Solvent-supported compaction of metal-organic frameworks

Patent metadata

Field	Value
Publication number	US-9757710-B1
Application number	US-201615241467-A
Country	US
Kind code	B1
Filing date	Aug 19, 2016
Priority date	Aug 19, 2016
Publication date	Sep 12, 2017
Grant date	Sep 12, 2017

Abstract

Methods of forming a high surface area compacted MOF powder are disclosed, as well as MOF pellets formed thereby. The method may include synthesizing a metal organic framework (MOF) powder using a first solvent, exchanging the first solvent with a second solvent such that pores of the MOF powder are at least 10% filled with the second solvent, compacting the MOF powder having pores at least 10% filled with the second solvent into a pellet, and desolvating the compacted pellet to remove the second solvent. The pellet may maintain a specific surface area after compacting that is at least 80% its initial specific surface area. Compacting the MOF powder with a solvent at least partially filling its pores may prevent or reduce crushing of the MOF pore structure and maintain surface area, for example, for hydrogen or natural gas storage.

First claim

What is claimed is:

1. A method, comprising:
synthesizing a metal organic framework (MOF) powder using a first solvent;
exchanging the first solvent with a second solvent such that pores of the MOF powder are at least 10% filled with the second solvent;
compacting the MOF powder having pores at least 10% filled with the second solvent into a pellet; and
desolvating the compacted pellet to remove the second solvent.

2. The method of claim 1 , wherein the MOF powder is compacted to a density of at least 60% of a theoretical density of the MOF crystal structure to form the pellet.

3. The method of claim 2 , wherein the pellet maintains a specific surface area after compacting that is at least 80% of an initial specific surface area of the pellet before compacting.

4. The method of claim 2 , wherein the pellet maintains a specific surface area after compacting that is at least 90% of an initial specific surface area of the pellet before compacting.

5. The method of claim 2 , wherein the pellet maintains a specific surface area after compacting of at least 80% compared to a pre-compacted specific surface area.

6. The method of claim 1 , wherein the second solvent has a lower boiling point than the first solvent.

7. The method of claim 1 , wherein the second solvent includes methanol, acetone, dichloromethane, ethanol, or water.

8. The method of claim 1 , wherein the MOF powder is dried using a flowing gas between the exchanging step and the compacting step.

9. The method of claim 1 , wherein desolvating the compacted pellet to remove the second solvent includes heating the pellet to at least a boiling point of the second solvent.

10. The method of claim 9 , wherein desolvating the compacted pellet to remove the second solvent further includes applying a vacuum to the compacted pellet.

11. A method, comprising:
exchanging a first solvent in pores of a metal organic framework (MOF) powder with a second solvent having a lower boiling point than the first solvent, such that the pores of the MOF powder are at least 10% filled with the second solvent;
compacting the MOF powder having at least 10% filled pores into a pellet; and
desolvating the compacted pellet to remove the second solvent.

12. The method of claim 11 , wherein the MOF powder is compacted to a density of at least 65% of a theoretical density of the MOF crystal structure to form the pellet.

13. The method of claim 12 , wherein the pellet maintains a specific surface area after compacting that is at least 80% of an initial specific surface area of the pellet before compacting.

14. The method of claim 12 , wherein the pellet maintains a specific surface area after compacting that is at least 90% of an initial specific surface area of the pellet before compacting.

15. The method of claim 12 , wherein the pellet maintains a specific surface area after compacting of at least 1,400 m 2 /g.

16. The method of claim 12 , wherein the pores of the MOF powder are at least 50% filled with the second solvent after the exchanging step and during the compacting step.

17. A gas storage material, comprising:
a compacted pellet of metal organic framework (MOF) powder, the pellet having a density of at least 60% of a theoretical density of the MOF crystal structure and a specific surface area of at least 1,000 m 2 /g, the specific surface area of the compacted pellet being at least 80% of a specific surface area of the MOF powder in a non-compacted state.

18. The gas storage material of claim 17 , wherein the specific surface area of the compacted pellet is at least 90% of a specific surface area of the MOF powder in a non-compacted state.

19. The gas storage material of claim 17 , wherein the compacted pellet has a specific surface area of at least 1,400 m 2 /g.

20. The gas storage material of claim 17 , wherein the compacted pellet does not include a binder.

Assignees

• Ford Global Tech Llc

Inventors

• Xu Chunchuan
• Purewal Justin
• Veenstra Michael J

Classifications

• C10L2290/542

  Adsorption of impurities during preparation or upgrading of a fuel · CPC title

• B01J20/226 Primary

  Coordination polymers, e.g. metal-organic frameworks [MOF], zeolitic imidazolate frameworks [ZIF] (preparation of metal complexes containing carboxylic acid moieties C07C51/418; MOF's per se C07F) · CPC title

• C01B3/0084

  Solid storage media characterised by their shape, e.g. porous compacts or hollow particles · CPC title

• B01J20/28066

  being more than 1000 m2/g · CPC title

• B01J20/28014

  characterised by their form · CPC title