Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutd...
Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutd...
Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutd...
Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutd...
Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutd...
Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutd...
Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutd...
Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutd...
Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutd...
Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutd...
Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutd...
Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutd...
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Operating Manual - Mole Sieve Adsorbents

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LOADING AND START-UP: ADSORBENTS AND ADSORPTION UNITS
PHILOSOPHY
PACKAGING AND INSPECTION
LOADING
1.1 Vessel Inspection
1.2 Loading of Bottom Support Material
1.3 Loading of Sieve
1.4 Special Precautions in the Case of PSA and VPSA Applications
1.5 Loading of Top Support Material
1.6 The vessel should then be closed in ready for process start-up.

2. START-UP
2.1 Check list before Commencing Start-up

3. INITIAL REGENERATION
3.1 Regeneration Gas Availability
3.2 Initial Regeneration Procedure

4. PROCESS START-UP


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Operating Manual - Mole Sieve Adsorbents

  1. 1. Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com GBH Enterprises, Ltd. Operating Manual Molecular Sieve Adsorbents Information contained in this publication or as otherwise supplied to Users is believed to be accurate and correct at time of going to press, and is given in good faith, but it is for the User to satisfy itself of the suitability of the information for its own particular purpose. GBHE gives no warranty as to the fitness of this information for any particular purpose and any implied warranty or condition (statutory or otherwise) is excluded except to the extent that exclusion is prevented by law. GBHE accepts no liability resulting from reliance on this information. Freedom under Patent, Copyright and Designs cannot be assumed.
  2. 2. Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com GBH Enterprises molecular sieves are manufactured by CAMChem, which is ISO 9001 System certified. Features & Applications CAMChem Crown Advanced Material Co. , Ltd Xiabu Industrial Park, Xiangdong District, Pingxiang, Jiangxi, China
  3. 3. Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com LOADING AND START-UP ADSORBENTS AND ADSORPTION UNITS – Note that before handling the molecular sieve for loading or other purposes, personnel should read and be conversant with the safety instructions. – A copy of these instructions is available on request. Remember that molecular sieves evolve much heat on contact with water. PHILOSOPHY Molecular sieves are desiccants which scavenge water and other small polar molecules down to very low concentrations, typically down to 1 ppm or less. The molecular sieve is loaded into the vessel in the open air, and in doing so may pick up inside the vessel or associated pipework. GBH Enterprises therefore recommend a regeneration of the complete unit after the unit has been closed-up for the last time and before bringing it on-stream. This regeneration should also be carried out when the unit has been off line for maintenance for an extended period of time. In thermal swing applications, regeneration ensures that the molecular sieve is in a highly active state when the unit is brought on stream. It involves heating the molecular sieve to above 250°C (or to 230°C for 3A molecular sieve) in a heated gas stream, which is passed through the column at the required mass flow rate. The gas provides both heat and a medium for sweeping away desorbed species from the molecular sieve. PACKAGING AND INSPECTION GBH ENTERPRISES molecular sieves are delivered in a variety of packaging, ranging from 25 kg cartons through 140 kg drums to Big Bags with 600 kg to 1000 kg of product. All these packages contain an inner polyethylene liner which protects the contents from atmospheric contaminants and moisture. However the product is a desiccant, and should be stored on site in clean, dry conditions.
  4. 4. Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com GBH ENTERPRISES molecular sieves are extensively tested before despatch. Certification and quality control to ISO 9001standards is provided and guarantees the quality of the product as delivered. Even so, a visual inspection of the product is recommended before loading into the vessels. – In the case of the Big Bags, it is simply a question of undoing the outer and inner liners on the top of the Big Bag. After inspection, which should be done under cover, it is important that the inner plastic liner should be tied tightly to the outside bag rope to prevent the liner from falling out during loading. – With steel drums, it is possible that a vacuum may have developed inside the drum. To break the vacuum remove the top rim closure and either release the vent on the top of the drum, or use a screwdriver to pries the lid up and release the vacuum. Then remove the lid and loosen the inner tie to inspect the molecular sieve. Re-seal after inspection. The total delivered quantity should be checked by grade and bead size, and against the expected total volume of the vessels to be loaded. Should the molecular sieve appear to be damaged in any way, then please notify GBH Enterprises for further instruction and assistance. LOADING Normally one of two loading configurations are to be used. The bed will either be made up completely of beads of a single size range; or there will be a two layer configuration where the bed is made up of approximately 2/3 large beads, and 1/3 small beads. If the bed has a two layer configuration, then the smaller beads always go at the adsorption outlet end of the column. With gas phase adsorbers the adsorption outlet is normally the bottom. With liquid phase adsorbers the adsorption outlet is normally the top. However this is NOT always the case, and drawings or specifications should be checked before loading. For further points and recommendations on support balls, please consult our brochure VULCAN Series A2 ST Advanced Alumina Support Technology 'Adsorbent Bed Supports' copy available on request.
  5. 5. Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com 1.1 Vessel Inspection Before loading the molecular sieve it is recommended that the inside of the vessel is also inspected, particularly during a re-charge of an existing vessel. The following checks can prevent major problems from occurring during operation. – Ensure the support grid is properly secured in the bottom of the vessel. – Inspect the caulking between the screen and the vessel wall. – Make certain that the screen above the support grid is free of embedded molecular sieve particles, support material and dust. – Note the condition of sample taps, thermal wells etc. – If possible check the calibration of the plant hygrometer probe. – If the vessel is internally insulated, check the surface for defects. 1.2 Loading of Bottom Support Material It is normal practice to load a 15 cm / 6 inch layer of inert balls at the bottom of the adsorber to prevent blinding of the bottom screen, and to prevent molecular sieve from passing through this screen. This may be done by loading through a manway in the lower section of the tower. NOTE: The ceramic balls should not be allowed to free-fall from the top of the tower as they can shatter when they hit the bottom screen. This may damage the screen, and may also cause an excessive pressure drop during operation. Molecular sieve should not be allowed to free-fall more than about 10 meters.
  6. 6. Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com 1.3 Loading of Sieve There are two basic methods of loading molecular sieve depending on the packaging in which they are supplied. – If the molecular sieve is delivered in drums, the material may be loaded by hoisting individual drums to the top of the tower and tipping them in. Alternatively a number of drums may be loaded into a hopper, which is then lifted to the top of the tower and discharged at one go. – If the molecular sieve is delivered in Big Bags, then individual Big Bags may be hoisted to the top of the tower. The bottom of the sack is then slit and the molecular sieve allowed to fall into a loading funnel and into the vessel. NOTE 1: Remember that the inner bag is not fixed to the outer bag, and it is possible for the weight of the molecular sieve to pull the inner liner into the tower if it is not secured as above. If this happens, it is essential that the plastic bag is recovered from inside the tower. NOTE 2: It is possible for the very dry adsorbent to build up a high static electricity loading. Therefore in flameproof areas earthing of the bags is essential. After all the molecular sieve has been loaded into the vessel, the surface should be leveled, and a floating screen of approximately 20 mesh stainless steel placed above the adsorbent. This is extremely important if ceramic balls are to be placed above the adsorbent as the ceramic balls are heavier than the molecular sieve, and will fall into the adsorbent bed if not separated. Note that the bed will settle during service, so the screen should not be fixed. 1.4 Special Precautions in the Case of PSA and VPSA Applications In some PSA applications the performance of the molecular sieve is particularly sensitive to moisture content of the molecular sieve. In such cases protective measures should be taken from environmental contamination, and it may be found desirable to flush the column to be loaded with dry air.
  7. 7. Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com It is vital that the molecular sieve is protected from contamination from either pick-up of moisture from the atmosphere, or from other local airborne contaminants. The drums should be kept tightly closed until immediately before loading. After completion of the loading steps which should be done as fast as possible, the column must be closed in and if necessary flushed with an inert dry suitable gas. If in any doubt as to the suitability of a particular gas then specialist opinion should be sought from GBH Enterprises. 1.5 Loading of Top Support Material Generally a 15 cm / 6 inch layer of support balls is loaded on top of the molecular sieve bed. This serves to hold the bed down during upflow operation, and to prevent destructive impingement of the gas stream on the molecular sieve during down-flow operation. The layer also acts as a distributor of gas through the molecular sieve. Loading of this layer should be done by using small buckets, or by hoisting individual drums to the top of the tower. The balls should be leveled over the surface area of the screen. 1.6 The vessel should then be closed in ready for process start-up. 2. START-UP 2.1 Check list before Commencing Start-up Before commencing Start-up the following plant items must be commissioned and ready for service: – the vessels and pipework clean, pressure tested and closed up ready for service; – all moving or rotating plant items checked and commissioned; – the plant checked to ensure all blanks and foreign matter including aids for construction have been removed; – pipework and vessels are connected according to the process drawings; – the various process streams are available for use; – the instrumentation and any automatic sequencers have been commissioned (especially any moisture indicators); – the utilities required for regeneration have been commissioned; – the vessels and pipework have been lagged as required.
  8. 8. Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com Molecular sieve can adsorb moisture down to very low levels (typically less than 1 ppm). They also evolve a large amount of heat on contact with water. Apart from safety considerations, this heat can permanently damage the molecular sieve. It is important to ensure that there is no possibility of any large volume of liquid water coming into contact with the molecular sieve beds. Also during their first exposure to some types of hydrocarbons some grades of molecular sieve may also adsorb enough of these hydrocarbons to give a temperature increase of up to 20°C or more. 3. INITIAL REGENERATION 3.1 Regeneration Gas Availability GBH Enterprises recommend that the initial regeneration is carried out with the gas stream to be used in standard plant running. However if this is not available then a dry nitrogen stream or a dry methane rich stream (without unsaturated hydrocarbons) may be used instead. Note: – Dry nitrogen is the preferred gas and may already be connected if the vessels have to be purged of air during commissioning. – The flow rate may need to be adjusted to allow for any difference in specific heat from the design stream, but the full designed gas flow rate should be used to ensure that there is no channelling of the gas flow through the bed. – Regeneration under plant conditions is generally carried out at a pressure of 25 / 30 bar or less. If a gas is used at a pressure lower than design, care should be taken that the pressure drop does not become too high leading to fluidization of the bed, which may then need repacking, or it can blow the molecular sieve out of the vessel. 3.2 Initial Regeneration Procedure a) Turn on the regeneration gas flow and adjust to the required mass flow rate. Care should be taken to ensure this stream is disposed of safely, particularly if the next unit up-stream is not yet commissioned and the regeneration gas stream is vented or flared off.
  9. 9. Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com b) Start up the heating for the gas stream, bringing the temperature up to specification over a period of say one hour or in accordance with the suppliers instructions (Maximum three hours). If refractory has to be dried out, or other commissioning work on other plant items, then this should have been done beforehand (but see note below on effects of temperature on the molecular sieve). c) Maintain heating until the outlet to the bed reaches a constant temperature within 20-30°C of the inlet. This outlet temperature should be monitored and verified during initial start-up. Further the exit gas stream should also be checked for water content during initial start-up. (Typical heating time about 5 hours) d) Maintain this constant temperature for a period of one hour. Note that molecular sieve can be degraded by an excessively high temperature. If heater trials are being undertaken during pre-service regeneration, care should be taken to protect the molecular sieve from excessive temperatures. A maximum safe temperature is 325°C. e) Stop heating. f) Cool the column down by blowing through DRY cool gas in accordance with standard plant instructions, until the temperature at the column outlet reaches a temperature 40-50°C above ambient. (Typical cooling time about 3 hours). g) Shut in the column ready for start-up on process gas. h) Repeat the above instructions on each of the columns in turn.
  10. 10. Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com 4. PROCESS START-UP 4.1 It is assumed that the molecular sieve has already been regenerated according to the instructions above. 4.2 The plant will typically be started off at low flow rates and gradually brought up to design conditions. GBH Enterprises therefore recommend that the adsorber is placed on a fixed cycle time during this commissioning phase, unless the switch-over to regeneration is done by means of a moisture indicator. In this case change-over should be monitored and verified during the first few cycles. Regeneration can be done in accordance with the plant manual from the start, provided gas is available. If not then the regeneration heat time should be extended until the specified heating maximum outlet temperature is reached. 4.3 At very low flow rates there is a danger of channelling of flow through the packed beds. In this case an automatic sensor may not see moisture which is being channeled away in another part of the bed. 4.4 The regeneration should be done with full flow design rates from the start. This is essential as it reconditions the desiccant for further use in the next adsorption cycle. 4.5 Automated plant running can be switched in once the flow reaches 50% design or the minimum turndown flow according to the plant operating manual. 4.6 Outlet streams should be monitored regularly to ensure the required moisture content is reached. 4.7 Inlet streams should also be monitored regularly to ensure there is no excessive moisture, oils, dusts or other contaminants reaching the active molecular sieve surface. 4.8 Automated operation should be switched in when the conditions in step 6.6 are regularly achieved.
  11. 11. Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com Process Information Disclaimer Information contained in this publication or as otherwise supplied to Users is believed to be accurate and correct at time of going to press, and is given in good faith, but it is for the User to satisfy itself of the suitability of the Product for its own particular purpose. GBHE gives no warranty as to the fitness of the Product for any particular purpose and any implied warranty or condition (statutory or otherwise) is excluded except to the extent that exclusion is prevented by law. GBHE accepts no liability for loss or damage resulting from reliance on this information. Freedom under Patent, Copyright and Designs cannot be assumed. For further Information on “Non-Proprietary” Vulcan Series Process catalyst absorbents & adsorbents, or recommendations for specific applications, please contact us.
  12. 12. Refinery Process Stream Purification Refinery Process Catalysts Troubleshooting Refinery Process Catalyst Start-Up / Shutdown Activation Reduction In-situ Ex-situ Sulfiding Specializing in Refinery Process Catalyst Performance Evaluation Heat & Mass Balance Analysis Catalyst Remaining Life Determination Catalyst Deactivation Assessment Catalyst Performance Characterization Refining & Gas Processing & Petrochemical Industries Catalysts / Process Technology - Hydrogen Catalysts / Process Technology – Ammonia Catalyst Process Technology - Methanol Catalysts / process Technology – Petrochemicals Specializing in the Development & Commercialization of New Technology in the Refining & Petrochemical Industries Web Site: www.GBHEnterprises.com

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