Hydrogen bond type rare-earth metal complexes and preparation method thereof
A technology of rare earth metals and rare earth metal ions, applied in botany equipment and methods, chemical instruments and methods, chemicals for biological control, etc., can solve the problems of low thermal stability and easy decomposition, and achieve antibacterial Effects of long aging, mild process conditions, and convenient operation
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Embodiment 1
[0045]Take by weighing yttrium chloride 0.1175g and be dissolved in 10mL water and make solution (A1), 0.3010g pyridine-2,6-dicarboxylic acid (pydcH 2 ) was dissolved in 30 mL of water at 80°C to prepare a solution (B1), and 0.1965 g of 2,6-diamino-pyridine (pyda) was dissolved in 10 mL of water to prepare a solution (C1).
[0046] The solution (B1) and the solution (C1) were mixed, stirred at 80° C. for 30 min, and then the solution (A1) was added dropwise thereto. After the above mixed solution was stirred for 4 h, it was allowed to stand at room temperature for 24 h. Filtrate, wash, and dry under vacuum at 60°C to obtain the hydrogen-bonded rare earth metal complex Y (pydc) 3 (pyda·H) 3 ·5H 2 O. With other rare earth metal ions RE 3+ replace Y 3+ , can be prepared according to the above general formula RE x M' y M" z ·nH 2 Hydrogen-bonding rare earth metal complexes of O.
Embodiment 2
[0048] (1) Ligand (pydc) 2- (pyda·H 2 ) 2+ Synthesis
[0049] A solution of 2,6-diamino-pyridine (pyda) (2.0 mmol) and triethylamine (4.0 mmol) in tetrahydrofuran (THF) (50 mL) was added dropwise to pyridine-2,6-dicarboxylic acid (pydcH 2 ) (2.0 mmol) in tetrahydrofuran (THF) (50 mL), stirred for 15 min. Then heated to reflux for 8h. After the reaction mixture was cooled, it was stirred at room temperature for 12 hours to obtain a yellow turbid liquid, which was left to stand, filtered, washed, and dried to obtain a yellow solid powder (pydc) 2- (pyda·H 2 ) 2+ .
[0050] (2) Preparation of rare earth complexes
[0051] Weigh 0.1655g of yttrium nitrate and dissolve it in 10mL water to make a solution (A2), weigh the above ligand (pydc) 2- (pyda·H 2 ) 2+ 0.4980g was stirred and dissolved in 30mL water at 60°C to prepare a solution (D2). Then solution A2 was added dropwise to solution D2, stirred at 60° C. for 4 h, and left standing at room temperature for 24 h. Filt...
Embodiment 3
[0053] Take by weighing yttrium nitrate 0.1655g and be dissolved in 10mL water and make solution (A3), take by weighing the part (pydc) among the embodiment 2 2- (pyda·H 2 ) 2+ 0.3324g was stirred and dissolved in 30mL water at 60°C to prepare a solution (D3). Then solution A3 was added dropwise to solution D3, stirred at 60° C. for 4 h, and allowed to stand at room temperature for 24 h. Filtrate, wash, and dry under vacuum at 60°C to obtain the hydrogen-bonded rare earth metal complex Y 2 (pydc) 4 (pyda·H) 2 10H 2 O. With other rare earth metal ions RE 3+ replace Y 3+ , can be prepared according to the above general formula RE x M' y M" z ·nH 2 Hydrogen-bonding rare earth metal complexes of O.
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