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Tri pyrazole ligand based nickel metal organic framework material, and preparation method and applications thereof

A technology of organic framework and three-headed pyrazole, which is applied in the field of crystalline materials, can solve problems such as difficulty in obtaining crystals, difficulty in reversible self-repair of coordination bonds, difficulty in forming MOFs single crystals, etc., and achieves the effect of good alkali stability

Active Publication Date: 2019-05-31
BEIJING UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Strong bond interactions usually make the reversible self-healing of coordination bonds difficult during the bonding process, making it difficult to form single crystals of MOFs, and it is even more difficult to obtain crystals suitable for single crystal testing.

Method used

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  • Tri pyrazole ligand based nickel metal organic framework material, and preparation method and applications thereof
  • Tri pyrazole ligand based nickel metal organic framework material, and preparation method and applications thereof
  • Tri pyrazole ligand based nickel metal organic framework material, and preparation method and applications thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0028] First, 4-bromoacetophenone (20.0mmol) was dissolved in ethanol solution (30mL), and thionyl chloride (40.0mmol) was slowly added dropwise to obtain 4,4"-dibromo-5' -(4-bromophenyl)-1,1':3',1"-terphenyl;

[0029] Under nitrogen protection, 4,4"-dibromo-5'-(4-bromophenyl)-1,1':3',1"-terphenyl (20.0mmol), 1-THP-4-pyrazole Boric acid pinacol ester (75.0mmol) and 1,4-dioxane (300mL) and water (100mL) were added in the 500mL round bottom flask, added magnetic sub-stirring, then added K 2 CO 3 (90.0mmol) and Pd(PPh 3 ) 4 (3.0 mmol), and the reaction system was stirred at 100° C. for 24 hours. After the reaction was completed, the solvent in the reaction system was spin-dried, and the residue was dissolved in ethyl acetate (300mL), washed with water (300mL×2) and saturated brine (300mL) successively, washed over anhydrous Na 2 SO 4 After drying, filter and concentrate. The crude product was purified by column chromatography (SiO 2, petroleum ether / ethyl acetate=20:1~1:1...

Embodiment 2

[0031] The white solid obtained in the previous step was dissolved in hydrochloric acid ethanol solution (2mol L -1 , 300 mL), stirred at 50°C for 24 hours, and after the reaction was completed, the organic solvent was removed by rotary evaporation. The remaining solid was dispersed in 300 mL of water, and then the pH was adjusted to 10 by adding a saturated sodium carbonate aqueous solution dropwise. The resulting suspension was filtered, the solid was washed with water (300mL×3), and dried in vacuum at 60°C to obtain a white solid 4,4'-(5'-(4-(1H-pyrazol-4-yl)benzene base)-[1,1':3',1"-tetraphenyl]-4,4"-diyl)bis(1H-pyrazole)(H 3 BTPP, 65% yield).

Embodiment 3

[0033] Weighing 1,3,5-H 3 BTPP(0.025mmol) and Ni(NO 3 ) 2 ·6H 2 O (0.05mmol, 14.5mg) was put into a 25mL beaker, 3mL of DMA solution and 3mL of deionized water were added, and then the beaker was sealed and put into an ultrasonic instrument, and ultrasonicated at room temperature for 5 minutes. After the end, the solution was transferred to 20mL polytetrafluoroethylene reactor. After sealing, the reaction kettle was placed in an oven at 120° C. for 48 hours to react. Close the oven after the reaction is over, open the reaction kettle after cooling to room temperature, filter and collect the solid particles obtained in the reaction kettle, and then use DMA, H 2 Washed with O and EtOH (5mL×3), observed under a microscope to obtain blue prism crystals (Ni 8 (OH) 4 (OH 2 ) 2 (BTPP) 4 ), (yield: 72%, based on 1,3,5-H 3 BTPP ligand).

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Abstract

The invention discloses a tri pyrazole ligand based nickel metal organic framework material, and a preparation method and applications thereof, and belongs to the technical field of crystalline statematerial. The chemical molecular formula is [Ni8(OH)4(OH2)2(BTPP)4], H3BTPP is used for presenting organic ligand 4, 4'-(5'-(4-(1H-pyrazole-4-yl)phenyl)-[1, 1':3'-1''-tetraphenyl]4, 4''-di yl)bi(1H-pyrazole). The tri pyrazole ligand based nickel metal organic framework material is synthesized under sealing conditions, organic ligand tri pyrazole ligand based nickel metal organic framework material(H3BTPP) and nickel nitrate are subjected to solvothermal reaction in a mixed solution of N, N-dimethyl formamide and water so as to obtain the tri pyrazole ligand based nickel metal organic framework material. The tri pyrazole ligand based nickel metal organic framework material is low in absorption capacity on low carbon hydrocarbons.

Description

technical field [0001] The invention belongs to the technical field of crystalline materials, and the technology relates to metal-organic coordination polymer materials, and is characterized in that it is a metal-organic framework material of nickel, a preparation method and application research thereof. Background technique [0002] Metal-Organic Frameworks (MOFs), which are composed of inorganic nodes composed of metal ions and organic ligands through coordination bonds, have the characteristics of large specific surface area, high porosity, and adjustable channels. MOFs have been rapidly developed in many fields such as separation, sensing, and catalysis. The synthesis of highly stable MOFs is a popular research hotspot in the research field of this type of materials, which will greatly promote the application range of this new type of materials and promote their practical applications. Strong bond interactions usually make the reversible self-healing of coordination bon...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J20/22
Inventor 李建荣孔祥婧张永正何涛
Owner BEIJING UNIV OF TECH
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