US 11,896,947 B2
System and process for continuous and controlled production of metal-organic frameworks and metal-organic framework composites
Radha Kishan Motkuri, Richland, WA (US); Jagannadha R. Bontha, Richland, WA (US); and B. Peter McGrail, Pasco, WA (US)
Assigned to Battelle Memorial Institute, Richland, WA (US)
Filed by Battelle Memorial Institute, Richland, WA (US)
Filed on Jun. 30, 2020, as Appl. No. 16/916,110.
Application 16/916,110 is a continuation of application No. 15/186,004, filed on Jun. 17, 2016, granted, now 10,695,741.
Prior Publication US 2020/0391174 A1, Dec. 17, 2020
This patent is subject to a terminal disclaimer.
Int. Cl. B01J 19/10 (2006.01); B01J 19/06 (2006.01); B01J 19/00 (2006.01); B01J 20/22 (2006.01); B01J 20/30 (2006.01); B01J 31/16 (2006.01); B01J 35/02 (2006.01); B01J 37/00 (2006.01); C07F 15/06 (2006.01); C07F 3/00 (2006.01); C07C 63/307 (2006.01); C07F 15/04 (2006.01); C07C 65/05 (2006.01); C07C 51/43 (2006.01); C07C 51/41 (2006.01); B01J 20/32 (2006.01); C07F 7/00 (2006.01)
CPC B01J 19/10 (2013.01) [B01J 19/0013 (2013.01); B01J 19/06 (2013.01); B01J 20/226 (2013.01); B01J 20/3085 (2013.01); B01J 20/3204 (2013.01); B01J 20/3236 (2013.01); B01J 20/3293 (2013.01); B01J 31/1691 (2013.01); B01J 35/026 (2013.01); B01J 37/0072 (2013.01); C07C 51/418 (2013.01); C07C 51/43 (2013.01); C07C 63/307 (2013.01); C07C 65/05 (2013.01); C07F 3/003 (2013.01); C07F 7/003 (2013.01); C07F 15/045 (2013.01); C07F 15/065 (2013.01); B01J 2219/00051 (2013.01); B01J 2219/0877 (2013.01); B01J 2231/005 (2013.01); B01J 2531/16 (2013.01); B01J 2531/845 (2013.01); B01J 2531/847 (2013.01)] 5 Claims
 
1. A continuous method for making Metal Organic Framework (MOF) composites that include a core and a shell about the core, the method comprising a first series of steps to form a core and a second series of steps to form a shell about the core, the first and the second series of steps of the method comprising:
performing the first series of steps in the following order:
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 comprising cobalt, aluminum, or chromium and a first linker comprising a terephthalic acid or a dihydoxyterephthalic acid;
forming a plume of aerosolized liquid droplets of the first MOF solution;
suspending the aerosolized liquid droplets of the first MOF solution in a carrier gas in a fluidized bed reactor;
condensing the aerosolized liquid droplets of the first MOF solution to form seed MOF particles;
removing the first solvent from the MOF seed particles to form cores of the MOF composites;
after performing the first series of steps, performing the second series of steps in the following order:
providing a second MOF solution of a second MOF precursor and a second solvent, wherein the second MOF precursor comprises a salt of metal comprising Ni, Zn, Co, Mg, Mn, Fe, or Cu, and a second linker comprising a dihydoxyterephthalic acid;
forming a plume of aerosolized liquid droplets of the second MOF solution;
suspending the aerosolized liquid droplets of the second MOF solution in the carrier gas in the fluidized bed reactor;
condensing the aerosolized liquid droplets of the second MOF solution to form the shell onto the existing MOF cores formed in the first series of steps to form the MOF composites; and
removing the second solvent from the MOF composites, wherein the MOF composites are from 200 μm to 1500 μm in size.