Bis-terpyridine based bi-metal polymer and preparation method thereof

A technology based on terpyridyl and double terpyridine, which is applied in chemical instruments and methods, organic compound/hydride/coordination complex catalysts, chemical/physical processes, etc., can solve the problem of high cost of composite materials, low relative catalytic efficiency, Poor stability and other problems, to achieve the effect of improving catalytic activity, high electricity price, and improving stability

Active Publication Date: 2018-08-28
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, in the prior art, due to the relatively weak metal ion coordination ability of the metal polymer catalytic materials prepared with terpyridine, the formed metal organic polymer composites have small size, poor stability, and low relative catalytic efficiency. And the cost of synthesizing the composite material is relatively high

Method used

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  • Bis-terpyridine based bi-metal polymer and preparation method thereof
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  • Bis-terpyridine based bi-metal polymer and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0045] (1) Preparation of double terpyridine ligands:

[0046]Add terephthalaldehyde (0.67g, 5mmol), 2-acetylpyridine (2.9g, 24mmol), NaOH (2.4g, 60mmol) into a 250mL single-necked round bottom flask, add 30mL of ethanol, stir at 25°C for 10h, Add 40mL of 25-28% ammonia water, stir and reflux for 20h, then cool to room temperature, add 100mL of methanol to ultrasonically reflux and filter with suction, repeat twice, then reflux and filter with 100mL glacial acetic acid, wash with methanol once more, and vacuum dry at 50°C to obtain 1.6g Product, white solid, yield 60%. Characterization: 1H NMR (CDCl 3 )δ (ppm): 8.818 (s, 4H), 8.770 (d, J = 2.8Hz, 4H), 8.704 (d, J = 6.4Hz, 4H), 8.075 (s, 4H), 7.908 (t, J = 6.2Hz, 4H), 7.382(t, J=5.0Hz, 4H).

[0047] (2) Preparation of double terpyridine cobalt polymer (Polymer-Co):

[0048] Cobalt Chloride (CoCl 2 ) and 1,4-bis(terpyridine)benzene 3 were refluxed and stirred in ethylene glycol at a molar ratio of 1 / 1 for 12 hours, cooled t...

Embodiment 2

[0052] Transmission Electron Microscopy (TEM) projects electron beams onto the sample, and the electrons collide with the atoms in the sample to change their direction, resulting in solid angle scattering and forming a clear image, so the morphology of nanostructures can be observed intuitively. Take a certain amount of flocculent precipitation of bimetallic terpyridine cobalt-tungsten bimetallic polymer nanomaterials, use 5 ml of methanol to ultrasonically disperse, take two drops of methanol dispersion and drop them on the copper grid covered with ultra-thin carbon film dedicated for transmission electron microscopy , tested after drying on a desiccator at 60 degrees Celsius for 20 minutes, it was observed that the synthesized high molecular polymer existed in a fibrous form.

[0053] Scanning electron microscope (SEM) uses a very narrow electron beam to scan the sample, and produces various effects through the interaction between the electron beam and the sample. It can dire...

Embodiment 3

[0055] Energy dispersive X-ray spectroscopy (EDX) is realized by analyzing the characteristic X-ray wavelength and intensity of the elements emitted by the sample. The elements contained in the sample are determined according to the wavelength, and the relative content of the element is determined according to the intensity. According to the EDX diagram, the existence of Co element and W element can be clearly seen, and the analysis of the content can facilitate the follow-up work.

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Abstract

The invention discloses a bis-terpyridine based bi-metal polymer and a preparation method thereof. A bis-terpyridine based metal complex is obtained through a self-assembly reaction of a transition metal salt and a bis-terpyridine ligand compound, the bis-terpyridine based metal complex reacts with excessive WO4<2-> solution, so as to obtain the bis-terpyridine based bi-metal polymer with high stability and high catalytic activity, and the polymer has wide application prospects in the field of catalysis.

Description

technical field [0001] The invention relates to a metal organic polymer catalytic material, in particular to a fibrous bis-terpyridine-based bimetallic polymer material and a synthesis method thereof, belonging to the technical field of catalytic materials. Background technique [0002] In chemical reactions, catalysis is widely used, which can increase the rate of chemical reactions and shorten the reaction time. In the field of catalysis, the research value of catalytic oxygen generation is particularly important. At present, organometallic polymer catalytic materials are mostly reported. Terpyridine is a good tridentate ligand, which can coordinate with some transition metal ions to obtain metallopolymer catalytic materials based on terpyridine ligand. For example, the literature (Energy & Environmental Science, 2012, 5, 7903–7907) reported that cobalt complexes of terpyridine derivatives can be used for water oxidation and hydrogen production, which belong to small mole...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G83/00B01J31/22
CPCB01J31/1691B01J2531/0244B01J2531/66B01J2531/845C08G83/008
Inventor 王平山刘海生刘叠
Owner CENT SOUTH UNIV
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