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1.发明授权公开(公告)号：US12227526B2
公开(公告)日：2025-02-18
申请号：US17310622
申请日：2020-03-30
Inventor： Joseph M. Falkowski , Carter W. Abney , Mary S. Abdulkarim , Aaron Sattler , Michele Paccagnini , Simon C. Weston
Abstract: Metal-organic framework materials (MOFs) are highly porous entities comprising a multidentate organic ligand coordinated to multiple metal centers, typically as a coordination polymer. Crystallization may be problematic in some instances when secondary binding sites are present in the multidentate organic ligand. Multidentate organic ligands comprising first and second binding sites bridged together with a third binding site comprising a diimine moiety may alleviate these issues, particularly when using a preformed metal cluster as a metal source to form a MOF. Such MOFs may comprise a plurality of metal centers, and a multidentate organic ligand coordinated to the plurality of metal centers to define an at least partially crystalline network structure having a plurality of internal pores, and in which the multidentate organic ligand comprises first and second binding sites bridged together with a third binding site comprising a diimine moiety. Particular MOFs may comprise N,N′-di(1H-pyrazol-4-yl)ethane-1,2-diimine as a multidentate organic ligand.
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公开(公告)号：US12037349B2
公开(公告)日：2024-07-16
申请号：US17310633
申请日：2020-03-30
Inventor： Joseph M. Falkowski , Mary S. Abdulkarim , Carter W. Abney
CPC classification number: C07F3/06 , C01B37/00 , C01B39/00 , C07F3/003 , C07F3/02 , C07F15/045 , C07F15/065 , C07F19/005
Abstract: Metal-organic framework materials (MOFs) are highly porous entities comprising a multidentate organic ligand coordinated to multiple metal centers, typically as a coordination polymer. MOFs may comprise a plurality of metal centers, and a multidentate organic ligand coordinated via at least two binding sites to the plurality of metal centers to define an at least partially crystalline network structure having a plurality of internal pores, and in which the multidentate organic ligand comprises first and second binding sites bridged together with a third binding site comprising a diimine moiety. The multidentate organic ligand may comprise a reaction product of a vicinal dicarbonyl compound and an amine-substituted salicylic acid to define the first, second and third binding sites. Particular MOFs may comprise 5,59′-(((1E,2E)-ethane-1,2-diylidene)bis-(azaneylylidene))bis(2-hydroxybenzoic acid) as a multidentate organic ligand.
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公开(公告)号：US20240261759A1
公开(公告)日：2024-08-08
申请号：US18561646
申请日：2022-05-31
Inventor： Matthew T. Kapelewski , Joseph M. Falkowski , Dominick A. Zurlo , Mary S. Abdulkarim
CPC classification number: B01J20/226 , B01J20/28064 , B01J20/28066 , B01J20/28071 , B01J20/28073 , B01J20/3078 , B01J2531/48
Abstract: Provided are methods of making a MOF UiO-66 comprising reacting zirconium oxychloride with terephthalic acid or derivative thereof and acetic acid in a solvent to provide a reaction solution; diluting the reaction solution with water, heating the diluted reaction solution and reducing the reaction temperature of the reaction mixture to provide the MOF UiO-66 having a micropore volume greater than or equal to 0.45 cc/g and a crystal size of between about 20 nm and about 1000 nm. Also provided are methods of making a MOF UiO-66 where a zirconium hydroxide acetate and zirconium hydroxide are reacted with a carboxylic acid or derivative thereof and acetic acid in a solvent to produce the metal-organic framework MOF UiO-66 having a micropore volume at least 0.35 cc/gram.
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公开(公告)号：US12036539B2
公开(公告)日：2024-07-16
申请号：US17621281
申请日：2020-05-28
Inventor： Joseph M. Falkowski , Yogesh V. Joshi , Mary S. Abdulkarim , Simon C. Weston
CPC classification number: B01J31/1691 , B01J35/617 , B01J35/618 , B01J35/633 , B01J35/635 , B01J35/643 , B01J35/647 , B01J37/04 , B01J37/30 , C07C5/03 , C07F3/06 , B01J2231/645 , B01J2531/0205 , B01J2531/0211 , B01J2531/0238 , B01J2531/26 , B01J2531/72 , B01J2531/845 , B01J2531/847 , C07C2531/22
Abstract: Metal-organic framework materials (MOFs) are highly porous entities comprising a multidentate organic ligand coordinated to multiple metal centers. MOFs having ambient condition stability may comprise a plurality of metal clusters comprising one or more M4O clusters (M is a metal), and a plurality of 4-pyrazolecarboxylate ligands coordinated to the plurality of metal clusters to define an at least partially crystalline network structure having a plurality of internal pores. The MOFs may have a Pa3 symmetry, which upon activation may convert into Fm3m symmetry. Methods for synthesizing the MOFs may comprise combining a metal source, such as a preformed metal cluster, with 4-pyrazolecarboxylic acid, and reacting the preformed metal cluster with the 4-pyrazolecarboxylic acid to form a MOF having an at least partially crystalline network structure with a plurality of internal pores defined therein and comprising a plurality of metal clusters coordinated to a multidentate organic ligand comprising 4-pyrazolecarboxylate.
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公开(公告)号：US20240300983A1
公开(公告)日：2024-09-12
申请号：US18572039
申请日：2022-06-23
Inventor： Joseph M. Falkowski , Mary S. Abdulkarim
CPC classification number: C07F7/003 , B01J20/226 , B01J20/3078 , B01J20/3085 , B01J31/1691 , B01J37/031 , B01J37/04 , B01J37/08 , B01J2531/48 , B01J2531/49
Abstract: Provided herein are methods of making a metal-organic framework comprising: combining a pre-ligand with a metal source to provide a plurality of solid reactants; adding a solvent to the plurality of solid reactants to form a reaction mixture, wherein at least 50 wt % of the reaction mixture are the plurality of solid reactants; heating the reaction mixture wherein the pre-ligand is converted to a ligand in the reaction mixture and the ligand reacts with the metal component; and cooling the reaction mixture to produce the metal-organic framework. The present methodologies are performed without dimethylformamide in the reaction mixture. The present methods may further comprise the step of adding a crystallization aid such as zinc oxide to the reaction mixture.
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Patent Agency Ranking
公开(公告)号：US20240278208A1
公开(公告)日：2024-08-22
申请号：US18572034
申请日：2022-06-23
Inventor： Joseph M. Falkowski , Mary S. Abdulkarim , Sophie Liu , Scott J. Weigel , Trong D. Pham
CPC classification number: B01J20/226 , B01J20/0225 , B01J20/0237 , B01J20/0244 , B01J20/0251 , B01J20/0288 , B01J20/0296 , B01J20/28066 , B01J20/28071 , B01J20/28073 , B01J20/28076 , B01J20/3085
Abstract: Provided are metal-organic frameworks made by the process of comprising the steps of reacting a first metal source that can generate a tetravalent metal cation in solution, a linear dicarboxylic acid, a second metal source that can generate a divalent cation in solution, and one or more monocarboxylic acid modulators in a solvent to provide a reaction solution. The reaction solution is heated to provide a metal-organic framework having between about 0 wt. % to 10 wt. % of divalent cation, surface area between about 1100 m2/g and 2700 m2/g, a porosity of between about 0.45 cc/g and 1.1 cc/g, and a relative intensity equal to or greater than 0.35 and a peak width ratio of less than 3.0.
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公开(公告)号：US20240254148A1
公开(公告)日：2024-08-01
申请号：US18413176
申请日：2024-01-16
Inventor： Joseph M. Falkowski , Mary S. Abdulkarim , Trong D. Pham , Julie J. Seo
CPC classification number: C07F7/00 , B01J20/226 , C07B2200/13
Abstract: Provided herein are methods of making metal-organic frameworks comprising combining a first pre-ligand and at least one of a second pre-ligand or a first ligand with a metal source comprising a metal component to provide a plurality of reactants where at least 50 wt % of the reaction mixture is the plurality of reactants after solvent has been added to the plurality of reactants. Also provided herein are methods of making metal-organic frameworks comprising combining a pre-ligand with a metal source selected from metal acetates, metal hydroxyacetates, metal carbonates, metal hydroxycarbonates, and mixtures thereof.
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公开(公告)号：US12172146B2
公开(公告)日：2024-12-24
申请号：US17607168
申请日：2020-05-26
Inventor： Joseph M. Falkowski , Yogesh V. Joshi , Mary S. Abdulkarim , Simon C. Weston
Abstract: Metal-organic framework materials (MOFs) are highly porous entities comprising a multidentate organic ligand coordinated to multiple metal centers, typically as a coordination polymer. Some highly porous MOFs lack stability at ambient conditions. MOFs having ambient condition stability may comprise a plurality of metal clusters (M4O clusters, M=a metal), and a plurality of 4-(1H-pyrazol-4-yl)benzoate ligands coordinated to the plurality of metal clusters to define an at least partially crystalline network structure having a plurality of internal pores. Methods for synthesizing these MOFs may comprise combining a metal source, such as a preformed metal cluster, with 4-(1H-pyrazol-4-yl)benzoic acid, and reacting the preformed metal cluster with the 4-(1H-pyrazol-4-yl)benzoic acid to form a MOF having an at least partially crystalline network structure with a plurality of internal pores defined therein and comprising a plurality of metal clusters coordinated to a multidentate organic ligand comprising 4-(1H-pyrazol-4-yl)benzoate.
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9.发明公开公开(公告)号：US20240286112A1
公开(公告)日：2024-08-29
申请号：US18572045
申请日：2022-06-23
Inventor： Joseph M. Falkowski , Mary S. Abdulkarim , Julie J. Seo
IPC: B01J20/22
CPC classification number: B01J20/226
Abstract: Provided herein are post-synthesis methods of thermally stabilizing a metal-organic framework having defects that decomposes after about 12 hours at a first temperature. The methods include contacting the metal-organic framework with a stabilizing solution to provide a treated metal-organic framework. The treated metal-organic framework is thermally stable after 12 hours at a second temperature at least about 50° C. greater than the first temperature. Also, the treated metal-organic framework has a PXRD pattern that is substantially the same as the PXRD pattern of the untreated metal-organic framework. Provided herein are also post-synthesis methods to improve CO2 adsorption of metal-organic frameworks. Provided herein are also modified EMM-71 metal-organic frameworks.
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公开(公告)号：US11891407B2
公开(公告)日：2024-02-06
申请号：US17400742
申请日：2021-08-12
Inventor： Carter W. Abney , Joseph M. Falkowski , Mary S. Abdulkarim , Anna C. Ivashko , Julie J. Seo , Aaron W. Peters , Matthew T. Kapelewski , Gerardo J. Majano Sanchez , Wesley Sattler , Simon C. Weston
CPC classification number: C07F3/02 , B01D53/04 , B01J20/226 , C01B37/00 , B01D2253/204 , B01D2257/504
Abstract: Provided herein are methods of novel methods of synthesizing a metal-organic framework system by vapor-phase appending of a plurality of ligands appended to a metal-organic framework. Also, provided are methods of recycling metal-organic framework systems by detaching the ligand and re-appending the same ligand or appending a different ligand to the metal-organic framework to provide a recycled or repurposed metal-organic framework system.
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