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GBH Enterprises, Ltd.

Key Operational Guidelines
During

Low Temperature Shift Catalyst
Reduction

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, damage or personnel injury
caused or resulting from reliance on this information. Freedom under Patent,
Copyright and Designs cannot be assumed.
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
KEY OPERATIONAL GUIDELINES:

LTS REDUCTION

1.

Make sure that sample taps are in the active flow region of the piping
connected to the LTS nozzles or at least within a maximum of two nozzle
diameters of the point at which the carrier/hydrogen stream enters or
leaves the main LTS piping.

2.

PREVENTION is the key word. Anticipate how you would expect the
reduction to proceed by knowing as much as possible about the system
you're working on. If something doesn't quite add up according to your
measurements and calculations, try and find reasons for it. Always be a
step ahead in your mind.

3.

Mapping out the reduction and having the expected events firmly in your
mind ahead of time will allow you to respond quickly and appropriately in a
tight situation or when you're very weary. Doing all your figuring and
calculating while you're still fresh and making notes will help prevent errors
at a later time.

4.

A thermocouple that isn't at least 10% deep in the catalyst bed probably
won't give a representative indication of the total temperature rise you'll
observe at points deeper in the bed.

5.

The rate of temperature rise in the bed should not exceed about 1oF/min.
in a reduction that is progressing at a moderate rate.

6.

Temperature is what can ruin LTS catalyst. Luckily, thermocouples are
probably the most accurate indicators in the plant. Rely on Ti's before
relying on flow meters, pressure gauges or gas analyses and instinctively
do whatever is necessary to control temperatures.

7.

ALWAYS go outside and walk the entire system from end to end to locate
pertinent valves, Ti's, sample taps, exchangers, heaters, KO pots, etc., no
matter how big a hurry the operators are in to get the reduction underway
and no matter what the weather is like outside. Ask questions about
where various things are and how they work if you don't find them on your
own.

8.

If at all possible, calibrate the hydrogen flowmeter or control valve before
the catalyst is at reaction temperature. It can still be done when the
catalyst is at reaction temperature, but it has to be done VERY quickly and
carefully then.

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
9.

The completion of the reduction is a matter of hydrogen partial pressure,
so either increase the H2 concentration or the vessel back-pressure to
finish it off.

10.

When thermocouples are all in a sheath and all/some seem to flatten out
around 220-250oF, look for steam coming from the flange at the top of the
sheath as entrapped water boils inside the sheath. Have the flange
loosened to allow the entrapped water to boil off more quickly.

11.

Don't assume that sketches of Ti placement provided by the customer are
accurately depicted. Ask for the thermocouple measurements, bed
dimensions and catalyst loading and confirm the Ti placement.

12.

If temperature indication is viewed on a computer screen and the temps
shown are generated/processed by a "card" or "board" internal to the
process control system, make sure that those cards or boards have not
been replaced during the turn-around leading to this reduction. Such
devices can apparently transmit either pressures when built-in resistors
are in place or temperatures with the resistors removed. When the
resistors are in place, reported "temperatures" will be much lower than
actual.

13.

Record temperatures at least every 10-15 minutes after starting the H2
and at least until the top half bed temps have turned over.

14.

Always be personally involved in the calibration of the H2 control valve and
flowmeter.

15.

If the H2 control valve is in a "high traffic" area where it can easily be
bumped by passers-by, then have the area cordoned off, have a shield of
some sort placed over the valve handle or have an operator put a wrench
on it and rotate it out of the way. Check it frequently yourself.

16.

In a recirculating system (closed loop), make sure that the top third of the
bed is at the catalyst's strike temp before starting the reduction. Also,
confirm that consumption is complete. Otherwise, the H2 will come back
around the loop, thereby raising the inlet concentration.

17.

Monitor H2 trailer total pressure regularly in order to anticipate exactly
when a new trailer will have to be put in service. Try and make the switch
without interrupting H2 flow, if possible.

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
18.

Know ahead of time what you should do in various plant upset situations,
e.g., loss of carrier, H2, power, instrument air, etc., so that you will respond
appropriately should the situation arise.

19.

Fluctuation of H2 supply pressure will change H2 flow rate with no change
in control valve position. Keep track of the supply pressure.

20.

Arrive on site well ahead of time to set up the portable GC and familiarize
yourself with the system.

21.

PREVENTION!! Concentrate fully on the reduction in the early stages to
see what is happening and to avert trouble. Once the process is well
underway and in control, you'll have more time to socialize with the plant
personnel.

22.

Once the operators have done their bit to get and keep things under
control, buy them pizzas.

23.

Don't ever be afraid to delay or stop a reduction if there is something you
think may be wrong or going wrong in the system. Explain your reasoning
to the contact people and try and get the answers, changes or assurances
you need to proceed. Call the home office for support and help.

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
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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Key Operational Guidelines - Low Temperature Shift Catalyst Reduction

  • 1. GBH Enterprises, Ltd. Key Operational Guidelines During Low Temperature Shift Catalyst Reduction 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, damage or personnel injury caused or resulting from reliance on this information. Freedom under Patent, Copyright and Designs cannot be assumed. 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
  • 2. KEY OPERATIONAL GUIDELINES: LTS REDUCTION 1. Make sure that sample taps are in the active flow region of the piping connected to the LTS nozzles or at least within a maximum of two nozzle diameters of the point at which the carrier/hydrogen stream enters or leaves the main LTS piping. 2. PREVENTION is the key word. Anticipate how you would expect the reduction to proceed by knowing as much as possible about the system you're working on. If something doesn't quite add up according to your measurements and calculations, try and find reasons for it. Always be a step ahead in your mind. 3. Mapping out the reduction and having the expected events firmly in your mind ahead of time will allow you to respond quickly and appropriately in a tight situation or when you're very weary. Doing all your figuring and calculating while you're still fresh and making notes will help prevent errors at a later time. 4. A thermocouple that isn't at least 10% deep in the catalyst bed probably won't give a representative indication of the total temperature rise you'll observe at points deeper in the bed. 5. The rate of temperature rise in the bed should not exceed about 1oF/min. in a reduction that is progressing at a moderate rate. 6. Temperature is what can ruin LTS catalyst. Luckily, thermocouples are probably the most accurate indicators in the plant. Rely on Ti's before relying on flow meters, pressure gauges or gas analyses and instinctively do whatever is necessary to control temperatures. 7. ALWAYS go outside and walk the entire system from end to end to locate pertinent valves, Ti's, sample taps, exchangers, heaters, KO pots, etc., no matter how big a hurry the operators are in to get the reduction underway and no matter what the weather is like outside. Ask questions about where various things are and how they work if you don't find them on your own. 8. If at all possible, calibrate the hydrogen flowmeter or control valve before the catalyst is at reaction temperature. It can still be done when the catalyst is at reaction temperature, but it has to be done VERY quickly and carefully then. 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
  • 3. 9. The completion of the reduction is a matter of hydrogen partial pressure, so either increase the H2 concentration or the vessel back-pressure to finish it off. 10. When thermocouples are all in a sheath and all/some seem to flatten out around 220-250oF, look for steam coming from the flange at the top of the sheath as entrapped water boils inside the sheath. Have the flange loosened to allow the entrapped water to boil off more quickly. 11. Don't assume that sketches of Ti placement provided by the customer are accurately depicted. Ask for the thermocouple measurements, bed dimensions and catalyst loading and confirm the Ti placement. 12. If temperature indication is viewed on a computer screen and the temps shown are generated/processed by a "card" or "board" internal to the process control system, make sure that those cards or boards have not been replaced during the turn-around leading to this reduction. Such devices can apparently transmit either pressures when built-in resistors are in place or temperatures with the resistors removed. When the resistors are in place, reported "temperatures" will be much lower than actual. 13. Record temperatures at least every 10-15 minutes after starting the H2 and at least until the top half bed temps have turned over. 14. Always be personally involved in the calibration of the H2 control valve and flowmeter. 15. If the H2 control valve is in a "high traffic" area where it can easily be bumped by passers-by, then have the area cordoned off, have a shield of some sort placed over the valve handle or have an operator put a wrench on it and rotate it out of the way. Check it frequently yourself. 16. In a recirculating system (closed loop), make sure that the top third of the bed is at the catalyst's strike temp before starting the reduction. Also, confirm that consumption is complete. Otherwise, the H2 will come back around the loop, thereby raising the inlet concentration. 17. Monitor H2 trailer total pressure regularly in order to anticipate exactly when a new trailer will have to be put in service. Try and make the switch without interrupting H2 flow, if possible. 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. 18. Know ahead of time what you should do in various plant upset situations, e.g., loss of carrier, H2, power, instrument air, etc., so that you will respond appropriately should the situation arise. 19. Fluctuation of H2 supply pressure will change H2 flow rate with no change in control valve position. Keep track of the supply pressure. 20. Arrive on site well ahead of time to set up the portable GC and familiarize yourself with the system. 21. PREVENTION!! Concentrate fully on the reduction in the early stages to see what is happening and to avert trouble. Once the process is well underway and in control, you'll have more time to socialize with the plant personnel. 22. Once the operators have done their bit to get and keep things under control, buy them pizzas. 23. Don't ever be afraid to delay or stop a reduction if there is something you think may be wrong or going wrong in the system. Explain your reasoning to the contact people and try and get the answers, changes or assurances you need to proceed. Call the home office for support and help. 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
  • 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