IP Library › Granted Patent US 10,377,786
Granted Patent B2
US 10,377,786 · App. 15/319,505 · Granted Aug 13, 2019

Green methods for preparing highly CO2 selective and H2S tolerant metal organic frameworks

Inventors: Mohamed Eddaoudi (Thuwal, SA); Osama Shekhah (Thuwal, SA); Youssef Belmabkhout (Thuwal, SA)
Assignee: KING ABDULLAH UNIVERSITY OF SCIENCE AND TECHNOLOGY
C07F15/045B01J20/226B01J20/3078B01J20/3085B01J31/1691B01J37/009B01J37/04C07F7/025B01J2231/005B01J2531/16B01J2531/26B01J2531/847
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Quick Facts
Patent No.
US 10,377,786
App. No.
15/319,505
Granted
Aug 13, 2019
Kind
B2
Abstract

A green route for preparing a metal organic framework include mixing metal precursor with a ligand precursor to form a solvent-free mixture; adding droplets of water to the mixture; heating the mixture at a first temperature after adding the water; and isolating the metal organic framework material including the metal and the ligand.

Claims (29)

1. A method for preparing a metal organic framework comprising:

mixing a solid metal precursor with a solid ligand precursor to form a mixture of the solid precursors, wherein the solid metal precursor includes M-SiF 6 , wherein M includes a metal;

wetting the mixture of the solid precursors with one or more drops of water; and

heating the wetted mixture at a first temperature to obtain a two-dimensional metal organic framework intermediate structure.

2. The method of claim 1 , wherein the metal of the solid metal precursor is selected from a group consisting of Ni, Cu, Zn, Fe, and Co.

3. The method of claim 1 , wherein the metal includes Ni.

4. The method of claim 1 , wherein the solid ligand precursor includes pyrazine, 4,4′-Bipyridin, 1,4-Diazabicyclo[2.2.2]octane, or 1,2-bis(4-pyridyl)acetylene.

5. The method of claim 1 , wherein the solid ligand precursor includes a nitrogen-containing heterocyclic ligand.

6. The method of claim 1 , wherein the molar ratio of the solid ligand precursor to the metal precursor is about 3:1 to about 6:1.

7. The method of claim 1 , further comprising forming SIFSIX-Ni-3 metal organic framework.

8. The method of claim 1 , wherein the two-dimensional metal organic framework intermediate structure is H 2 S tolerant.

9. A method for preparing a metal organic framework comprising:

mixing a solid metal precursor with a solid ligand precursor to form a mixture of the solid precursors, wherein the solid metal precursor includes M-SiF 6 , wherein M includes a metal;

wetting the mixture of the solid precursors with one or more drops of water; and

heating the wetted mixture at a first temperature and thereafter further heating the wetted mixture to a second temperature to obtain a three-dimensional metal organic framework structure.

10. The method of claim 9 , wherein the metal of the solid metal precursor is selected from a group consisting of Ni, Cu, Zn, Fe, and Co.

11. The method of claim 9 , wherein the metal includes Ni.

12. The method of claim 9 , wherein the solid ligand precursor includes pyrazine, 4,4′-Bipyridin, 1,4-Diazabicyclo[2.2.2]octane, or 1,2-bis(4-pyridyl)acetylene.

13. The method of claim 9 , wherein the solid ligand precursor includes a nitrogen-containing heterocyclic ligand.

14. A method for preparing a metal organic framework comprising:

mixing a metal precursor with a ligand precursor to form a mixture, wherein the metal precursor includes NiSiF 6 and the ligand precursor includes pyrazine;

adding water to the mixture;

heating the mixture at a first temperature after the water is added to the mixture; and heating the mixture to a second temperature to obtain a three-dimensional metal organic framework structure.

15. The method of claim 9 , further comprising forming SIFSIX-Ni-3 metal organic framework.

16. The method of claim 9 , wherein the three-dimensional metal organic framework intermediate structure is H 2 S tolerant.

17. The method of claim 9 , wherein the first temperature is less than the second temperature.

18. The method of claim 14 , wherein the first temperature is less than the second temperature.

19. The method of claim 9 , wherein the solid metal precursor includes one or more of NiSiF 6 , CuSiF 6 , ZnSiF 6 , CoSiF 6 , and FeSiF 6 .

20. The method of claim 14 , wherein the solid metal precursor includes one or more of NiSiF 6 , CuSiF 6 , ZnSiF 6 , CoSiF 6 , and FeSiF 6 .

Assignments (1)
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jul 25, 2019
From: EDDAOUDI, MOHAMED; SHEKHAH, OSAMA; BELMABKHOUT, YOUSSEF
To: KING ABDULLAH UNIVERSITY OF SCIENCE AND TECHNOLOGY
Reel/Frame 049862/0248 →
Continuity (2)
Provisional Application 62012982 · Jun 17, 2014
Related Publication 20170137450A1 · May 18, 2017