Laboratory process for deactivation of a porous solid

Patent metadata

Field	Value
Publication number	US-10626332-B2
Application number	US-201615754080-A
Country	US
Kind code	B2
Filing date	Aug 18, 2016
Priority date	Aug 21, 2015
Publication date	Apr 21, 2020
Grant date	Apr 21, 2020

Abstract

A process for the laboratory deactivation of a porous solid comprising subjecting the porous solid to a cyclic treatment, the treatment being selected from a hydration/dehydration cyclic treatment, a thermal cyclic treatment, or combinations thereof.

First claim

We claim:

1. A process for the laboratory deactivation of a porous solid comprising subjecting the porous solid to a cyclic treatment, the treatment being selected from a hydration/dehydration cyclic treatment, a thermal cyclic treatment, or combinations thereof, the hydration/dehydration cyclic treatment comprising at least five cycles of:
contacting in a hydration step the porous solid with a hydrating gas stream selected from nitrogen, air, noble gases, water vapor, or mixtures thereof, at a relative humidity of 20 to 100% and a temperature of 50° F. to 400° F., thereby forming a hydrated solid; and
contacting in a dehydration step the hydrated solid with a dehydrating gas stream comprising water at a relative humidity of less than 20%, and a temperature of from 200° F. to 1600° F., thereby forming a dehydrated solid, wherein for each cycle, except the first cycle, the dehydrated solid is the porous solid for the hydration step in the next cycle; and

the thermal cyclic treatment comprising at least five cycles of:
heating the porous solid to a heated temperature of 900° F. to 1575° F., thereby forming a heated porous solid; and
cooling the heated porous solid to a cooled temperature, thereby forming a cooled porous solid, wherein the difference between the heated temperature and the cooled temperature is at least 200° F., and where for each cycle, except the first cycle, the cooled porous solid is the porous solid for the heating step in the next cycle.

2. The process of claim 1 wherein the temperature of the hydration step is from 60 to 230° F.

3. The process of claim 2 wherein the temperature of the hydration step is from 100 to 225° F.

4. The process of claim 1 wherein the temperature of the dehydration step is from 500 to 1575° F.

5. The process of claim 4 wherein the temperature of the dehydration step is from 800 to 1550° F.

6. The process of claim 5 wherein the temperature of the dehydration step is from 950 to 1500° F.

7. The process of claim 1 wherein the dehydrating gas stream is selected from nitrogen, air, noble gases, or mixtures thereof.

8. The process of claim 1 wherein water is present in the hydrating gas stream at a relative humidity of 35 to 90%.

9. The process of claim 1 wherein the concentration of water in the dehydrating gas stream is from 0 to 10%.

10. The process of claim 1 wherein the porous solid is treated in at least 10 hydration-dehydration cycles.

11. The process of claim 10 wherein the porous solid is treated in at least 20 hydration-dehydration cycles.

12. The process of claim 11 wherein the porous solid is treated in at least 30 hydration-dehydration cycles.

13. The process of claim 1 wherein the pressure of the hydrating gas stream is from 14.1 psia to 150 psig.

14. The process of claim 1 wherein the pressure of the dehydrating gas stream is from 14.1 psia to 150 psig.

15. The process of claim 1 wherein the difference between the heated temperature and the cooled temperature is at least 450° F.

16. The process of claim 15 wherein the difference between the heated temperature and the cooled temperature is at least 500° F.

17. The process of claim 1 wherein the heated temperature is 950° F. to 1560° F.

18. The process of claim 17 wherein the heated temperature is 975° F. to 1555° F.

19. The process of claim 18 wherein the heated temperature is 1100° F. to 1550° F.

20. The process of claim 19 wherein the heated temperature is 1250° F. to 1525° F.

21. The process of claim 1 wherein the cooled temperature is 40° F. to 975° F.

22. The process of claim 21 wherein the cooled temperature is 60° F. to 960° F.

23. The process of claim 22 wherein the cooled temperature is 75° F. to 950° F.

24. The process of claim 1 wherein the porous solid is heated with a heating gas.

25. The process of claim 1 wherein the porous solid is cooled with a cooling gas.

26. The process of claim 25 wherein the heating gas is selected from nitrogen, air, noble gases, water vapor, or mixtures thereof.

27. The process of claim 26 wherein the cooling gas is selected from nitrogen, air, noble gases, water vapor, or mixtures thereof.

28. The process of claim 1 wherein the porous solid is a fluid cracking catalyst.

29. The process of claim 28 wherein the fluid cracking catalyst has a fresh zeolite surface area and a fresh matrix surface area.

30. The process of claim 29 wherein the fresh zeolite surface area is from 20 to 500 m 2 /g.

31. The process of claim 30 wherein the fresh matrix surface area is from 10 to 200 m 2 /g.

32. The process of claim 31 wherein the fluid cracking catalyst comprises metals selected from nickel, vanadium, iron, sodium or mixtures thereof.

33. The process of claim 32 wherein the level of nickel on the fluid cracking catalyst is from 0 to 20,000 ppm based on the weight of the fluid cracking catalyst.

34. The process of claim 32 wherein the level of vanadium on the fluid cracking catalyst is from 0 to 10,000 ppm based on the weight of the fluid cracking catalyst.

35. A process comprising:
treating a porous solid in a hydrothermal steaming process, thereby forming a deactivated porous solid;
subjecting the deactivated porous solid to a cyclic treatment, the cyclic treatment being selected from a hydration/dehydration cyclic treatment, a thermal cyclic treatment, or combinations thereof, the hydration/dehydration cyclic treatment comprising at least five cycles of:
contacting in a hydration step the deactivated porous solid with a hydrating gas stream selected from nitrogen, air, noble gases, water vapor, or mixtures thereof, at a relative humidity of 20 to 100% and a temperature of 50° F. to 400° F., thereby forming a hydrated solid; and
contacting in a dehydration step the hydrated solid with a dehydrating gas stream comprising water at a relative humidity of less than 20%, and a temperature of from 200° F. to 1600° F., thereby forming a dehydrated solid, wherein for each cycle, except the first cycle, the dehydrated solid is the deactivated porous solid for the hydration step in the next cycle;

the thermal cyclic treatment comprising at least five cycles of:
heating the deactivated porous solid to a heated temperature of 900° F. to 1575° F., thereby forming a heated porous solid; and
cooling the heated porous solid to a cooled temperature, thereby forming a cooled porous solid,
wherein the difference between the heated temperature and the cooled temperature is at least 200° F., and where for each cycle, except the first cycle, the cooled porous solid is the deactivated porous solid for the heating step in the next cycle.

36. A process for the laboratory deactivation of a porous solid comprising subjecting the porous solid to a cyclic treatment, the cyclic treatment being selected from a hydration/dehydration cyclic treatment, a thermal cyclic treatment, or combinations thereof, thereby forming a deactivated porous solid,
the hydration/dehydration cyclic treatment comprising at least five cycles of:
contacting in a hydration step the porous solid with a hydrating gas stream comprising water at a relative humidity of 20 to 100% and a temperature of 50° F. toy 400° F., thereby forming a hydrated solid; and
contactin

Assignees

• Grace W R & Co

Inventors

• Hu Ruizhong
• Weatherbee Gordon Dean
• Orlicki Dariusz
• Berg Michael

Classifications

• B01J29/084

  Y-type faujasite · CPC title

• G01N31/10

  using catalysis · CPC title

• B01J29/90

  Regeneration or reactivation · CPC title

• C10G11/18 Primary

  according to the "fluidised-bed" technique · CPC title

• B01J2229/42

  Addition of matrix or binder particles · CPC title