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.

Inactive Publication Date: 2012-06-27
BOHAI UNIV
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  • Abstract
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Problems solved by technology

However, the synthesis of such complexes is restricted by the number of coordination sites, coordination ability, and interdentate spacing of organic ligands, and it is difficult to synthesize such multi-acid-based inorganic-organic functional complexes.
In addition, the nitrogen-containing ligands currently used to synthesize polyacid-based organic-inorganic complexes generally use imidazole, pyridine and other derivatives linked by hydrocarbon structural units. It is

Method used

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  • Copper complex based on dipyridine bisamide organic ligand and Keggin type polyoxometalate, its synthetic method and its application
  • Copper complex based on dipyridine bisamide organic ligand and Keggin type polyoxometalate, its synthetic method and its application
  • Copper complex based on dipyridine bisamide organic ligand and Keggin type polyoxometalate, its synthetic method and its application

Examples

Experimental program
Comparison scheme
Effect test

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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Abstract

The invention relates to a copper complex based on a dipyridine bisamide organic ligand and Keggin type polyoxometalate, its synthetic method and its application. A molecular formula is one of the following formulas: [Cu2(L<1>)3(H2O)6(SiMo12O40)].2H2O; [Cu2(L<2>)3(H2O)6(SiMo12O40)].9H2O; [Cu2(L<2>)3(H2O)6(SiW12O40)].6H2O; [Cu2(L<3>)3(H2O)6(SiMo12O40)].6H2O; [Cu2(L<3>)3(H2O)6(SiW12O40)].6H2O; wherein L<1> is N, N'-di(3- pyridylformamido)-1,2-ethane; L<2> is N, N'-di(3-pyridylformamido)-1,4-butane; L<3> is N, N'-di(3-pyridylformamido)-1,6-hexane. The method comprises the following steps: addingdeionized water in the Cu(NO3).3H2O, Keggin type polyoxometalate, dipyridine diamide organic ligand, stirring under room temperature, regulating pH value, dumping in a high pressure reaction vessel and heating, insulating under hydrothermal condition, cooling to the room temperature to obtain bulk blue green crystals, alternatively cleaning by deionized water and ethanol, naturally drying under room temperature to prepare the copper complex based on dipyridine bisamide organic ligand and Keggin type polyoxometalate. The complex has the advantages of simple synthetic method, easy crystallization, high synthesis yield, strong affinity capability to water-soluble pollutants and good catalytic degradation effect, and can be used as photocatalysis materials.

Description

technical field [0001] The invention belongs to a photocatalytic material and a synthesis method, in particular to a copper complex based on a bispyridine bisamide organic ligand and a Keggin type polyacid, and a synthesis method and application thereof. Background technique [0002] Polyacid-based inorganic-organic functional complexes are inorganic functional materials, which have the characteristics of diverse structures, good catalytic performance and wide application range. However, the synthesis of such complexes is restricted by the number of coordination sites, coordination ability, and interdentate spacing of organic ligands, and it is difficult to synthesize such multi-acid-based inorganic-organic functional complexes. In addition, the nitrogen-containing ligands currently used to synthesize polyacid-based organic-inorganic complexes generally use imidazole, pyridine and other derivatives linked by hydrocarbon structural units. It is relatively difficult to crysta...

Claims

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Application Information

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IPC IPC(8): B01J31/22C02F1/32C02F101/38
Inventor 王秀丽刘国成徐闯林宏艳张巨文田爱香
Owner BOHAI UNIV
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