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CECA -Adsorbents Handling Procedures

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    PROCEDURE

    CECA ADSORBENTS FOR THE OIL AND GAS INDUSTRY  

    HANDLING

    PROCEDURES

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    CECA Adsorbents Handling Procedures

    CONTENT :

    INTRODUCTION

    BASICS OF ADSORPTION

    STORAGE INSTRUCTIONS

    HANDLING INSTRUCTIONS

     VESSEL LOADING INSTRUCTIONS

     VESSEL UNLOADING INSTRUCTIONS

    DISPOSAL OF CECA ADSORBENTS

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    CECA Adsorbents Handling Procedures

    INTRODUCTION

    This document details CECA requirements for the

    handling of adsorbents (molecular sieves, activated

    alumina, silica gel) and ceramic balls in process units.

    All the information and recommendations enclosedshould be well understood in order to optimize the

    loading, unloading and disposal operations, and to

    perform them safely.

    This document is for the sole internal use of CECA

    adsorbents customers. It is confidential and not to bedisclosed to any third party without CECA explicit

    consent in writing.

    Do not hesitate to contact us for any question you

    may have :

    CECA S.A., Molecular Sieve Department

    Dynamic Applications

    Tel : +33 1 49 00 38 19

    Fax : +33 1 49 00 38 03Email : [email protected]

    BASICS OF ADSORPTION

    In gas and liquid separation applications, the aim is

    to selectively retain molecules that form low energy

    bonds with the adsorbent internal structure. This

    phenomenon is called physisorption and follows

    adsorption isotherms. It is exothermic (it releasesenergy in the form of heat).

    To be efficiently adsorbed, the polar molecules must

    be small enough to enter the cavities of the adsorbent

    via their pores. The diameter (or the size distribution)

    of the pores and cavities depend on the type ofadsorbent, which is therefore chosen depending on

    the application and the molecules to be separated.

    Typical adsorbents are available in the form of 0.5 to

    5.0 mm beads or pellets. They are loaded in vessels

    and used as fixed bed.

    The impurities in the treated stream saturate the

    adsorbent bed generally within a few hours or days.

    By changing the adsorption equilibrium conditions

    (lower pressure, higher temperature or both), the

    adsorbed molecules can be desorbed from the active

    sites, and the adsorbent can recover most of itsoriginal adsorption capacity: it is “regenerated”.

     Introduction

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    CECA Adsorbents Handling Procedures

    STORAGE INSTRUCTIONS

    CECA adsorbents are shipped in air-tight, non

    returnable steel drums or semi-bulk bags (called “big

    bags” in the following). See our Standard Offer for

    Packing, Marking and Expedition for details.

    In all cases we recommend to warehouse the pallets

    indoor in order to prevent them from bad weather

    conditions (rain, sand storm, etc.), direct sun and

    ground humidity.

    Outside storage is not recommended, in particular forbig bags. Should indoor storage not be feasible, the

    drums or big bags pallets would have to be protected

    by waterproof tarps and be isolated from the ground.

    In the case of big bags, outside storage has to be

    limited, in all cases, to short periods (for instance

     just before loading the vessels).

    The drums can be stored up to 5 years under cover.

    Big bags cannot be stored for more than 2 years, even

    under cover. For longer storage durations, we

    recommend to sample and analyse the products, in

    order to make sure they are still fit for use.

    These recommendations are general and may slightly

    differ depending on the product type, packaging,

    storage location, etc. In any case, ask CECA to make

    sure your storage conditions meet our requirements.

    HANDLING INSTRUCTIONS

    Before handling CECA adsorbents, read the

    corresponding Material Safety Data Sheet (MSDS)

    for the up-to-date safety, handling and regulatory

    information.

    CECA adsorbents are silica gels, aluminas or

    alumino-silicates (zeolite-based molecular sieves).

    They are chemically similar to ordinary clays and are

    therefore inert under normal handling conditions.

    They exhibit no vapour pressure and have no

    flammable constituents.

    The main potential serious hazard is related to non

    (or poorly) regenerated adsorbents desorbing

    hazardous species (H2S, etc.) after unloading of the

    vessels. This scenario and how to avoid it is

    described in CECA Unloading Procedure.

    CECA adsorbents are extremely powerful desiccants.

    They remove water from any substance they come in

    contact with. As adsorption is exothermic, it can

    cause burns to a sweating skin. Gloves must be worn

    while handling CECA adsorbents. No adsorbent dust

    must be inhaled or allowed to come in contact witheyes. The use of dust mask, goggles, and Breathing

    Apparatus systems, if in confined space, are

    mandatory. Excessive or severe handling can cause

    some dusting.

    Do not hesitate to contact us for any question you

    may have :

    CECA S.A., Molecular Sieve Department

    Dynamic Applications

    Tel : +33 1 49 00 38 19

    Fax : +33 1 49 00 38 03Email : [email protected]

     

    The statements, technical information and recommendations contained herein are believed to be accurate as of the date hereof. Since

    the conditions and methods of use of the product and of the information referred to herein are beyond our control, ARKEMA expressly

    disclaims any and all liability as to any results obtained or arising from any use of the product or reliance on such information; NO

    WARRANTY OF FITNESS FOR ANY PARTICULAR PURPOSE, WARRANTY OF MERCHANTABILITY OR ANY OTHER WARRANTY, EXPRESS

    OR IMPLIED, IS MADE CONCERNING THE GOODS DESCRIBED OR THE INFORMATION PROVIDED HEREIN. The information provided

    herein relates only to the specific product designated and may not be applicable when such product is used in combination with other

    materials or in any process. The user should thoroughly test any application before commercialization. Nothing contained herein

    constitutes a license to practice under any patent and it should not be construed as an inducement to infringe any patent and the user

    is advised to take appropriate steps to be sure that any proposed use of the product will not result in patent infringement. See MSDS for

    Health & Safety Consideration

    CECA

    89, boulevard National

    92257 La Garenne-Colombes Cedex - France

    cecachemicals.comStorage & Handling 1/1

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    CECA Adsorbents Handling Procedures

    VESSEL LOADING INSTRUCTIONS

    These instructions detail the standard loading method.

    Special methods such as dense loading or pneumatic

    loading are not discussed here.

    1/ REQUESTED EQUIPMENT

    1.1/ Area

    Enough space is needed around the vessels to store

    the drums or big bags. As a reminder, ground surface

    for 1 pallet (4 drums or 1 big bag) is about 1m2.

    Moreover, some space is necessary for the loadingprocess : filling the hopper, crane and forklift

    manoeuvres, etc.

    1.2/ Hopper and loading system

    Except for the bottom ceramic balls (see § 5.3/below),

    the products are usually loaded via a hopper.

    In the case of drums, it is recommended to first pour a

    few drums in the hopper, and to lift the hopper with a

    crane (the hopper must be equipped with lifting

    hooks).

    Loading drums one by one is not recommended as

    the quantities involved are important. Big bags can

    also be first poured in a hopper, or they can

    alternatively be lifted directly. See Figures 1 and

    Figure 2 below.

    When a hopper is used, its capacity and resistance

    must comply with the requested use (1 pallet = 4 to 5drums = 500 to 700 kg) or 1 big bag (800 to 1000 kg).

    The bottom opening must be large enough to preventclogging. A diameter of 150 mm is a minimum (300

    mm is recommended).

    The hopper valve must be easy to operate and must be

    able, if needed, to quickly stop the product without

    crushing the beads or pellets. A guillotine valve isusually the best compromise. When big bags are used

    and directly lifted, their bottom short sleeve must be

    opened with care and the flow of product must also be

    controlled.

     Loading 1/7

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    CECA Adsorbents Handling Procedures

    Attached to the bottom of the hopper, or to a cone-

    shaped system fixed to the manhole (in particular

    when big bags are lifted), a long sleeve prevents the

    adsorbents from falling from too high. It is a flexible

    cylinder-shape piece, which diameter is at least equalto the diameter of the bottom opening of the hopper or

    cone-shaped system.

    The sleeve can be made from various flexible,

    resistant materials, such as any cloth, plastic films,flexible pipes, constructions conducts, etc. Its length

    is reduced from time to time, in order to always havebetween 600 and 1000 mm from the bottom of the

    sleeve to the top of the bed. The sleeve must also be

    equipped with a rope attached to its end. This rope is

    used to direct the product flow inside the vessel.

    Example of an equipped hopper

    1.3/ Crane

    A crane is required to lift the filled hopper (or the big

    bags) from the ground up to the vessel manway.

    1.4/ Forklifts

    Forklifts are used to carry the drum or big bag pallets.Two forklifts is a minimum : one to bring full drums

    from the storage area to the hopper filling area, andanother to bring empty drums on pallets to another

    storage area.

    1.5/ Hopper filling area / Scaffolding platform

    When drums have to be loaded in a hopper, a securedplatform is convenient to handle the pallets and to fill

    the hoppers securely (see § 4.6 for details).

    Note: The platform can be replaced by a hole made in

    the ground, in which the hopper is loaded. In this casedrums are simply rocked on the hopper.

    sleeve

    rope

    valve

    Cone-bottomshaped hopper

    pouredproducts

    Figure 1

    sleeve

    rope

    valve

    Cone-bottomshaped hopper

    pouredproducts

    Figure 1

    liftedbig bag

    sleeve

    rope

    Figure 2

    liftedbig bag

    sleeve

    rope

    Figure 2

     Loading 2/7

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    CECA Adsorbents Handling Procedures

    1.6/ Safety equipments

    Safety / PPE (Personal Protective Equipment) outfits

    and fittings have to be available and used accordingto the plant’s safety rules. Contact CECA in caseyou have any question or any doubt. Equipment

    typically includes :

    Helmet, gloves, safety shoes, dust mask, harness,

    goggles, clothes with long sleeves, Breathing

    Apparatus systems, portable oxygen detector.

    1.7/ Wood boards and ladder

    A ladder (long enough to go from the top manway

    down to the support grid) is necessary. At least 3

    wood boards are needed in order to put up the ladderand walk on the bed during the levelling steps.

    Note : a winch can also be used instead of a ladder.

    1.8/ Rake 

    A rake (or a “rake-type” tool) is needed for bed

    levelling operations.

    1.9/ Rulers 

    Rulers are useful to measure the level of product in

    the vessel from time to time, and therefore controlits homogeneity all around the vessel after a

    levelling operation. Rulers have to be long enough.

    If they cannot be easily provided, they can be

    replaced by scaled ropes or by tape-measures.

    Note : an alternate solution is to graduate the vessel

    wall in several locations on its circumference and all

    along its height while the vessel is empty (for

    example using a chalk).

    1.10/ Stainless yarn 

    Stainless yarn is used when wire mesh screens aresupplied in several pieces that have to be partially

    overlapped and tied together (usually for large vesseldiameters).

    Note : blind rivets can also be used.

    1.11/ Spare screens

    For each kind of wire mesh screen in the vessel, it is

    necessary to have spares (and / or spare parts). This

    is true essentially for change outs, in order to be able

    to immediately replace former screens if damaged,

    or at least to repair them.

    1.12/ Tarpaulin - Plastic cover

    If sudden rain or snow occurs during the loading

    operation, it is important to be equipped to protect theproduct from exposure (hopper and vessels). For eachvessel, at least one plastic cover, to be put on the

    manhole, is requested. Tape is needed to fix it tightly.

    1.13/ Lighting equipment 

    Lights (flashlights, spotlights) are needed to see insideand inspect the vessels.

    1.14/ Other useful tools

    Cutters, scissors, adhesive tape, etc.

    2/ UTILITIES

    No specific utilities are required to perform CECA

    adsorbents loading. However, a source of inert dry

    gas (typically nitrogen) is highly desirable in order to

    purge and remove atmospheric air from the bed after

    loading.

    3/ MANPOWER

    In order to proceed securely, we highly recommend tohave at least 7 workers per team. We also suggest the

    following dispatch :

    Crane : 1

    Forklifts : 2

    Hopper filling / big bag preparation : 2

    Filling operation / levelling / supervision : 2

    The number of needed teams depends on the loading

    conditions (day shift, 24hr/day, several vessels loaded

    at the same time, etc.)

    Loading supervision can sometimes, upon request andcommercial agreement, involve a CECA

    representative. In that case, the CECA representativeis only responsible for indicating what has to be done

    and what has to be avoided. He / She has no

    hierarchical link with the loading team, and it is

    essential that he / she directly reports to a company

    official loading supervisor who organizes the work in

    practice.

    CECA representative can, at any time, instruct to

    stop the loading operation, upon circumstances

    which to his judgment, could result in unsafe or

    improper performance.

     Loading 3/7

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    CECA Adsorbents Handling Procedures

    4/ PRELIMINARY OPERATIONS & SPECIAL

    RECOMMENDATIONS

    4.1/ Typical vessel layout

    See Figure 3 for a typical vessel layout (may slightly

    differ from a unit to another)

    In some cases, a V-wire grid type (by “Johnson

    Screens” and others) is used instead of the support

    grid and bottom wire mesh screens.

    4.2/ Wire mesh screens

    The wire mesh screens that are installed over the

    grid and / or below the top ceramic balls must be

    new or damage free. For large vessel diameters, theyare usually supplied in several pieces that need to be

    partially overlapped (5-10cm) and well tied together

    with the use of stainless yarn, wire or blind rivets.

    4.3/ Grid – wall sealing

    Due to thermal expansion (especially in the case of a

    TSA - Temperature Swing Adsorption system), thesupport grid and the vessel show a little gap. In orderto prevent any product leakage, it is paramount to

    ensure a perfect sealing between the grid and the

    vessel wall. This is usually done with several layers

    of ceramic rope inserted in the gap.

    Ceramic rope sealing

    Figure 3

     Loading 4/7

    Ceramic balls layers

    Ceramic balls layers

    Ceramic balls 1”

    Alumina or Silica gel guard bed layer

    (when applicable)

    Molecular sieves layers

    Fiber rope around the

    whole circumference

    (gasket / tightness)

    Manhole /

    dump port

    Baffleplate

    with 4

    holes

    Inlet nozzle with rectangular slots

    showing suitable open area, and

    covered with 20 mesh screen*.

    Bottom of distributor

    Top of products

    600 mm

    mini.

    20 mesh screen*

    (+ 15 cm overlap)

    10 mesh screen*

    3 mesh screen*

    Main support grid

    I-beam supports 20 mesh screen*

    * US size N° 20, 10 and 3 Stainless Steel Mesh Screen

    Floating screen

    Optional and strongly recommended : Hold-down ring

    all around the vessel circumference, to reliably maintain

    the bottom screens and ensure a suitable tightness

    Ceramic balls layers

    Ceramic balls layers

    Ceramic balls 1”

    Alumina or Silica gel guard bed layer

    (when applicable)

    Molecular sieves layers

    Fiber rope around the

    whole circumference

    (gasket / tightness)

    Manhole /

    dump port

    Manhole /

    dump port

    Baffleplate

    with 4

    holes

    Inlet nozzle with rectangular slots

    showing suitable open area, and

    covered with 20 mesh screen*.

    Bottom of distributor

    Top of products

    600 mm

    mini.

    20 mesh screen*

    (+ 15 cm overlap)

    10 mesh screen*

    3 mesh screen*

    Main support grid

    I-beam supports

    20 mesh screen*

    (+ 15 cm overlap)

    10 mesh screen*

    3 mesh screen*

    Main support grid

    I-beam supports 20 mesh screen*20 mesh screen*

    * US size N° 20, 10 and 3 Stainless Steel Mesh Screen

    Floating screen

    Optional and strongly recommended : Hold-down ring

    all around the vessel circumference, to reliably maintain

    the bottom screens and ensure a suitable tightness

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    CECA Adsorbents Handling Procedures

    In addition to that, the upper 20 mesh screen overthe grid must be larger than the vessel diameter in

    order to provide a 10-15 cm overlap up the wall. A

    hold-down ring that maintains the mesh screen is

    recommended.

    Mesh screen with overlap and a hold-down ring

    4.4/ Clean and dry vessel

    Before the loading starts, the vessel and all internals

    must be perfectly clean and dry (air movers or dry

    gas blowers may have to be used). It is extremely

    important to make sure there is no remaining dead

    volume of water.

    4.5/ Side manhole blind

    The side manhole can sometimes represent a

    significant volume. It is recommended to insert a

    blind with a few tiny hole for pressure equalization.(The holes must be small enough to prevent beads or

    pellets to go through.) See Figure 4.

    Figure 4

    4.6/ Management of drums and big bags

    It is very important to foresee and organize the

    transfer of the drums and big bags from their mainstorage to the loading operation area. Removal /

    disposal of empty packaging has to be planned aswell, in order not to clutter the loading area.

    The quantity of big bags and / or drums

    corresponding to a given vessel load must be stored in

    a dedicated area near it. They must be arranged in theorder of loading.

    When loading a hopper with drums using a platform,

    bring the pallet on the platform with a forklift. Drums

    are brought one by one to the tilting area of the

    scaffolding. They are opened and poured into the

    hopper. Empty drums are brought back on the pallet,and the pallet with empty drums is brought to the

    specific storage area by the second forklift.

    Example of a platform

    4.7/ Prevention from humidity or air

    In order to prevent adsorption of atmospheric water

    on the adsorbents, it is important not to open the

    drums before being ready to pour the product into the

    hopper.

    Several minutes of exposure during loading does not

    cause significant water pick up.

    During the night, manholes have to be hermeticallyclosed. If possible, it is recommended to flow dry air

    or nitrogen into the vessels.

    5/ LOADING OPERATION

    The following procedure is made of standard

    suggestions and advice that must be adapted to each

    case. The operation must always conform with site

    safety rules. We consequently ask you to read this

    procedure carefully, and to contact us if any questionarises.

     Loading 5/7

    Ceramic balls

    Grid and screens

    Ceramic balls

    Grid and screens

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    CECA Adsorbents Handling Procedures

    5.1/ Hopper / big bag lifting

    The hopper (or the big bag) filled with products is

    lifted by the crane up to the top level of the vessel;

    right above the manhole.

    Hopper and big bag lifting Here a second hopper with a long sleeve is already

    installed on the vessel manhole

    5.2/ Adsorbents loading

    The product is carefully released by slowly openingthe hopper valve (or the bottom of the big bag), and

    flows into the sleeve. The flow must be controlled

    (in order to prevent clogging of the sleeve) and

    directed (thanks to the rope, in order to well spread

    the products and avoid a too large slope).

    When the hopper is empty, it is brought back to the

    ground level for the next operation.

    It is highly recommended to prepare andcontinuously fill out “loading sheets” with the lot

    numbers, timing, product height (see § 5.4), etc.

    5.3/ Ceramic balls loading

    It is possible to load the bottom ceramic balls from

    the top, like the adsorbents. However, as they are

    bigger (typically up to 1/2 inch diameter) and denser,

    the flow must be very well controlled in order to

    avoid damaging the balls and the bottom mesh

    screens.

    When it is possible, bottom ceramic balls arepreferably loaded using a rope and buckets (or

    directly through the side manhole when there is one).

    It is necessary to first put the ceramic balls all aroundthe circumference of the vessel, in order to well

    maintain the mesh screens and ensure a good seal

    thanks to the 20 mesh screen overlap.

    Top ceramic balls can also be loaded with buckets.

    Ceramic balls lying on the mesh screen

    5.4/ Bed levelling

    Bed levelling is a crucial operation that needs to be

    performed regularly and neatly in order to have

    homogeneous layers of products.

    The number of levelling operations is a function of

    the number of loaded grades, height of the layers,

    vessel diameter, etc. As a minimum, it has to be done

    for each layer of products; but is usually alsoperformed at intermediate levels.

    The person in charge, who enters the vessel must

    wear all the required safety equipments (see § 1.6).

    He / She has to stand on wood boards and levels the

    bed using a rake or a rake-like tool.

    After the bed is considered flat and well levelled, the

    height between the top of the bed and the manhole is

    measured and compared to the forecasted one.

    5.5/ Top 20 mesh screen

    The 20 mesh screen with overlap is installed on top of

    the adsorbents (below the top ceramic balls, seeFigure 3). It is important not to tie this mesh screen

    with the vessel.

    If any internal such as a purge pipe (or a feed pipe or

    temperature probes) has to go through the 20 mesh

    screen, it is requested to make a hole of the samediameter in the screen, and to surround the internal

    with a cone-shaped piece of 20 mesh screen. This

    piece must be attached to the 20 mesh screen, but not

    to the internal. It is recommended to do this work

    once the screen is in the vessel.

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    CECA Adsorbents Handling Procedures

    Operators equipped for internal operation

    5.6/ Waiting for start-up 

    After the loading and before the start-up, the oxygen

    must be removed from the vessel, typically by a

    nitrogen purge. Often the available flow-rate of

    nitrogen is too low to provide the required turbulentflow. The vessel has to be pressurized and

    depressurized several times with nitrogen

    (preferably downstream in order not to lift the bed) –

    contact CECA if this is not feasible.

    If the unit is loaded and not to be put in service

    before several weeks or months, it is recommended

    to isolate the vessel from the rest of the process. This

    will prevent trace contaminants and moisture from

    being introduced into it. If the above procedures are

    followed, it is not be necessary to regenerate the

    beds prior to start-up. Here also a small nitrogen

    pressurization can help ensure no outside moisturewould come in.

    Do not hesitate to contact us for any question

    you may have :

    CECA S.A., Molecular Sieve Department

    Dynamic Applications

    Tel : +33 1 49 00 38 19

    Fax : +33 1 49 00 38 03Email : [email protected]

     

    The statements, technical information and recommendations contained herein are believed to be accurate as of the date hereof. Since

    the conditions and methods of use of the product and of the information referred to herein are beyond our control, ARKEMA expressly

    disclaims any and all liability as to any results obtained or arising from any use of the product or reliance on such information; NO

    WARRANTY OF FITNESS FOR ANY PARTICULAR PURPOSE, WARRANTY OF MERCHANTABILITY OR ANY OTHER WARRANTY, EXPRESS

    OR IMPLIED, IS MADE CONCERNING THE GOODS DESCRIBED OR THE INFORMATION PROVIDED HEREIN. The information provided

    herein relates only to the specific product designated and may not be applicable when such product is used in combination with other

    materials or in any process. The user should thoroughly test any application before commercialization. Nothing contained herein

    constitutes a license to practice under any patent and it should not be construed as an inducement to infringe any patent and the user is

    advised to take appropriate steps to be sure that any proposed use of the product will not result in patent infringement.

    See MSDS for Health & Safety Consideration

    CECA

    89, boulevard National

    92257 La Garenne-Colombes Cedex - France

    cecachemicals.com Loading 7/7

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    CECA Adsorbents Handling Procedures

    VESSEL UNLOADING INSTRUCTIONS

    1/ SAFETY

    Unloading adsorbents from a process vessel requires

    a good knowledge of the application and a thoroughunderstanding of the possible hazards. Most of the

    time, toxic and/or explosive substances are present

    in the vessel at the end of the process operation

    (including after the last regeneration). This can be

    the regeneration medium itself (fuel gas, etc.), heavy

    hydrocarbon deposit (coke), or toxic adsorbed

    molecules (H2S, etc.) in some applications, when the

    last regeneration is not complete or not

    homogeneous. In any case safety requires absolute

    caution.

    1.1/ Safety equipments and concerns

    Safety / PPE (Personal Protective Equipment) outfits

    and fittings have to be available and used accordingto the plant’s safety rules. Contact CECA in case

    you have any question or any doubt. Equipment

    typically includes :

    Helmet, gloves, security shoes, dust mask, harness,

    goggles, clothes with long sleeves, BreathingApparatus systems, portable oxygen detector.

    Before any entry in the vessel, the inside has to be

    checked with an appropriate device to be lower than

    20% of the Lower Explosive Limit (LEL).

    Grounding of all equipments is recommended,

    including trucks (for vacuum unloading). However,static sparks may still occur because of non-

    conducting containers or other materials.

    CECA adsorbents are silica gels, aluminas or

    alumino-silicates (zeolite-based molecular sieves),

    chemically similar to ordinary clays. As fresh

    materials they are chemically inert under normal

    handling conditions, exhibit no vapour pressure and

    have no flammable constituents. However, used

    adsorbents have been exposed to liquid or gaseous

    materials containing traces of other products, such as

    saturated and unsaturated hydrocarbons, coke or

    sulphur compounds. These products may be toxic,flammable or explosive. When exposed to air or rain,

    they may heat up or be released in the atmosphere.

    It may happen that during unloading, the adsorbents

    start to burn. In this case, all operation must be

    stopped immediately by trained and equipped fire-

    fighters.

    Note : This is the only case which allows to spray

    water on (non vessel flooded) unloaded adsorbents.

    Spraying water on dry adsorbents can release all the

    other adsorbed molecules, potentially toxic, that

    would remain in the material.

    Unloading 1/3

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    CECA Adsorbents Handling Procedures

    1.2/ Last Regeneration

    Before being unloaded, the adsorbents must be

    properly and completely regenerated in order to

    remove as much adsorbed compounds and depositsas possible. Use the same regeneration procedure asusual, unless you have clues or evidence that it is not

    reliable enough to desorb all impurities. In this case,

    or if the usual regeneration gas is not available,

    contact CECA.

    1.3/ Purge and deactivation

    After the last regeneration, adsorbent beds have to

    undergo a special treatment to remove the last traces

    of impurities still present. One of two treatments are

    usually implemented : nitrogen purge or water

    flooding. It is not always possible to choose betweenthe two as this is subject to constraints (nitrogen

    availability, type of insulation, etc.) Furthermore, it

    is important to understand that these 2 methods are

    not equivalent (they do not act the same way) :

    - Nitrogen purge removes the process fluid that is

    still in the vessel, but does not desorb the molecules

    still in the pores. It is a vessel purge only,

    preferentially used for the cleaner applications

    (natural gas drying, etc.) that do not involve too

    reactive or toxic substances.

    - Water flooding removes the process fluid but alsocompletely desorbs each and every adsorbed

    molecule (which are displaced by water molecules).

    This is an adsorbent deactivation process that is

    preferentially used in case of reactive / toxic streams

    involving hazardous adsorbates. In case of poor

    regeneration (too low flow-rate, channelling issues,

    etc.), some hazardous molecules (such as H2S and

    others) can stay in the adsorbents porosity. If the

    material is directly unloaded and then exposed to air

    and / or moisture, it can burn or be released, leading

    to dangerous situations.

    Nitrogen purge :

    This method is the most common, and is generallyfaster than water flooding as it is not required to dry

    the unit afterwards. Its main drawback is the use of

    large quantities of nitrogen, which is sent to the flare.

    After the last regeneration cooling step, totally

    isolate the vessel, and depressurize down toatmospheric pressure. Install blind flanges on every

    pipe, except to the flare and on a sample tap at the

    bottom of the vessel, which has to be connected to

    the nitrogen network. Start the purge by flowing

    nitrogen through the bed and direct the outlet to theflare. The nitrogen flow-rate must be sufficient to

    avoid channelling. Minimum flow-rate and durationof the purge can be estimated by your CECA

    representative. It must be maintained until the gas

    going to the flare reaches 20% of the Lower

    Explosive Limit (LEL). Measurement is usuallydone at a tap on the flare line, using an appropriateanalyser.

    If the nitrogen availability is too low to provide the

    requested flow-rate, the alternate solution is to

    perform this purge by successive pressurizations and

    depressurizations of the vessel. In that case the flareline is closed, and only the nitrogen valve is opened.

    Gas fills the vessel till the pressure stabilizes at

    network pressure. The valve is then closed and the

    flare line is opened, so that the vessel depressurises

    through it. Once the pressure is stabilized, the flare

    line is closed again and a new cycle starts. Usually 3to 5 pres. / depress. steps are required to obtain less

    than 20% LEL.

    Water flooding :

    Water flooding is used when nitrogen is not

    available, or when there is a risk that hazardous

    substances are still imprisoned in the adsorbents’

    porosity.

    Note : water flooding cannot be used in case of

    internal insulation (as it would damage the casting).

    Vacuum unloading can also be difficult to proceed,especially if a lot of fines is present.

    After the last regeneration cooling step, totally

    isolate the vessel, and depressurize down to

    atmospheric pressure. Install blind flanges on every

    pipe, except to the flare and on a sample tap at the

    bottom of the vessel, which has to be connected to

    the water network. Slowly fill the vessel with water.

    A fast temperature increase will be observed as the

    water comes into contact with the regenerated

    adsorbents. This is a normal non hazardous

    phenomenon which can be somehow controlled by

    the vessel filling rate. Fill the vessel until theadsorbents and the ceramic ball layers are totally

    flooded by water, but be careful not to overfill andflood the flare line (the water height can be

    estimated from a flow-meter and / or a differential

    pressure gauge). Plug a flexible pipe to the tap and

    send all the water to the waste water treatment

    station. In the vessel, adsorbents and ceramic balls

    are soaked, and ready for unloading.

    Note : For special cases involving hazardous

    substances, that cannot be water flooded, the

    regenerated adsorbents have to be unloaded into

    special metal containers with a bottom tap connectedto water and a top tap connected to a vent line and to

    Unloading 2/3

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    CECA Adsorbents Handling Procedures

    the flare. A water flooding process can therefore beimplemented outside of the vessel for each container. 

    2/ UNLOADING

    All internals must be removed from the adsorbent

    bed (temperature probes, sampling devices, etc.)

    After having performed the operations described at

    chapter 1.2/ and 1.3/, the vessel can be opened and

    the unloading can start.

    Top 1” ceramic balls and mesh screen must be first

    removed by the top manway (See chapter 1.1 for

    safety equipment). Sometimes 1” ceramic balls and

    mesh screen are not removed and go down in the

    vessel as adsorbents are unloaded by through sidemanway. In this case, a hook-type device should be

    used to retain the top screen prior to unloading the

    bed, in order to prevent it is pulled down and block

    the outlet.

    Used material can be removed either by pneumatic

    unloading (vacuum unloading), or by gravity

    unloading.

    Pneumatic unloading :

    If a pneumatic truck is chosen, the adsorbents must

    be dry. A flexible pipe is put into the vessels andsucks the products under vacuum. Most of the time

    it is necessary that one person remains in the vessel

    to direct the flexible pipe. Used adsorbents are then

    sent to a bin or to empty big bags. The used material

    is often broken and partially reduced to fines when

    going through the suction system.

    Grounding of the truck is required. This method is

    the fastest and the easiest one.

    Gravity unloading :

    If gravity unloading is chosen, the bottom side

    manway (or the dump port) is carefully opened to let

    the product flow. A special cone-shaped piece ofmetal or wood is put below the manway to direct theflow into the bin or big bags. The flow is controlled

    by adjusting the manway opening. The product flow

    is important at the beginning, and slowly decreases.

    After some time, no more material goes out of the

    vessel, and it is necessary to complete the unloading

    manually, using rakes.

    When all the used adsorbents are out of the vessel,

    the bottom ceramic balls are unloaded manually. If

    they are to be re- used, the different sizes can be

    separated by sieving.

    When the bottom ceramic balls are unloaded, check

    the bottom support grid and the mesh screens (or the

    V-wire screen) to make sure they can be reused or

    need to be repaired or changed.

    Before reloading of fresh adsorbents, carefully and

    thoroughly dry the vessels, piping and internals,

    (including the ceramic balls). Fresh material should

    avoid any contact with remaining moisture

    Do not hesitate to contact us for any question

    you may have :

    CECA S.A., Molecular Sieve Department

    Dynamic Applications

    Tel : +33 1 49 00 38 19

    Fax : +33 1 49 00 38 03

    Email : [email protected]

     

    The statements, technical information and recommendations contained herein are believed to be accurate as of the date hereof. Since

    the conditions and methods of use of the product and of the information referred to herein are beyond our control, ARKEMA expressly

    disclaims any and all liability as to any results obtained or arising from any use of the product or reliance on such information; NO

    WARRANTY OF FITNESS FOR ANY PARTICULAR PURPOSE, WARRANTY OF MERCHANTABILITY OR ANY OTHER WARRANTY, EXPRESS

    OR IMPLIED, IS MADE CONCERNING THE GOODS DESCRIBED OR THE INFORMATION PROVIDED HEREIN. The information provided

    herein relates only to the specific product designated and may not be applicable when such product is used in combination with other

    materials or in any process. The user should thoroughly test any application before commercialization. Nothing contained herein

    constitutes a license to practice under any patent and it should not be construed as an inducement to infringe any patent and the user

    is advised to take appropriate steps to be sure that any proposed use of the product will not result in patent infringement. See MSDS for

    Health & Safety Consideration

    CECA

    89, boulevard National

    92257 La Garenne-Colombes Cedex - France

    cecachemicals.comUnloading 3/3

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    CECA Adsorbents Handling Procedures

    DISPOSAL OF WASTE ADSORBENTS

    Before dumping used adsorbents, please consult thecorresponding MSDS. If you don’t have it, please

    ask your CECA representative to send you a copy.

    Unloaded adsorbents may retain toxic or flammable

    components. Do not directly flood adsorbents with

    water, and keep them in bin or big bags until they

    leave the plant.

    Depending on local environmental regulations,

    adsorbents may or may not be disposed in a

    controlled landfill. Landfill is the final destination of

    used adsorbents in most cases. Preliminary analysis

    of adsorbents are requested to determine the type ofappropriate landfill.

    If the adsorbents cannot be spread on an open field,

    it is then necessary to dead burn them in cement

    factory ovens, and to further use them as raw

    material for the cement industries. This is especially

    true for very large quantities of used material.

    Adsorbents residual hydrocarbon content shall be in

    any case less than 0.5% by weight.

    Please note that a large number of specialised

    companies propose to handle used adsorbents. These

    companies know local regulations and take care ofall required testing and administrative declarations.

    They are usually the same companies handling the

    other waste chemicals produced in the plant.

    Do not hesitate to contact us for any question

    you may have :

    CECA S.A., Molecular Sieve Department

    Dynamic ApplicationsTel : +33 1 49 00 38 19

    Fax : +33 1 49 00 38 03

    Email : [email protected]

    The statements, technical information and recommendations contained herein are believed to be accurate as of the date hereof. Since

    the conditions and methods of use of the product and of the information referred to herein are beyond our control, ARKEMA expressly

    disclaims any and all liability as to any results obtained or arising from any use of the product or reliance on such information; NO

    WARRANTY OF FITNESS FOR ANY PARTICULAR PURPOSE, WARRANTY OF MERCHANTABILITY OR ANY OTHER WARRANTY, EXPRESS

    OR IMPLIED, IS MADE CONCERNING THE GOODS DESCRIBED OR THE INFORMATION PROVIDED HEREIN. The information provided

    herein relates only to the specific product designated and may not be applicable when such product is used in combination with other

    materials or in any process. The user should thoroughly test any application before commercialization. Nothing contained herein

    constitutes a license to practice under any patent and it should not be construed as an inducement to infringe any patent and the user

    is advised to take appropriate steps to be sure that any proposed use of the product will not result in patent infringement. See MSDS for

    Health & Safety Consideration

    CECA

    89, boulevard National


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