IP Library Granted Patent US 12,109,549
Granted Patent B2
US 12,109,549 · App. 17/054,590 · Granted Oct 8, 2024

Method of making colloidal suspensions of metal organic frameworks in polymeric solutions and uses thereof

Inventors: Ignacio Luz Minguez (Durham, NC); Mustapha Soukri (Cary, NC); Marty Lail (Raleigh, NC); Lora Goon Toy (Morrisville, NC)
Assignee: Research Triangle Institute
B01J20/226B01D53/02B01D53/228B01J20/28026B01J20/28033B01J20/28059B01J20/28061B01J20/28064B01J20/28066B01J20/28083B01D2253/204
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Quick Facts
Patent No.
US 12,109,549
App. No.
17/054,590
Granted
Oct 8, 2024
Kind
B2
Abstract

A method for making a metal organic framework suspension is described herein. The method includes providing a hybrid material comprising a nano-crystalline metal organic framework comprising micropores and a mesoporous polymeric material comprising mesopores, wherein the nano-crystalline metal organic framework is homogeneously dispersed and substantially present only within the mesopores or void spaces of the mesoporous polymeric material; and wherein the hybrid material has a weight percentage of the metal organic framework in the range of 5-50% relative to the total weight of the hybrid material. The method includes contacting the hybrid material with a solvent in which the mesoporous polymeric material is soluble, thereby forming a polymeric solution in which the nano-crystalline metal organic framework is substantially homogeneously dispersed and suspended.

Claims (22)

1. A method for making a metal organic framework suspension comprising

providing a hybrid material comprising a nano-crystalline metal organic framework comprising micropores and a mesoporous polymeric material comprising mesopores, wherein the nano-crystalline metal organic framework is homogeneously dispersed and substantially present only within the mesopores or void spaces of the mesoporous polymeric material; and wherein the hybrid material has a weight percentage of the metal organic framework in the range of 5-50% relative to the total weight of the hybrid material; and

contacting the hybrid material with a solvent in which the mesoporous polymeric material is soluble, thereby forming a polymeric solution in which the nano- crystalline metal organic framework is substantially homogeneously dispersed and suspended.

2. The method of claim 1 , further comprising

providing a solution of a second polymeric material; and

combining the metal organic framework suspension with the second polymer solution to form a second metal organic framework suspension.

3. The method of claim 1 , wherein the metal organic framework, comprises at least one metal selected from the group consisting of Mg, V, Cr, Mo, Zr, Hf, Mn, Fe, Co, Cu, Ni, Zn, Ru, Al, and Ga.

4. The method of claim 1 , wherein the metal organic framework is at least one selected from the group consisting of MIL-101, MIL -100, MIL-53, MOF-74, UiO-66, UiO-67, ZIF-8, ZIFs, HKUST-1, M 2 (dobpdc), NU -1000, PCN-222, PCN-224, and derivatives thereof.

5. The method of claim 1 , wherein the micropores have an average diameter in the range of 0.5-5.0 nm.

6. The method of claim 1 , wherein the hybrid material comprises mesopores with an average diameter in the range of 2-50 nm and micropores with an average diameter in the range of 0.5-5.0 nm.

7. The method of claim 1 , wherein the mesopores, the micropores, or both are monodisperse, having a coefficient of variation of less than 10%.

8. The method of claim 1 , wherein the nano- crystalline metal organic framework has an average longest linear dimension of less than 200 nm.

9. The method of claim 1 , wherein the hybrid material has a surface area in the range of 10-1200 m 2 /g.

10. The method of claim 1 , wherein the hybrid material has an average longest linear dimension of 100-500 μm.

11. The method of claim 1 , wherein the polymeric material comprises Tenax®, mesoporous polyacrylamides, or mesoporous polyacrylonitriles.

12. The method of claim 1 , wherein the solvent comprises an organic solvent.

13. The method of claim 1 , wherein the organic solvent comprises: acetone, methanol, ethanol, isopropanol, propanol, butanol, acetonitrile, THF, DMF, CHCl 3 , CH 2 Cl 2 , toluene, or dioxane.

14. The method of claim 1 , further comprising purifying the hybrid material prior to contacting it with the solvent.

15. The method of claim 14 , wherein purifying comprises

dissolving the hybrid material in a solvent;

filtering the resulting solution; and

precipitating a purified hybrid material from the filtered solution.

Assignments (2)
CONFIRMATORY LICENSE Recorded Apr 27, 2021
From: RESEARCH TRIANGLE INSTITUTE
To: UNITED STATES DEPARTMENT OF ENERGY
Reel/Frame 056119/0004 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Nov 11, 2020
From: LUZ-MINGUEZ, IGNACIO; SOUKRI, MUSTAPHA; LAIL, MARTY; TOY, LORA GOON
To: RESEARCH TRIANGLE INSTITUTE
Reel/Frame 054334/0255 →
Continuity (2)
Provisional Application 62673389 · May 18, 2018
Related Publication 20210053024A1 · Feb 25, 2021