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Preparation method and application of a metal-organic framework catalyst with twisted structure

A metal-organic framework and catalyst technology, applied in the field of photocatalytic materials, can solve problems such as unfavorable catalytic reactions and high efficiency

Active Publication Date: 2021-12-31
DALIAN UNIV OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

Previous work has shown that the direct conjugation between the photosensitive center and the variable-valence metal center is often conducive to the formation of a "molecular wire" type of bidirectional electron transfer. The excited-state photosensitizer is easy to transfer electrons to the variable-valence metal center, and it is also easy for electrons to return. This is not conducive to the efficient progress of the catalytic reaction

Method used

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  • Preparation method and application of a metal-organic framework catalyst with twisted structure
  • Preparation method and application of a metal-organic framework catalyst with twisted structure
  • Preparation method and application of a metal-organic framework catalyst with twisted structure

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] The preparation of Cu-Twisted comprises the following steps:

[0037] Step 1. Dissolve triphenylamine (10.0g, 40.8mmol) in 120mL N,N-dimethylformamide, and add N-bromosuccinimide (25.1g, 134.6mmol ) and stirred for 12 hours, added 150mL dichloromethane to dilute after the reaction was finished, then washed with deionized water and saturated sodium chloride solution successively, collected the organic phase and added anhydrous sodium sulfate to dry, poured 200mL into the organic phase after filtration Iced methanol, then filtered and collected the filter cake to obtain 16.7g of white needle-shaped solid, 85% of productive rate, and the H NMR spectrum was 1 H NMR (400MHz, CDCl 3 ) δ = 7.35 (d, J = 8.8Hz, 6H), 6.92 (d, J = 8.8Hz, 6H).

[0038] Step 2. Weigh the white needle-like solid (3.86g, 8.0mmol) prepared in step 1, bis-linked pinacol diboron (7.6g, 30.0mmol), potassium acetate (13.7g, 140.0mmol) and bis (Diphenylphosphino)ferrocenepalladium chloride (0.8g, 1.2mmol...

Embodiment 2

[0047] Preparation of Cu-Planar, the ligand H 3 Planar (180mg, 0.3mmol) and copper nitrate (241mg, 1.0mmol) were dissolved in a mixed solution of 40mL N,N-dimethylformamide and 10mL ethanol, and then 1.5mL was added to it at a concentration of 3mol L -1 Hydrochloric acid, after ultrasonic solubilization, sealed into a hydrothermal reaction kettle with a polytetrafluoroethylene lining, and placed in an oven at 85°C for 50h, then lowered to room temperature, removed the supernatant, and added ethanol to wash , and centrifuged to obtain 195 mg of green massive crystal Cu-Planar with a yield of 45%. Single crystal tests reveal crystallographic data for Cu-Planar: Molecular formula, C 78 h 48 Cu 3 N 2 o 15 , molecular weight Mr=1443.83, cubic crystal system, space group Fm-3m, green blocky crystal, unit cell parameter is α=β=γ=90°, The number of molecules in the unit cell Z = 16, the crystal density D c =0.168g cm -1 , the absorption factor is 0.119mm -1 , there are...

Embodiment 3

[0049] Add 5.3mg of Cu-Twisted and 3.5mg of Cu-Planar to 5mL of ethanol to make a suspension, then add 0.5mL of Nafin and mix by ultrasonic, take 80μL of the suspension and apply it on the surface of FTO glass, The coating area is 1cm 2 , dried, and then clamp the FTO glass on the electrode holder as the working electrode. The photocurrent test was carried out on a CHI 660E electrochemical workstation, using a three-electrode system, an Ag / AgCl electrode as a reference electrode, a platinum sheet electrode as a counter electrode, and 0.05M tetrabutylammonium hexafluorophosphate acetonitrile solution as an electrolyte. The current test is performed under the condition of 1atm oxygen, the temperature is room temperature, the light source is a 300W xenon lamp and the ultraviolet light band is removed through a 400nm filter. The test spectrum of photocurrent, such as image 3 shown. The test of electron sequential resonance is carried out on the A200-9.5 / 12 paramagnetic resonan...

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Abstract

The invention belongs to the technical field of photocatalytic materials, and relates to a preparation method and application of a metal-organic framework catalyst with a twisted structure, wherein the preparation method is to use a ligand H with a twisted structure 3 Twisted and copper nitrate, a metal-organic framework catalyst with a twisted structure was prepared by a solvothermal method, and its synthetic route is as follows: H 3 Twisted+Cu(NO 3 ) 2 ·H 2 O→Cu-Twisted; Cu-Twisted, the metal-organic framework catalyst Cu-Twisted with a twisted structure of the present invention, benefits from the controlled electron transfer process, and the retained divalent copper node exerts an inner shell electron regulation effect on the substrate, realizing Selective chlorotrifluoromethyl difunctionalization of electron-deficient alkenes without homogeneous catalysts exhibiting chemical regioselectivity in this reaction.

Description

technical field [0001] The invention relates to a preparation method and application of a metal-organic framework catalyst with a twisted structure, belonging to the technical field of photocatalytic materials. Background technique [0002] Carbon-heteroatom coupling reactions play an important role in the field of medicinal chemistry, and the construction of many physiologically active drug molecules relies on this type of reaction. As a synthetic methodology that has advanced by leaps and bounds in recent years, photocatalysis can generate free radical intermediates through electron transfer between excited-state photosensitizers and substrates, so that many reactions that are difficult to achieve by conventional methods can be achieved through free radical pathways. Thanks to its own multi-valence characteristics, divalent copper catalysts are easy to capture carbon radical intermediates and undergo reduction and elimination processes, thereby realizing carbon-heteroatom ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): B01J31/22C08G83/00C07C41/01C07C67/347C07C213/00C07C231/12C07C319/14C07D207/44C07D209/42C07D209/48C07D231/56C07C217/84C07C43/235C07C321/28C07C69/63C07C233/07C07J9/00
CPCB01J31/2239C08G83/008C07D231/56C07D209/42C07D209/48C07D207/44C07C213/00C07C319/14C07C41/01C07C67/347C07C231/12C07J9/00B01J2531/16B01J2231/4283B01J2231/4288B01J2231/4294B01J2231/32B01J35/39C07C217/84C07C43/235C07C321/28C07C69/63C07C233/07
Inventor 段春迎张铁欣史雨生姜小明徐刚何成
Owner DALIAN UNIV OF TECH
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