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Copper complex based on dipyridine piperazine ligand and Anderson type polyacid, and synthetic method and application thereof

A technology of bispyridine piperazine and bispyridine bispiperazine, which is applied in the field of photocatalytic materials and synthesis, can solve the problems of inability to achieve effective catalytic degradation, limited application range, poor affinity, etc., and achieve good stability and symmetry , Increase hydrophilicity and prevent secondary pollution

Inactive Publication Date: 2014-08-20
BOHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In addition, nitrogen-containing ligands used to construct polyacid-based metal-organic complexes generally use bisimidazole, bispyridine, bistriazole and other derivatives linked by alkane structural units. Such derivatives are hydrophobic, and the use of this It is relatively difficult to crystallize polyacid-based metal-organic complexes, requiring high hydrothermal temperatures (usually 150°C to 180°C), and low yields (about 40%)
At the same time, polyacid-based metal-organic complex materials based on bisimidazole, bispyridine, bistriazole and other derivatives of alkane structural units have poor affinity for water-soluble organic pollutants, and have poor affinity for water-soluble organic pollutants. Catalytic degradation of compounds can only be carried out under UV light irradiation
At present, the application of polyacid-based metal-organic complex materials in photocatalysis is limited to the ability to degrade a specific organic pollutant under ultraviolet light irradiation, but cannot achieve effective catalytic degradation under visible light irradiation and sunlight. purpose, which severely limits its scope of application

Method used

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  • Copper complex based on dipyridine piperazine ligand and Anderson type polyacid, and synthetic method and application thereof
  • Copper complex based on dipyridine piperazine ligand and Anderson type polyacid, and synthetic method and application thereof
  • Copper complex based on dipyridine piperazine ligand and Anderson type polyacid, and synthetic method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0066] Example 1 Synthesis of H[Cu 2 L 1 Cr(OH) 6 Mo 6 o 18 (μ 2 -OH) 2 ]·4H 2 O, where L 1 for N , N '-bis(3-pyridineformyl)piperazine, the structural formula is:

[0067] 0.2mmol CuCl 2 2H 2 O, 0.10mmol N , N '-bis(3-pyridineformyl)piperazine, 0.10mmol Na 3 [CrMo 6 h 6 o 24 ]·8H 2 O and 7.0 mL H 2 O was sequentially added into a 25mL beaker, and stirred at room temperature for 20min to obtain a suspension mixture. After the pH of the suspension mixture was adjusted to 3.0 with 0.5mol / L HCl solution, it was transferred to a 25mL autoclave. The heating rate was increased to 120°C, and the temperature was kept for 24 hours under hydrothermal conditions, and the temperature was lowered to room temperature at a cooling rate of 5°C / h to obtain dark green blocky crystals, which were washed alternately with deionized water and ethanol for 4 times, and naturally dried at room temperature Dry, get H[Cu 2 L 1 Cr(OH) 6 Mo 6 o 18 (μ 2 -OH) 2 ]·4H 2 O, the pr...

Embodiment 2

[0068] Example 2 Synthesis of H[Cu 2 L 1 Cr(OH) 6 Mo 6 o 18 (μ 2 -OH) 2 ]·4H 2 O, where L 1 for N , N '-Bis(3-pyridinecarbonyl)piperazine

[0069] 0.4mmol Cu(NO 3 ) 2 ·3H 2 O, 0.15mmol N , N '-bis(3-pyridineformyl)piperazine, 0.20mmol Na 3 [CrMo 6 h 6 o 24 ]·8H 2 O and 11.0 mL H 2 O was sequentially added into a 25mL beaker, and stirred at room temperature for 10min to obtain a suspension mixture. After the pH of the suspension mixture was adjusted to 3.5 with 1.0mol / L HCl solution, it was transferred to a 25mL autoclave. The heating rate was increased to 110°C, and the temperature was kept for 72 hours under hydrothermal conditions, and the temperature was lowered to room temperature at a cooling rate of 5°C / h to obtain dark green blocky crystals, which were washed twice with deionized water and ethanol alternately, and naturally dried at room temperature Dry, get H[Cu 2 L 1 Cr(OH) 6 Mo 6 o 18 (μ 2 -OH) 2 ]·4H 2 O, the productive rate is 56%, and ...

Embodiment 3

[0070] Example 3 Synthesis of H[Cu 2L 1 Cr(OH) 6 Mo 6 o 18 (μ 2 -OH) 2 ]·4H 2 O, where L 1 for N , N '-Bis(3-pyridinecarbonyl)piperazine

[0071] 0.5mmol CuCl 2 2H 2 O, 0.10mmol N , N '-bis(3-pyridineformyl)piperazine, 0.30mmol Na 3 [CrMo 6 h 6 o 24 ]·8H 2 O and 15.0 mL H 2 O was sequentially added to a 25mL beaker, and stirred at room temperature for 30min to obtain a suspension mixture. After the pH of the suspension mixture was adjusted to 4.0 with 1.5mol / L HCl solution, it was transferred to a 25mL autoclave. The heating rate was increased to 120°C, and the temperature was kept for 96 hours under hydrothermal conditions, and the temperature was lowered to room temperature at a cooling rate of 2.5°C / h to obtain dark green blocky crystals, which were washed alternately with deionized water and ethanol for 3 times, and naturally dried at room temperature Dry, get H[Cu 2 L 1 Cr(OH) 6 Mo 6 o 18 (μ 2 -OH) 2 ]·4H 2 O, the productive rate is 64%, and it...

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Abstract

A copper complex based on dipyridine piperazine organic ligand and Anderson type polyacid, and a synthesis method and application thereof. The molecular formula of the complex is one selected from the followings: H[Cu2L1Cr(OH 6Mo6O18 (mu2-OH)2].4H2O, and [Cu2L2Cr(OH)6MoVI5MoVO18 (H2O)4].4H2O. The method is as below: adding copper salt, Anderson type polyacid, and dipyridine piperazine organic ligand into deionized water, stirring at room temperature, adjusting the pH value, insulating under hydrothermal conditions in a high-pressure reaction kettle, cooling to room temperature to produce massive dark green crystals, cleaning and drying, so as to prepare the copper complex based on dipyridine piperazine organic ligand and Anderson type polyacid. The synthetic method of the complex is simple, easy for crystallization and high in synthesis yield, the complex has strong affinity and good photocatalytic degradation effect on water-soluble pollutants, and can be used as photocatalytic materials.

Description

technical field [0001] The invention belongs to the field of photocatalytic materials and synthesis methods, and in particular relates to a copper complex based on bispyridine piperazine ligand and Anderson polyacid and its synthesis method and application. technical field [0002] The invention belongs to the field of photocatalytic materials and synthesis methods, and in particular relates to a copper complex based on bispyridine piperazine ligand and Anderson polyacid and its synthesis method and application. Background technique [0003] Polyacid-based metal-organic functional complexes are a kind of inorganic-organic functionalized hybrid materials, which have the characteristics of complex and diverse structures, good catalytic performance and wide application range. Although hydrothermal synthesis techniques have been successfully applied to the preparation of such materials, it is still a challenging task to effectively design and synthesize polyacid-based comple...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F1/08B01J31/22A62D3/17A62D101/26A62D101/28
Inventor 王秀丽林宏艳刘国成常之晗田爱香张巨文
Owner BOHAI UNIV
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