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Rare earth complex based on 2-HNCP and pyridine-3-carboxylic acid as mixed ligands, preparation method, structure and application of rare earth complex

A technology of rare earth complexes and mixed ligands, applied in organic compound/hydride/coordination complex catalysts, chemical instruments and methods, separation methods, etc., to achieve stable product performance, high yield, and strong repeatability

Inactive Publication Date: 2017-08-11
JILIN NORMAL UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

According to research, so far, rare earth complexes constructed with 2-HNCP and pyridine-3-carboxylic acid (abbreviated as 3-Hpyc) as mixed ligands have not been reported.

Method used

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  • Rare earth complex based on 2-HNCP and pyridine-3-carboxylic acid as mixed ligands, preparation method, structure and application of rare earth complex
  • Rare earth complex based on 2-HNCP and pyridine-3-carboxylic acid as mixed ligands, preparation method, structure and application of rare earth complex
  • Rare earth complex based on 2-HNCP and pyridine-3-carboxylic acid as mixed ligands, preparation method, structure and application of rare earth complex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0021] The chemical formula described in the present invention is C 46 h 26 N 9 o 6 Rare earth Pr complexes of Pr [Pr(2-NCP) 2 (3-pyc)] n The preparation method is as follows:

[0022] Pr(NO 3 ) 3 ·6H 2O (0.087g, 0.2mmol), 2-HNCP (0.0340g, 0.1mmol) and 3-Hpyc (0.0123g, 0.1mmol), add deionized water 10mL and stir for 10min, adjust the pH to 6.5 with 1mol / L NaOH solution, Put in a 25mL polytetrafluoroethylene reactor, heat to 180°C, react for 3 days, gradually cool to room temperature, wash with deionized water and dry at room temperature to obtain yellow blocky crystals, which are rare earth Pr complexes, with a yield of 52 % (based on Pr). Theoretical values ​​(%) of elemental analysis: C 58.67, H 2.78, N 13.39; experimental values ​​(%): C 58.31, H 2.80, N 13.32.

[0023] Relevant characterization of complexes

[0024] (1) Crystal structure determination of rare earth Pr complexes

[0025] The diffraction data of the complexes were collected on an Oxford Diffracti...

Embodiment 2

[0030] The chemical formula described in the present invention is C 46 h 26 N 9 o 6 Rare earth La complexes of La [La(2-NCP) 2 (3-pyc)] n The preparation method is as follows:

[0031] LaCl 3 ·6H 2 O (0.0706g, 0.2mmol), 2-HNCP (0.0680g, 0.2mmol) and 3-Hpyc (0.0246g, 0.2mmol), add deionized water 10mL and stir for 15min, adjust the pH to 7 with 1.1mol / L NaOH solution , placed in a 25mL polytetrafluoroethylene reactor, heated to 170°C, reacted for 3 days, gradually cooled to room temperature, washed with deionized water and dried at room temperature to obtain yellow blocky crystals, selected suitable crystals for X-ray single crystallization Diffraction analysis (49% yield based on metal La). Elemental analysis: (theoretical value): C, 58.80; H, 2.79; N, 13.42; (experimental value): C, 58.48; H, 2.82; N, 13.34.

[0032] The crystal structure determination of the rare earth La complex is the same as that of the Pr complex. Detailed crystallographic data are shown in Tab...

Embodiment 3

[0035] The synthetic chemical formula is C 46 h 26 N 9 o 6 Rare earth complexes of Nd [Nd(2-NCP) 2 (3-pyc)] n :

[0036] Nd(CH 3 COO) 3 2H 2 O (0.0357g, 0.1mmol), 2-HNCP (0.0680g, 0.2mmol) and 3-Hpyc (0.0185g, 0.15mmol), add deionized water 12mL and stir for 8min, adjust the pH to 6 with 0.7mol / L NaOH solution, Place in a 25mL polytetrafluoroethylene reactor, heat to 160°C, react for 3 days, gradually cool to room temperature, wash with deionized water and dry at room temperature to obtain yellow blocky crystals, select suitable crystals for X-ray single crystal diffraction Analysis (45% yield based on metal Nd). Elemental analysis: (theoretical value): C, 58.47; H, 2.77; N, 13.34; (experimental value): C, 58.15; H, 2.81; N, 13.27.

[0037] The crystal structure determination of rare earth Nd complexes is the same as that of Pr complexes. Detailed crystallographic data are shown in Table 1; important bond length and bond angle data are shown in Table 2; the crystal ...

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Abstract

The invention relates to a rare earth complex based on 2-HNCP and pyridine-3-carboxylic acid as mixed ligands, a preparation method, a crystal structure and an application of the rare earth complex. The molecular formula of the rare earth complex is [RE(2-NCP)2(3-pyc)]n. According to the preparation method, trivalent rare-earth salt, 2-HNCP and pyridine-3-carboxylic acid are mixed in the substance ratio being 1:(0.5-1.5):(0.5-1.5), a certain amount of water is added, the mixture is stirred for a period of time, pH of the mixture is regulated to be 5-8 with an NaOH solution, then the mixed solution is transferred to a reactor with a polytetrafluoroethylene liner, subjected to a reaction in a temperature range of 140-180 DEG C for a period of time and then cooled gradually to room temperature, a product is washed with water and aired at room temperature, and obtained bulk crystals are the rare earth complex. The rare earth complex is applied to aspects of catalysis of organic synthesis, selective adsorption and separation of CO2, CH4, H2, N2, O2 and other gas as well as selective adsorption, separation and photocatalytic degradation of organic dyes and phenolic endocrine disruptors. The synthetic method has the characteristics of high repeatability, high yield, stable product performance and the like.

Description

technical field [0001] The invention belongs to the field of complex science and technology, and in particular relates to a rare earth complex based on 2-HNCP and pyridine-3-carboxylic acid as mixed ligands, a preparation method, a crystal structure and an application thereof. Background technique [0002] The complex is a new type of functional material with a periodic structure. Most of the complexes are formed by the coordination of metal ions and multifunctional organic ligands. Because such materials generally have the characteristics of large specific surface area, porosity, and diverse structures, they are widely used in catalysis, magnetism, gas storage and separation, and luminescent materials (J.M.Zhou, H.M.Li, N.Xu, P.Cheng, Inorg.Chem. Commun.2013, 37, 30; B.Liu, W.P.Wu, L.Hou, Y.Y.Wang, Chem.Commun.2014, 50, 8731; X.Zhao, X.Y.Yu, T.L.Chen, Y.H.Luo, J.J.Yang, H. Zhang, Inorg.Chem.Commun.2012, 20, 247) and other fields have a wide range of applications. [0003...

Claims

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Application Information

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IPC IPC(8): C08G83/00B01J31/22B01D53/02
CPCB01D53/02B01D2257/102B01D2257/104B01D2257/108B01D2257/504B01D2257/7025B01J31/2217B01J2531/37B01J2531/38C08G83/008Y02C20/20Y02C20/40Y02P20/151
Inventor 乔宇周艳凤车广波胡博王炫博
Owner JILIN NORMAL UNIV
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