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Cobalt complex based on flexible bipyridine bisamide ligand and benzenedicarboxylic acid, synthesis method and application thereof

A bispyridine bisamide, cobalt complex technology, applied in the direction of organic compound/hydride/coordination complex catalyst, cobalt organic compound, chemical instruments and methods, etc., to speed up the crystallization process, reduce power consumption, improve synthesis yield. rate effect

Inactive Publication Date: 2014-07-23
BOHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] Transition metal functional complexes based on benzenedicarboxylic acid and organic amine mixed ligands can be synthesized by hydrothermal synthesis, but due to various factors such as reaction time, temperature, ligand type, raw material ratio, system pH value, etc. The synthesis of the target complex and its final structure have an important impact, so it is still a challenging task to effectively design and synthesize complex materials with novel structures and specific functions

Method used

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  • Cobalt complex based on flexible bipyridine bisamide ligand and benzenedicarboxylic acid, synthesis method and application thereof
  • Cobalt complex based on flexible bipyridine bisamide ligand and benzenedicarboxylic acid, synthesis method and application thereof
  • Cobalt complex based on flexible bipyridine bisamide ligand and benzenedicarboxylic acid, synthesis method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0058] Example 1 Synthesis of [Co( L 1 ) 0.5 (5-AIP)], where, L 1 for N , N '-bis(3-pyridine)-succinamide, the structural formula is: , 5-AIP is 5-aminoisophthalate

[0059] 0.1mmol CoCl 2 ·6H 2 O, 0.10mmol N , N '-bis(3-pyridine)-succinamide, 0.10mmol 5-aminoisophthalic acid and 7.5mL H 2 O was sequentially added to a 25mL beaker, and stirred at room temperature for 20min to obtain a suspension mixture. After adjusting the pH of the suspension mixture to 6.8 with 0.1mol / L NaOH solution, it was transferred to a 25mL autoclave. The heating rate was increased to 110°C, and the temperature was kept for 48 hours under hydrothermal conditions, and the temperature was lowered to room temperature at a cooling rate of 5°C / h to obtain pink blocky crystals, which were washed alternately with deionized water and ethanol for 4 times, and dried naturally at room temperature , get [Co(L 1 ) 0.5 (5-AIP)], productive rate is 45%, and its XRD diffraction pattern is as figure 1...

Embodiment 2

[0060] Example 2 Synthesis of [Co( L 1 ) 0.5 (5-AIP)], where, L 1 for N , N '-Bis(3-pyridine)-succinamide, 5-AIP as 5-aminoisophthalate

[0061] 0.2mmol CoCl 2 ·6H 2 O, 0.10mmol N , N '-bis(3-pyridine)-succinamide, 0.15mmol 5-aminoisophthalic acid and 9.0mL H 2 O was sequentially added to a 25mL beaker, and stirred at room temperature for 30min to obtain a suspension mixture. After adjusting the pH of the suspension mixture to 7.2 with 0.1mol / L NaOH solution, it was transferred to a 25mL autoclave and heated at 5°C / h The temperature was raised to 120°C, kept under hydrothermal conditions for 96 hours, and the temperature was lowered to room temperature at a cooling rate of 15°C / h to obtain pink blocky crystals, which were washed alternately with deionized water and ethanol for 3 times, and dried naturally at room temperature. get [Co( L 1 ) 0.5 (5-AIP)], productive rate is 69%, and its XRD diffraction pattern is as figure 1 As shown, the coordination environmen...

Embodiment 3

[0062] Example 3 Synthesis of [Co( L 1 ) 0.5 (5-AIP)], where, L 1 for N , N '-Bis(3-pyridine)-succinamide, 5-AIP as 5-aminoisophthalate

[0063] 0.3mmol CoCl 2 ·6H 2 O, 0.10mmol N , N '-bis(3-pyridine)-succinamide, 0.10mmol 5-aminoisophthalic acid and 11.0mL H 2 O was sequentially added to a 25mL beaker, stirred at room temperature for 10min to obtain a suspension mixture, adjusted the pH of the suspension mixture to 7.4 with 1mol / L NaOH solution, then transferred to a 25mL autoclave, and heated at 10°C / h The temperature was raised to 130°C, kept under hydrothermal conditions for 72 hours, and the temperature was lowered to room temperature at a cooling rate of 10°C / h to obtain pink blocky crystals, which were washed twice with deionized water and ethanol alternately, and dried naturally at room temperature. get [Co( L 1 ) 0.5 (5-AIP)], productive rate is 58%, and its XRD diffraction pattern is as figure 1 As shown, the coordination environment diagram is shown...

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Abstract

The invention relates to a cobalt complex based on a flexible bipyridine bisamide ligand and benzenedicarboxylic acid, a synthesis method and application thereof. The molecular formula of the cobalt complex is: [Co(L<1>)0.5(5-AIP)]; [Co(L<3>)(5-AIP)]; [Co2(L<1>)2(1, 3-BDC)2].4H2O; and [Co2(L<2>)1.5(1, 2-BDC) (mu2-OH)(mu3-OH)(H2O)].H2O. The synthesis method includes: adding cobalt chloride, the flexible bipyridine bisamide ligand and benzenedicarboxylic acid into deionized water, adjusting the pH value, pouring the mixture into a high-pressure reaction kettle to undergo hydrothermal reaction, and carrying out washing and airing, thus obtaining the cobalt complex based on the flexible bipyridine bisamide ligand and benzenedicarboxylic acid. The cobalt complex provided by the invention has the advantages of: simple synthesis method, easy crystallization, high synthesis yield, strong affinity to water soluble pollutants, good catalytic degradation effect, and exhibition of anti-ferromagnetic coupling behavior, and can be applied as a photocatalytic material and magnetic material.

Description

technical field [0001] The invention belongs to the field of photocatalytic and magnetic materials and synthesis methods, and in particular relates to a cobalt complex based on flexible bispyridine bisamide ligand and benzenedicarboxylic acid and its synthesis method and application. Background technique [0002] Transition metal functional complexes based on mixed ligands of benzenedicarboxylic acid and organic amines are a kind of inorganic-organic hybrid materials. At present, rigid or semi-rigid organic amine ligands have attracted extensive attention from researchers of functional complex materials due to their relatively fixed length and easy synthesis. However, due to the relatively poor flexibility of rigid or semi-rigid ligands, the metal-organic complexes constructed by them have low dimensions and simple topology, which also limits the application of such complex crystal materials. At present, the application of bispyridine bisamide rigid or semi-rigid organic am...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/06B01J31/22H01F1/42
Inventor 林宏艳王秀丽刘国成隋芳芳张巨文田爱香
Owner BOHAI UNIV
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