A zirconium metal-organic framework material as crystal sponge and preparation method thereof

A technology of metal-organic frameworks and crystals, applied in material analysis using radiation diffraction, analyzing materials, and using wave/particle radiation for material analysis, etc., can solve problems such as unsuitable for single crystal testing and easy loss of crystallinity, and achieve improvement The performance and preparation method are simple, and the effect of widening the application range

CN110283328BActive Publication Date: 2021-12-07JIANGHAN UNIVERSITY
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Patent Information

Authority / Receiving Office
CN · China
Patent Type
Patents(China)
Current Assignee / Owner
Publication Date
2021-12-07

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Abstract

The invention discloses a zirconium metal organic framework material as a crystal sponge and a preparation method thereof, belonging to the field of metal organic framework materials. The chemical formula of the zirconium metal organic framework material is: [Zr 6 (μ 3 -O) 4 (μ 3 -OH) 4 (OH) 2 (H 2 O) 2 (HCOO) 2 (L) 4 ] n , where L is 2'-amino-5'-cyano-[1,1':3',1"-terphenyl]-4,4"-dicarboxylic acid, n is ∞, and the overall framework structure is a quadruple Interspersed with a metal organic framework, the zirconium metal organic framework material belongs to the trigonal crystal system, the space group is R-3c, the unit cell parameters are α=β=90°, γ=120°, and the unit cell volume is provided by the embodiment of the present invention Zirconium metal-organic framework materials can act as crystal sponges to adsorb iodine molecules, and the structure of iodine after adsorption was characterized by single crystal X‑ray diffraction. This invention broadens the range of applications of MOFs in characterizing guest molecules, especially for inorganic substances dissolved in non-pure organic solvents.
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Description

technical field

[0001] The invention relates to the field of metal organic framework materials, in particular to a zirconium metal organic framework material as crystal sponge and a preparation method thereof. Background technique

[0002] Metal-organic frameworks (MOFs), as one of the current hot research materials, have unique application prospects in many fields due to their specific framework structure and channel effect. Metal-organic frameworks have a highly ordered spatial configuration, stable pore structure, excellent adsorption performance, and periodically repeated component arrangements, and can fully explore their structural differences at the atomic level by using single crystal diffraction techniques. Studies have begun to explore the use of MOFs as carriers to test the related research of guest molecules. This strategy is called crystal sponge. The advantage of this technique is that it can clearly characterize the relevant configuration and other structural...

Examples

Embodiment 1

[0043] Preparation of zirconium metal-organic frameworks

[0044] The preparation method is as follows:

[0045]1. Preparation of 2'-amino-5'-cyano-[1,1':3',1″-terphenyl]-4,4″-dicarboxylic acid:

[0046] (1) Under a nitrogen atmosphere, 3,5-dibromoaminobenzonitrile (16.0mmol), 4-phenylboronic acid methyl formate (38.0mmol), potassium phosphate (93.0mmol), were added to 1,4-dioxane Tetrakis(triphenylphosphine)palladium (1.1mmol) was added into the ring (500mL) solvent, then the temperature was raised to 80°C, refluxed for 45 hours, and cooled to room temperature;

[0047] (2) After removing the organic solvent by rotary evaporation, dichloromethane (100 mL) and H 2 O (50mL), the organic phase was separated, then the aqueous phase was extracted three times with dichloromethane (60mL), the combined organic phases were washed with saturated brine for extraction, and washed with anhydrous MgSO 4 Dry to obtain solution A;

[0048] (3) Solution A was rotary evaporated to remove t...

Embodiment 2

[0055] Preparation of zirconium metal-organic frameworks

[0056] The preparation method is as follows:

[0057] 1. Preparation of 2'-amino-5'-cyano-[1,1':3',1″-terphenyl]-4,4″-dicarboxylic acid:

[0058] (1) Under a nitrogen atmosphere, 3,5-dibromoaminobenzonitrile (16.8mmol), 4-phenylboronic acid methyl formate (40.0mmol), potassium phosphate (95.0mmol), were added to 1,4-dioxane Tetrakis(triphenylphosphine)palladium (1.3mmol) was added to the ring (550mL) solvent, then the temperature was raised to 100°C, refluxed for 50 hours, and cooled to room temperature;

[0059] (2) After removing the organic solvent by rotary evaporation, dichloromethane (100 mL) and H 2 O (50mL), the organic phase was separated, then the aqueous phase was extracted three times with dichloromethane (60mL), the combined organic phases were washed with saturated brine for extraction, and washed with anhydrous MgSO 4 Dry to obtain solution A;

[0060] (3) Solution A was rotary evaporated to remove t...

Embodiment 3

[0067] Preparation of zirconium metal-organic frameworks

[0068] The preparation method is as follows:

[0069] 1. Preparation of 2'-amino-5'-cyano-[1,1':3',1″-terphenyl]-4,4″-dicarboxylic acid:

[0070] (1) Under a nitrogen atmosphere, 3,5-dibromoaminobenzonitrile (16.4mmol), 4-phenylboronic acid methyl formate (39.0mmol), potassium phosphate (94.0mmol), were added to 1,4-dioxane Add tetrakis(triphenylphosphine)palladium (1.2mmol) into the ring (530mL) solvent, then raise the temperature to 90°C, reflux for 48 hours, and cool to room temperature;

[0071] (2) After removing the organic solvent by rotary evaporation, dichloromethane (100 mL) and H 2 O (50mL), the organic phase was separated, then the aqueous phase was extracted three times with dichloromethane (60mL), the combined organic phases were washed with saturated brine for extraction, and washed with anhydrous MgSO 4 Dry to obtain solution A;

[0072] (3) Solution A was rotary evaporated to remove the organic sol...