Copper complex based on dipyridine bisamide organic ligand and Keggin type polyoxometalate, its synthetic method and its application
A bispyridine bisamide, organic ligand technology, applied in organic compound/hydride/coordination complex catalysts, chemical instruments and methods, water pollutants, etc., can solve the problem of poor catalytic degradation effect of water-soluble organic pollutants, The problems of poor affinity and low synthesis yield can achieve the effect of good catalytic degradation effect, strong affinity and improved synthesis yield.
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Embodiment 1
[0039] Example 1 Synthesis of [Cu 2 (L 1 ) 3 (H 2 O) 6 (SiMo 12 O 40 )] 2H 2 O, where L 1 is N,N'-bis(3-pyridinecarboxamido)-1,2-ethane
[0040] 0.1 mmol N,N'-bis(3-pyridinecarboxamido)-1,2-ethane, 0.13 mmol H 4 SiMo 12 O 40 ·29H 2 O, 0.5mmol Cu(NO 3 ) 3H 2 O and 10 mL H 2 O was added to a 50mL beaker in turn, stirred at room temperature for 30min, adjusted the pH to 5.5 with a 1.0mol / L NaOH solution, poured into a 25mL autoclave, heated to 120°C at a heating rate of 20°C / hour, and heated with water. The temperature was lowered to room temperature at a cooling rate of 5 °C / hour for 3 days, to obtain blue-green massive crystals, which were alternately washed with deionized water and ethanol twice, and dried naturally at room temperature to obtain [Cu 2 (L 1 ) 3 (H 2 O) 6 (SiMo 12 O 40 )] 2H 2 O, the yield is 64%, and its coordination environment diagram is as follows Figure 5 shown, the stacking diagram is as follows Image 6 shown.
Embodiment 2
[0041] Example 2 Synthesis of [Cu 2 (L 1 ) 3 (H 2 O) 6 (SiMo 12 O 40 )] 2H 2 O, where L 1 is N,N'-bis(3-pyridinecarboxamido)-1,2-ethane
[0042] 0.1 mmol N,N'-bis(3-pyridinecarboxamido)-1,2-ethane, 0.11 mmol H 4 SiMo 12 O 40 ·29H 2 O, 0.4 mmol Cu (NO 3 ) 3H 2 O and 8mL H 2 O was added to a 50 mL beaker in turn, stirred for 20 min at room temperature, adjusted to pH 4 with 0.5 mol / L NaOH solution, poured into a 25 mL autoclave, heated to 110 ° C at a heating rate of 20 ° C / hour, and water The temperature was lowered to room temperature at a cooling rate of 5 °C / hour for 4 days under thermal conditions to obtain blue-green bulk crystals, which were alternately washed with deionized water and ethanol for 3 times, and dried naturally at room temperature to obtain [Cu 2 (L 1 ) 3 (H 2 O) 6 (SiMo 12 O 40 )] 2H 2 O, the yield is 82%, and its coordination environment diagram is as follows Figure 5 shown, the stacking diagram is as follows Image 6 shown.
Embodiment 3
[0043] Example 3 Synthesis of [Cu 2 (L 1 ) 3 (H 2 O) 6(SiMo 12 O 40 )] 2H 2 O, where L 1 is N,N'-bis(3-pyridinecarboxamido)-1,2-ethane
[0044] 0.1 mmol N,N'-bis(3-pyridinecarboxamido)-1,2-ethane, 0.15 mmol H 4 SiMo 12 O 40 ·29H 2 O, 0.6 mmol Cu (NO 3 ) 3H 2 O and 12 mL H 2 O was added to a 50mL beaker in turn, stirred for 40min at room temperature, adjusted to pH 4.6 with 2.0mol / L NaOH solution, poured into a 25mL autoclave, heated to 130°C at a heating rate of 10°C / hour, hydrothermal conditions The temperature was lowered to room temperature at a cooling rate of 10 °C / hour for 5 days, and the blue-green massive crystals were washed alternately with deionized water and ethanol for 3 times, and air-dried at room temperature to obtain [Cu 2 (L 1 ) 3 (H 2 O) 6 (SiMo 12 O 40 )] 2H 2 O, the yield is 68%, and its coordination environment diagram is as follows Figure 5 shown, the stacking diagram is as follows Image 6 shown.
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