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Preparation method of transition metal complex based on mixed N,O-ligand, crystal structure and application thereof

A technology of transition metals and transition metal ions, applied in organic compound/hydride/coordination complex catalysts, 1/11 group organic compounds without C-metal bonds, separation methods, etc., to achieve stable product performance and high yield High, repeatable results

Inactive Publication Date: 2017-05-31
JILIN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the co-introduction of 2-HNCP and another multifunctional ligand pyridine-3-carboxylic acid (abbreviated as 3-Hpyc) containing N,O-coordinating atoms into transition metal complexes has not been reported yet.

Method used

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  • Preparation method of transition metal complex based on mixed N,O-ligand, crystal structure and application thereof
  • Preparation method of transition metal complex based on mixed N,O-ligand, crystal structure and application thereof
  • Preparation method of transition metal complex based on mixed N,O-ligand, crystal structure and application thereof

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Embodiment 1

[0020] The chemical formula described in the present invention is C 26 h 15 N 5 o 4 Complexes of Zn [Zn(2-NCP)(3-pyc)] n The preparation method is as follows:

[0021] To Zn(NO 3 ) 3 ·6H 2 To the mixed reagent of O (0.0296g, 0.1mmol), 2-HNCP (0.0170g, 0.05mmol) and 3-Hpyc (0.0123g, 0.1mmol), add 10mL of deionized water and stir for 10min, adjust with 1mol / L NaOH solution To pH = 6.5, put in a 25mL polytetrafluoroethylene reactor, heat to 170°C for 3 days, gradually cool to room temperature, wash with deionized water and dry at room temperature to obtain yellow blocky crystals, which are transition metal Zn complexes , the yield was 56% (based on metal Zn salt). Elemental analysis: (theoretical value): C 59.27, H 2.87, N 13.29; (experimental value): C 59.22, H 2.99, N 13.25.

[0022] Relevant characterization of complexes

[0023] (1) Crystal structure determination of transition metal Zn complexes

[0024] The diffraction data of the complexes were collected on a Br...

Embodiment 2

[0030] The chemical formula described in the present invention is C 26 h 15 N 5 o 4 Cu complex [Cu(2-NCP)(3-pyc)] n The preparation method is as follows:

[0031] to CuCl 2 2H 2 To the mixed reagent of O (0.0170g, 0.1mmol), 2-HNCP (0.0340g, 0.1mmol) and 3-Hpyc (0.0123g, 0.1mmol), add 12mL of deionized water and stir for 8min, then use 0.5mol / L NaOH solution Adjust the pH to 7, put it in a 25mL polytetrafluoroethylene reactor, heat to 160°C for 3 days, gradually cool to room temperature, wash with deionized water and dry at room temperature to obtain green blocky crystals, which are transition metal Cu complexes. product with a yield of 48% (based on metal Cu salt). Elemental analysis: (theoretical): C, 59.48; H, 2.88; N, 13.34. (Experimental values): C, 59.40; H, 2.91; N, 13.30.

[0032] The crystal structure determination of transition metal Cu complexes is the same as that of transition metal Zn complexes. Detailed crystallographic data are shown in Table 1; import...

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Abstract

The invention relates to a preparation method of a transition metal complex based on mixed N,O-ligand, a crystal structure and an application thereof. The molecular formula of the transition metal complex is [M(2-NCP)(3-pyc)]n. The preparation method comprises the following steps: mixing bivalent transition metal salt, 2-HNCP and 3-Hpyc in a substance amount ratio of 1:(0.5-1.5):(0.5-1.5); adding a certain amount of water and stirring for a period of time; regulating the pH to 5-8 with a NaOH solution; transferring the mixed solution into a reaction kettle with a polytetrafluoroethylene lining; reacting for a period of time at 140-180 DEG C; gradually cooling to room temperature; and washing the product with water and airing at room temperature to obtain a bulk crystal which is the transition metal complex. The complex provided by the invention is applied to luminous materials, magnetic materials, catalytic synthesis, selective adsorption and separation of the gases such as H2, N2, CO2, CH4 and O2 as well as the selective adsorption, separation and photocatalytic degradation of organic dye and phenol endocrine disrupters.

Description

technical field [0001] The invention belongs to the field of complex science and technology, in particular to a compound based on 2-(2-carboxyphenyl)imidazo(4,5-f)(1,10)-phenanthroline and pyridine-3-carboxylic acid Mixed N,O-ligand transition metal complexes, preparation methods, crystal structures and applications. Background technique [0002] The diverse structures and unique functional properties of the complexes have outstanding performance in the fields of light, electricity, magnetism, selective catalysis, gas adsorption and separation, and gas storage (G.Lu, J.T.Hupp, J.Am.Chem. Soc.2010, 132, 7832; Y.C.Pan, Z.P.Lai, Chem.Commun.2011, 47, 10275; H.Wang, W.T.Yang, Z.M.Sun, Chemistry2013, 8, 982; M.H.Zeng, Z.Yin, Y.X.Tan, W.X.Zhang , Y.P.He, M.Kurmoo, J.Am.Chem.Soc.2014, 136, 4680; R.Tania, V.D.Marion, G.P.Elena, S.C.Pablo, Z.Beatriz, K.Freek, G.Jorge, Adv.Funct .Mater.2014,24,249; N,L.Torad,M.Hu,S.Ishihara,H.Sukegawa,A.A.Belik,M.Imura,K.Ariga,Y.Sakka,Y.Yamauchi,Sma...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F3/06C07F1/08B01J31/22C09K11/06B01D53/02H01F1/42
CPCB01D53/02H01F1/42C09K11/06C07F1/005C07F3/06B01J31/2217C07B2200/13B01J2531/16B01J2531/26C09K2211/188B01J35/39Y02P20/151
Inventor 车广波周艳凤乔宇王炫博胡博
Owner JILIN NORMAL UNIV
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