IP Library Granted Patent US 10,695,741
Granted Patent B2
US 10,695,741 · App. 15/186,004 · Granted Jun 30, 2020

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

Inventors: Radha Kishan Motkuri (Richland, WA); Jagannadha R. Bontha (Richland, WA); B. Peter McGrail (Pasco, WA)
Assignee: Battelle Memorial Institute
B01J19/10B01J19/0013B01J19/06B01J20/226B01J20/3085B01J20/3204B01J20/3236B01J20/3293B01J31/1691B01J35/026B01J37/0072C07C51/418C07C51/43C07C63/307C07C65/05C07F3/003C07F7/003C07F15/045C07F15/065B01J2219/00051B01J2219/0877B01J2231/005B01J2531/16B01J2531/845B01J2531/847
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Quick Facts
Patent No.
US 10,695,741
App. No.
15/186,004
Granted
Jun 30, 2020
Kind
B2
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%.

Claims (15)

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).

Assignments (2)
CONFIRMATORY LICENSE Recorded Jul 18, 2016
From: BATTELLE MEMORIAL INSTITUTE, PACIFIC NORTHWEST DIVISION
To: U.S. DEPARTMENT OF ENERGY
Reel/Frame 039376/0557 →
ASSIGNMENT OF ASSIGNOR'S INTEREST Recorded Jun 28, 2016
From: MOTKURI, RADHA KISHAN; BONTHA, JAGANNADHA R.; MCGRAIL, B. PETER
To: BATTELLE MEMORIAL INSTITUTE
Reel/Frame 039028/0304 →
Continuity (1)
Related Publication 20170361300A1 · Dec 21, 2017
Cited By (9)
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