There must
be flow applied when an adsorbent bed
is pressurized with hydrocarbon gas.
The loading track records should
be collected and the actual loading
diagram should be constructed with
the adsorbent loading contractor and a
Grace representative, if present. Grace
needs to be provided the “as loaded”
vessel loading diagram to cross-check
the design and guarantees.
After the process piping is purged
to low oxygen level – typically by N2
purging – it should be connected to the
adsorber unit. The adsorber should be
ready for use. Grace® adsorbents can
be immediately put in use as delivered
and do not require an extra regeneration
or activation step prior to being used
in adsorption processes. While an
initial regeneration is not required,
there is no harm in performing it. It is
of the operator discretion to perform

an initial regeneration or not. Grace
Technical Customer Service (TCS) may
recommend initial regeneration steps for
products that have been stored overtime
in the warehouse i.e. when there is
an extended period of time between
the delivery of the adsorbent and the
installation of the adsorbent.
3) Start-Up and
Commissioning
Adsorbent loading is generally one of the
many activities happening during a plant
turn-around or plant construction and
commissioning. Consequently, there may
be a significant time gap between the
end of the loading and the start-up of the
plant and adsorption unit. Until start-up,
the adsorbent unit is to be kept under
positive inert atmosphere. Refer to section
3.6 where N2 purging is described after
finalization of the loading process.
Once the adsorbent loading is finished
and the adsorber vessel is put under N2
pressure, the next step is connecting to
the process piping. The piping should
be free of liquids, dust and any other
debris, and is also purged with N2 up to
the next nearest flange. The connection
is made between the adsorber vessel
and the next nearest flange of process
piping. All flanges should be checked
for proper connection and a leak test
should be performed.
An additional step can be performed to
remove dust that may have potentially
formed during or after loading operations.
If desired, this can be completed by
passing inert gas over the product gas
filters. Repeated depressurizations to
the product gas filters can also work to
remove dust. It could be possible that
the product gas dust filters need to be
changed after performing this step prior
to plant start-up. If no dust removal is
done, faster blocking of the product gas
filters can be expected, as the dust will
be removed during first adsorption cycle.
The way loading is done will largely
define if there is dust and the content of
the dust formation.
W. R. GRACE & CO. ­— SYLOBEAD® Adsorbents Handling Brochure
Prior to start-up of the unit, an initial
regeneration can be performed. This is
an optional step. Grace’s SYLOBEAD®
adsorbents are generally freshly delivered
and installed and should not require an
initial regeneration if loaded under the
proper conditions, as advised to perform
loading operations outside humid seasons
and as we recommend against loading
during rain, snow, or any other form of
precipitation. Only for adsorbents that
have been stored for an extended period
in the warehouse, an initial regeneration
step can be beneficial. Discuss with your
Grace representative if there is a need
for an initial regeneration. If required, the
initial regeneration can be performed with
process regeneration gas, provided it is
already available at that stage, or N2.
In the next phase, applicable for
adsorber units processing liquid phase
streams, the adsorber vessel needs to
be filled with liquid. For adsorber units
processing paraffinic liquid hydrocarbons,
the filling can be done directly with clean,
dry process liquid, if available. Otherwise
feed stream liquid will need to be used. In
order not to disturb the bed configuration,
maintain below lifting limits with liquid
flow rate. Units processing olefinic liquid
streams and utilizing molecular sieves of
the type 4A, 5A or 13X require an extra
preloading step to avoid excessive heat
of adsorption from olefinic components.
Units utilizing 3A-type adsorbents do not
require this step. For preloading, we refer
to the intermezzo specifically dedicated
to preloading. The preloading step is
required in gas phase adsorber units
processing olefinic gas phase streams
and utilizing molecular sieves of the type
4A, 5A or 13X.
Intermezzo – Preloading procedure
The preloading step is applicable for both
gas and liquid phase units that process
olefinic streams and use molecular sieve
types 4A, 5A or 13X. It generally comes
after the initial regeneration step – if
applicable – and prior to the filling step
(liquid units) or the process adsorption step
(gas phase units).
The preloading step can be performed in
the gas phase or in the liquid phase. For
a liquid phase preloading step, the bed
is filed first with paraffinic liquid followed
by introducing the process olefinic liquid.
This is called a displacement step. As the
bed is already filled with paraffinic liquid,
introduction of the olefinic liquid after will
not cause high heat of adsorption.
The gas phase preloading step follows
the philosophy of typically using N2 stream
with olefinic component blended into it at
2.5 – 5 mol%. This is typically completed in
2 separate preloading steps. The first step
processes N2 with 2.5 mol% olefin, while
the second step processes N2 with 5 mol%
olefin. Temperature should be monitored
during the steps and should be kept below
80 °C / 176°F. In case temperature rises
above that value, the olefinic stream
blended into the N2 flow should be cut off
and purged with pure N2. We recommend
the following practical guidelines:
Kmol/100 kg
adsorbent
Preloading 1 10
Preloading 2 4
As an example, an adsorbent bed
with 10 ton SYLOBEAD® 13X used in
propylene service needs 1000 kmol
during preloading 1 and 400 kmol during
preloading 2. Say N2 is used with 2.5
mol% propylene during preloading 1 and
with 5 mol% during preloading 2, one
can set a flow and calculate the duration
of the preloading steps. Assuming for
example 2000 kg/h is used as flow
rate, preloading 1 takes 14 hours and
preloading 2 6 hours.
The gas phase preloading step can be
applied to both gas and liquid olefinic
stream processing adsorbent units. In
case gas phase preloading is done in an
adsorbent unit processing olefinic liquid
phase, the next step is the filling step,
followed by putting the bed in adsorption.
For an adsorbent unit processing gas
streams, the preloading step comes prior
to putting the bed in service.
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W. R. GRACE & CO. ­— SYLOBEAD® Adsorbents Handling Brochure
Once the adsorbent unit has been
preloaded and/or filled, the adsorber
vessel can be taken into operation. Gas
and liquid phase units procedure:
Open the process valves (inlet and
outlet) and allow process fluid, gas
or liquid phase, to flow through the
adsorbent bed. Confirm the DCS
system is activated and programmed
with correct adsorber unit operational
parameters from the Grace design and
verify it is monitoring the adsorption time
and all relevant process parameters
related to the adsorbent unit such as
feed stream temperature, pressure
and feed rate; regeneration fluid
temperature, pressure and flow rate;
adsorption, heating and cooling times;
and adsorber unit pressure drop. Do
not operate the adsorber unit below
its minimum turn-down rate. This will
result in channeling and incomplete
usage of the bed, with perceived short
cycle time and early breakthrough or
slippage of contaminants. Contact your
Grace representative for guidelines on
minimum allowable flow rates. During
start-up of the first cycle, monitor the
adsorber unit temperature to confirm
there is no excessive heat formation.
It is normal that the temperature can
rise by a delta of 5°C due to the heat
of adsorption of contaminants that are
getting removed by the adsorbent.
Under normal operating conditions,
most of the heat of adsorption is
carried away by the process stream.
This provides an additional reason to
run above minimum turn-down rates.
Excessive heat could induce reactions
in presence of reactive components
like acetylene, ethylene, propylene,
isobutylene since adsorbents offer a
large surface area where reactions
can take place. Grace’s SYLOBEAD®
adsorbents are not catalytically
active and will not induce reactivity
by themselves. Reactivity will only be
observed if the following 3 conditions
are obeyed: the inherent chemical
reactivity of certain components, the
presence of the necessary reaction
energy (due to excessive heat of
adsorption) and the availability of large
surface area. While inherent chemical
Page 7
reactivity of components cannot
be avoided, for example ethylene,
and while large surface area is an
inherent characteristic of adsorbents,
the presence of the required reaction
energy can be avoided by following
the proper start-up and commissioning
guidelines, avoiding excessive heat
of adsorption. If a temperature rise is
observed during the start-up phase that
goes beyond 65°C (150°F), the process
flow should be stopped immediately and
the vessel should be purged with N2 to
lower the temperature.
Under no circumstances can the
adsorber unit be kept stagnant,
pressurized with hydrocarbon process
fluid for more than 6 hours. If this
happens, the unit needs to be purged
with N2 till below 50% of LEL (Lower
Explosion Limit) and can only be boxed
in after that.
Once the process flow is introduced, the
process flow can continue to be ramped
up to a normal flow rate as soon as
possible and the adsorption unit will be in
full operation. Refer to the Grace design
summary for all relevant set points such
as adsorption cycle time, regeneration
cycle times, etc.
4) Unloading Activities and
Handling Spent Adsorbent
At the end of the adsorbent service life
which usually collides with the plant
turn-around schedule, the adsorbent
needs to be unloaded and the unit needs
to be inspected, repaired if needed, and
reloaded for the next service cycle.
4.1) Deactivation of spent adsorbent
Prior to unloading, the installed
adsorbent needs to be prepared and
deactivated. This is particularly important
since adsorbents are often used to
process hazardous streams. Processing
hazardous streams includes, but is not
limited to, processing flammable or
explosive components like hydrocarbons,
or processing streams with toxic
components like H2S.
The first method is to regenerate the bed
and purge it with N2 till below 50% of LEL
(Lower Explosion Limit). The installed
adsorbent should be regenerated with
clean gas. This can typically still be the
clean, dry regeneration gas from the
process. If that gas is no longer available,
N2 can be used as an alternative.
After regeneration, the adsorber unit is
to be made free of hydrocarbons until
below LEL. This is done by purging N2,
or by repeated de-/ and repressurization
with N2 if the available N2 flow rate is not
sufficient for efficient purging. Consult
your Grace representative for guidelines
on minimum acceptable N2 flow rates to
have proper flow distribution.
The vessel can now be ready for dry
unloading practices. Unloading can be
done by vacuum unloading from the top,
or by gravity unloading by dumping the
material from the bottom side manway
/ dump nozzle. The top manway can
be opened for vacuum unloading
and if gravity dumping is chosen, the
side dump nozzle can be opened as
well. NEVER APPLY AN ACTIVE
AIR PURGE TO THE VESSEL DUE
TO RISK OF FIRE, EXPLOSION OR
TOXIC RELEASE. While the adsorbent
is regenerated, local spots with
accumulated hydrocarbons in the form
of heavier polymerized components or
in the form of coke, might still be present
on the adsorbent. If exposed to air, they
impose an explosion risk and/ or a risk
of fire. Additionally, exposure to humid
air my release components still present
on the adsorbent surface, as water will
displace any other adsorbed component.
Thus, the risk to release toxic or reactive
compound to the environment arises.
This is the main disadvantage of
regeneration and N2 purge method. The
advantage is that no water is involved in
the deactivation steps, avoiding intensive
cleaning and drying after the unloading
procedure is completed. Adsorber units
that are processing H2S and/or sulfur
containing streams or reactive olefinic
streams, are best to not be deactivated
using regeneration and N2 purging, but
with the next available method: water

flooding. The regeneration and N2 purge
method is most suitable for adsorber
units processing relatively inert and clean
process streams, for example lean sweet
natural gas driers.
The second method is water flooding.
This method is advisable when the
adsorbent unit has been used on toxic
and/or reactive streams. Water will
completely displace all other adsorbed
molecules from the adsorbent. By
saturating the adsorbent with water,
it becomes fully pacified even if there
were still “hot spots” present due to
improper regeneration. Disadvantages
in this method include: handling of
the spent water which will contain
hydrocarbons and/or toxic components
like H2S in an environmentally
acceptable way; potential mud or slurry
formation of adsorbent(s) exposed to
excessive amounts of liquid water,
making the unloading more difficult,
regardless if that’s done by gravity or
by vacuum unloading; and intensive
cleaning and drying is required after
adsorbent unloading.
Prior to executing water flooding,
confirm the vessel mechanical design
allows for water flooding. As a first
step, the adsorber vessel needs to
be regenerated with either the normal
process regeneration gas or N2.
After cooling down, the vessel will be
disconnected from the process and all
blinds installed. Only the flare connection
should be kept in place (usually at the
top) and a water hose can be connected
from the bottom. Liquid water can be
introduced from the bottom and fill the
vessel. Steam formation is expected. The
filling height can be monitored by using
a differential pressure gauge and the
principle of hydrostatic pressure. Avoid
overfilling or flare line flooding. After
filling, drain the water by closing the flare
line and disconnecting the water hose.
A vent line should be open to prevent
the vacuum from draining. Prior to
opening the blind flanges for unloading,
the vessel should be checked to be
below LEL once draining is complete.
Apply N2 purge to monitor LEL. If results
W. R. GRACE & CO. ­— SYLOBEAD® Adsorbents Handling Brochure
are not satisfactory, perform a second
water flooding. Otherwise the vessel
top manway can be opened to the
atmosphere. Do not apply an active air
purge to the vessel. The adsorber can
now be unloaded.
4.2) Unloading and handling of spent
adsorbent
Once the adsorbent has been prepared
for unloading by means of one of
outlined methods, the actual unloading
can begin. The top manway is opened
to the atmosphere and all necessary
safety precautions should be in place.
Unloading always starts with removing
the top hold-down layer of ceramic
balls and the floating mesh screen.
The ceramic balls can be removed
by vacuum suction or manually with
buckets. The floating mesh is to be
removed manually. Safe vessel entry
practices should be in place at all times.
The adsorbent material is then unloaded.
If using gravity unloading, the bottom
side dump nozzle can be opened and
the adsorbent will start to flow out. The
necessary containers should be present
to collect the adsorbent flowing out. The
bottom ceramic ball support layers are
usually located below the dump nozzle
and need to be removed by manpower.
If using vacuum unloading, the bottom
manway stays closed and vessel entry is
done from the top manway by an operator
equipped with respiratory equipment,
handling the vacuum hose and removing
the adsorbent by suction. The bottom
side manway is opened once the level
of adsorbent is below the manway and
the bottom ceramic ball support layers
are removed by vacuum suction from the
bottom side manway.
If the material has been pacified by
water flooding, vacuum unloading may
be more difficult due to potential mud
and lump formation of the material when
exposed to excess liquid water. However,
if water flooding has been used properly,
the concern of potentially releasing
of toxic components by exposure of
the unloaded material to atmospheric
conditions by gravity dumping is off the
table. If the adsorbent has been prepared
for unloading by regeneration and N2
purging, unloading by vacuum unloading
is advised since the dry adsorbent
will be contained in the vacuum truck
containers and not openly exposed to
the atmosphere. If dry gravity dumping
is performed and the spent adsorbent
is dumped into open containers, we
recommend to have the containers
removed from site as quickly as possible
and not expose them to water contact.
There is one additional unloading
method where everything is kept in inert
atmosphere. The adsorbent is then
prepared for unloading by regeneration
and inert purging with N2, after which the
vessel is kept under N2 atmosphere. The
unloading is typically gravity dumping by
a controlled flow of spent adsorbent and
the whole unloading is executed under N2
atmosphere. The adsorbent is captured in
inerted drums and stored in sealed inerted
drums, which are sent off site for disposal.
This method is the most time-consuming
and requires a large amount of N2 input.
Contact a specialized catalyst and
adsorbent handling company to execute
this work. In general, inert unloading is not
required with Grace adsorbents. However,
it might be considered for adsorbent units
in sweetening service, where proper
deactivation of the adsorbent prior to
unloading is difficult for the operators.
Refer to local legislation for the disposal
of the spent adsorbent. We recommend
to find local companies that are allowed
to handle spent adsorbents and have
the necessary accreditations to dispose
of spent adsorbents. Some typical
applications include but are not limited to,
land fill or usage as filler in concrete for
the building industry.
Grace has collaborated for many years
with several catalyst handling companies
such as Mourik, Group Peeters,
Unidense, Petroval, Buchen ICS, Cat
Tech Ltd., Anabeeb, Al Muzain, HPA
Global Reactor Services, in the industry
but does not indicate any preference or
endorsement of any of these companies.
grace.com | Page 8
 5) Storage of Adsorbents
Grace’s SYLOBEAD® adsorbents are
delivered in drums or in big bags on
pallets. They need to be stored in a
dry warehouse, on a dry clean surface,
and shielded from direct sun light and
weather elements like wind, snow, rain or
any form of precipitation.

The shelf life of the adsorbents is

typically 4 years for material delivered in
drums and 1 year for material delivered
in big bags.

References
SYLOBEAD® product information sheet
and safety data sheets

Grace Corporate Headquarters Regional Locations

W. R. Grace & Co.-Conn. Latin America Asia/Pacific Europe

7500 Grace Drive São Paulo, Brasil Shanghai, China Worms, Germany
Columbia, MD 21044 USA Tel: +55.11.4197.7540 Tel: +86.21.3325.8288 Tel: +49.6241.40300
Tel: +1.410.531.4000

The information contained herein is based on our testing and experience and is offered for the user’s consideration, investigation
and verification. GRACE DISCLAIMS ALL WARRANTIES EXPRESSED OR IMPLIED, regarding the advice and instructions provided
herein and all results obtained from the use of our products, since customer operating and use conditions vary and are beyond
Grace’s control. Test methods are available on request. GRACE® and SYLOBEAD® are trademarks, registered in the United States
and/or other countries, of W. R. Grace & Co.-Conn. TALENT TECHNOLOGY TRUST™ is a trademark of W. R. Grace & Co.-Conn.
This trademark list has been compiled using available published information as of the publication date of this brochure and may
not accurately reflect current trademark ownership or status. © 2021 W. R. Grace & Co.-Conn. All rights reserved.