Systems and methods for the synthesizing ZSM-22 zeolites

Patent metadata

Field	Value
Publication number	US-11618013-B2
Application number	US-202117206938-A
Country	US
Kind code	B2
Filing date	Mar 19, 2021
Priority date	Mar 19, 2021
Publication date	Apr 4, 2023
Grant date	Apr 4, 2023

Abstract

According to one or more embodiments, non-agglomerated, nano-sized ZSM-22 zeolites may be synthesized by methods comprising operating a mechanical rotation drum unit at a first temperature of from 40° C. to 60° C. and a first speed of from 200 rpm to 1000 rpm for a first time period of from 1.3 hours to 2.7 hours; operating the mechanical rotation drum unit at a second speed of from 30 rpm to 90 rpm for a second time period of from 0.05 hours to 0.4 hours; heating the mechanical rotation drum unit at a ramping temperature of from 8° C./minute to 12° C./minute to a second temperature of from 115° C. to 185° C. at the second speed; operating the mechanical rotation drum unit at the second temperature and the second speed for a third time period of from 30 hours to 90 hours; and cooling the mechanical rotation drum unit at a fourth speed of 0 rpm.

First claim

What is claimed is:

1. A method of synthesizing a non-agglomerated, nano-sized ZSM-22 zeolite, the method comprising:
passing a silica solution and an aluminate solution into a mechanical rotation drum unit;
operating the mechanical rotation drum unit at a first temperature of from 40° C. to 60° C. and a first speed of from 200 rpm to 1000 rpm for a first time period of from 1.3 hours to 2.7 hours;
operating the mechanical rotation drum unit at a second speed of from 30 rpm to 90 rpm for a second time period of from 0.05 hours to 0.4 hours;
heating the mechanical rotation drum unit at a ramping temperature of from 8° C./minute to 12° C./minute to a second temperature of from 115° C. to 185° C. at the second speed of from 30 rpm to 90 rpm;
operating the mechanical rotation drum unit at the second temperature of from 115° C. to 185° C. and the second speed of from 30 rpm to 90 rpm for a third time period of from 30 hours to 90 hours; and
cooling the mechanical rotation drum unit at a fourth speed of 0 rpm to produce the non-agglomerated, nano-sized ZSM-22 zeolite; and
wherein the non-agglomerated, nano-sized ZSM-22 zeolite comprises crystals each having a length within a range of from 100 nanometers to 400 nanometers and a width within a range of from 50 nanometers to 250 nanometers.

2. The method of claim 1 , wherein the mechanical rotation drum unit is cooled to a temperature of from 20° C. to 50° C.

3. The method of claim 1 , further comprising drying the non-agglomerated, nano-sized ZSM-22 zeolite.

4. The method of claim 1 , further comprising calcining the non-agglomerated, nano-sized ZSM-22 zeolite.

5. The method of claim 1 , further comprising activating the non-agglomerated, nano-sized ZSM-22 zeolite to produce an active catalyst.

6. The method of claim 1 , wherein the non-agglomerated, nano-sized ZSM-22 zeolite comprises crystals each having a length within a range of from 100 nanometers to 200 nanometers and a width within a range of from 50 nanometers to 100 nanometers.

7. The method of claim 1 , wherein the non-agglomerated, nano-sized ZSM-22 zeolite comprises crystals each having a length within a range of from 150 nanometers to 400 nanometers and a width within a range of from 100 nanometers to 250 nanometers.

8. The method of claim 1 , wherein the non-agglomerated, nano-sized ZSM-22 zeolite has a silica/alumina ratio of from 25 to 100.

9. A method of synthesizing a non-agglomerated, nano-sized ZSM-22 zeolite, the method comprising:
passing a silica solution and an aluminate solution into a mechanical rotation drum unit; and
operating the mechanical rotation drum unit at five stages to produce the non-agglomerated, nano-sized ZSM-22 zeolite;

wherein:
the first stage operates at a first mixing speed of from 200 rpm to 1000 rpm and at a first time period of from 1.3 hours to 2.7 hours;
the second stage operates at a second mixing speed of from 30 rpm to 90 rpm and at a second time period of from 0.05 hours to 0.4 hours;
the third stage operates at a third mixing speed of from 30 rpm to 90 rpm and at a third time period of from 0.05 hours to 0.4 hours;
the fourth stage operates at a fourth mixing speed of from 30 rpm to 90 rpm and at a first time period of from 30 hours to 90 hours; and
the fifth stage operates at a fifth mixing speed of 0 rpm.

10. The method of claim 9 , wherein the first stage operates at a temperature of from 40° C. to 60° C.

11. The method of claim 9 , wherein the second stage operates at a temperature of from 40° C. to 60° C.

12. The method of claim 9 , wherein the fourth stage operates at a temperature of from 115° C. to 185° C.

13. The method of claim 9 , wherein the fifth stage operates at a temperature of from 20° C. to 50° C.

14. The method of claim 9 , wherein the third stage operates a ramping temperature of from 8° C./minute to 12° C./minute.

15. The method of claim 9 , further comprising producing the silica solution in a silicate unit; producing the aluminate solution in an aluminate unit; and combining the silica solution and the aluminate solution prior to passing the silica solution and the aluminate solution into the mechanical rotation drum unit.

16. The method of claim 9 , further comprising activating the non-agglomerated, nano-sized ZSM-22 zeolite to produce an active catalyst.

17. The method of claim 9 , wherein the non-agglomerated, nano-sized ZSM-22 zeolite comprises crystals each having a length within a range of from 100 nanometers to 400 nanometers and a width within a range of from 50 nanometers to 250 nanometers.

18. The method of claim 17 , wherein the non-agglomerated, nano-sized ZSM-22 zeolite comprises crystals each having a length within a range of from 100 nanometers to 200 nanometers and a width within a range of from 50 nanometers to 100 nanometers.

19. The method of claim 17 , wherein the non-agglomerated, nano-sized ZSM-22 zeolite comprises crystals each having a length within a range of from 150 nanometers to 400 nanometers and a width within a range of from 100 nanometers to 250 nanometers.

20. The method of claim 9 , wherein the non-agglomerated, nano-sized ZSM-22 zeolite has a silica/alumina ratio of from 25 to 100.

Assignees

• Saudi Arabian Oil Co
• Univ King Fahd Pet & Minerals

Inventors

• Al-Shafei Emad
• Muraza Oki
• Jamil Anas Karrar
• Choi Ki-Hyouk
• Punetha Ashok K
• Yamani Zain Hassan

Classifications

• B01J35/45

  Nanoparticles · CPC title

• B01J35/40

  characterised by dimensions, e.g. grain size (in a colloidal state B01J35/23; crystallite size B01J35/77) · CPC title

• C10G2400/20

  C2-C4 olefins · CPC title

• B01J37/08

  Heat treatment {(B01J37/0009, B01J37/0018 take precedence)} · CPC title

• C01B39/48 Primary

  using at least one organic template directing agent · CPC title