System and process for continuous and controlled production of metal-organic frameworks and metal-organic framework composites

Patent metadata

Field	Value
Publication number	US-10695741-B2
Application number	US-201615186004-A
Country	US
Kind code	B2
Filing date	Jun 17, 2016
Priority date	Jun 17, 2016
Publication date	Jun 30, 2020
Grant date	Jun 30, 2020

Abstract

A MOF production system and method of making are detailed for continuous and controlled synthesis of MOFs and MOF composites. The system can provide optimized yields of MOFs and MOF composites greater than or equal to 95%.

First claim

What is claimed is:

1. A continuous method for making Metal Organic Framework (MOF) composites that include a core and a shell about the core, the method comprising:
in one series of steps ( 1 a - 5 a ), step 1 a , providing a first MOF solution of a first MOF precursor and a first solvent, wherein the first MOF precursor comprises a salt of a metal selected from the group consisting of cobalt, aluminum and chromium, and a linker selected from the group consisting of a terephthalic acid (MIL-101 or MIL-53), and a dihydoxyterephthalic acid (MOF-74);
step 2 a , forming a plume of aerosolized liquid droplets of the first MOF solution;
step 3 a , suspending the aerosolized liquid droplets of the first MOF solution in a carrier gas in a fluidized bed reactor;
step 4 a , condensing the aerosolized liquid droplets of the first MOF solution to form seed MOF particles;
step 5 a , removing the first solvent from the MOF seed particles to form cores of the MOF composites;
in another series of steps ( 1 b - 3 b ), step 1 b , providing a second MOF solution of a second MOF precursor and a second solvent, wherein the second MOF precursor comprises a Ni-salt and a dihydroxyterephthalic acid (MOF-74);
step 2 b , forming a plume of aerosolized liquid droplets of the second MOF solution;
step 3 b , suspending the aerosolized liquid droplets of the second MOF solution in the carrier gas in the fluidized bed reactor;
and further, condensing the aerosolized liquid droplets of the second MOF solution of the step 3 b to form the shell onto the existing MOF cores of the step 5 a to form the MOF composites;
removing the second solvent from the MOF composites, wherein the MOF composites are from 200 um to 1500 um in size.

2. The method of claim 1 further comprising recovering the first and the second solvents from the reactor and recycling the solvents to form the first and the second MOF solutions comprising the first and the second MOF precursors.

3. The method of claim 1 wherein the aerosolizing the first and the second MOF solutions to form the aerosolized liquid droplets comprises ultrasonically aerosolizing the solutions.

4. The method of claim 1 further comprising providing the MOF composites to a separation device configured to separate the composites by size.

5. The method of claim 1 wherein the MOF composites comprise one or more of: Ni-MOF-74(shell)/Cr-MIL-101(core); Ni-MOF-74(shell)/Co-MOF-74(core); or Ni-MOF-74(shell)/Al-MIL-53(core).

Assignees

• Battelle Memorial Institute

Inventors

• Motkuri Radha Kishan
• Bontha Jagannadha R
• Mcgrail B Peter

Classifications

• B01J2235/00

  Indexing scheme associated with group B01J35/00, related to the analysis techniques used to determine the catalysts form or properties · CPC title

• B01J2235/15

  X-ray diffraction · CPC title

• B01J2235/30

  Scanning electron microscopy; Transmission electron microscopy · CPC title

• B01J35/50

  characterised by their shape or configuration · CPC title

• C07C63/307

  Monocyclic tricarboxylic acids · CPC title