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Transition metal compounds based on semi-rigid, synthetic method and applications

A technology of methyl isophthalic acid and bispyridine bisamide, applied in the direction of organic compound/hydride/coordination complex catalysts, chemical instruments and methods, cobalt organic compounds, etc., can solve the problem of poor catalytic degradation effect and catalytic ability Limitations, poor affinity for organic pollutants, etc., to achieve the effect of increasing flexibility, good catalytic performance, and increasing hydrophilicity

Inactive Publication Date: 2014-04-09
BOHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

Although some transition metal complex materials with excellent properties and novel structures have been synthesized by hydrothermal technology so far, not only transition metal ions will affect the structure and performance of such hybrid materials, but also nitrogen-containing heterocyclic ligands The change of species is also an important factor determining the final structure and performance of functional complexes. The inherent structural characteristics of nitrogen-containing heterocyclic ligands will restrict the synthesis of such functional complexes, such as ligand flexibility, ligand length, coordination The number of points, etc.; therefore, it is still difficult to effectively design and synthesize complex materials with specific functions
[0003] At present, among the nitrogen-containing heterocyclic organic ligands used to construct transition metal functional complexes, ligands containing pyridine groups account for the largest proportion, but the pyridine functional group only plays a role in coordinating with transition metals, resulting in the formation of The complex is hydrophobic, so it has poor affinity for water-soluble organic pollutants and poor catalytic degradation effect
In addition, the known functional complexes as photocatalysts usually have a good degradation ability to a specific organic pollutant in wastewater, but cannot catalyze multiple organic pollutants at the same time, and the catalytic ability has limitations.

Method used

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  • Transition metal compounds based on semi-rigid, synthetic method and applications
  • Transition metal compounds based on semi-rigid, synthetic method and applications
  • Transition metal compounds based on semi-rigid, synthetic method and applications

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0071] Example 1 Synthesis of [Cu(3-bpah)(5-MIP)]·2H 2 O, where 3-bpah is N , N '-bis(3-pyridinecarboxamide)-1,2-cyclohexane, the structural formula is: , 5-MIP is 5-methylisophthalic acid

[0072] 0.1mmol CuCl 2 2H 2 O, 0.10mmol N , N '-bis(3-pyridinecarboxamide)-1,2-cyclohexane, 0.10mmol 5-methylisophthalic acid and 7.8mL 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 6.4 with 0.1mol / L NaOH solution, it was transferred to a 25mL autoclave. The heating rate was increased to 130°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 blue blocky crystals, which were washed alternately with deionized water and ethanol for 3 times, and naturally dried at room temperature Dry to get [Cu(3-bpah)(5-MIP)]·2H 2 O, the productive rate is 30%...

Embodiment 2

[0073] Example 2 Synthesis of [Cu(3-bpah)(5-MIP)]·2H 2 O, where 3-bpah is N , N '-bis(3-pyridinecarboxamide)-1,2-cyclohexane, 5-MIP as 5-methylisophthalic acid

[0074] 0.1mmol CuCl 2 2H 2 O, 0.10mmol N , N '-bis(3-pyridinecarboxamide)-1,2-cyclohexane, 0.15mmol 5-methylisophthalic acid and 8.0mL H 2O was sequentially added to a 25mL beaker, and stirred at room temperature for 40min to obtain a suspension mixture. After adjusting the pH of the suspension mixture to 6.7 with 0.1mol / L NaOH solution, it was transferred to a 25mL autoclave and heated at 15°C / h Raise the temperature to 110°C, keep it warm for 96 hours under hydrothermal conditions, then lower the temperature to room temperature at a cooling rate of 5°C / h to obtain blue blocky crystals, wash them alternately with deionized water and ethanol for 5 times, and dry them naturally at room temperature , to get [Cu(3-bpah)(5-MIP)]·2H2O, the productive rate is 33%, and its XRD diffraction pattern is as figure 1 As s...

Embodiment 3

[0075] Example 3 Synthesis of [Cu(3-bpah)(5-MIP)]·2H 2 O, where 3-bpah is N , N '-bis(3-pyridinecarboxamide)-1,2-cyclohexane, 5-MIP as 5-methylisophthalic acid

[0076] 0.2mmol CuCl 2 2H 2 O, 0.10mmol N , N '-bis(3-pyridinecarboxamide)-1,2-cyclohexane, 0.2mmol 5-methylisophthalic acid and 8.0mL H 2 O was sequentially added to 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 7.0 with 0.1mol / L NaOH solution, it was transferred to a 25mL autoclave. The heating rate was increased to 120°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 blue blocky crystals, which were washed twice with deionized water and ethanol alternately, and naturally dried at room temperature Dry to get [Cu(3-bpah)(5-MIP)]·2H 2 O, the productive rate is 39%, and its XRD diffraction pattern is a...

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Abstract

Provided are a The molecular formulas are as follows: [Cu(3-bpah)(5-MIP)].2H20; [Ni(3-bpah)(5-MIP)].H20; [Co(3-bpah)(5-MIP)].H20; [Cu(4-bpah)(5-MIP)(H20)]; [Ni(4-bpah)(5-MIP)(H20)].H2O; [Co(4-bpah)(5-MIP)]. Transition metal chlorides, semi-rigid bispyridine bisamide ligands and 5-methyl isophthalic acid are added into deionized water, after pH adjustment, the above mixture is reacted under hydrothermal conditions, and products are obtained. The transition metal compounds are advantageous in that the transition metal compounds have a simple synthetic method, have strong affinity to organic pollutants of methylene blue, methyl orange and rhodamine B, and have good catalytic degradation effects.

Description

technical field [0001] The invention belongs to the field of photocatalytic materials and synthesis methods, and in particular relates to a transition metal complex based on semi-rigid bispyridine bisamide ligand and 5-methylisophthalic acid and its synthesis method and application. Background technique [0002] The transition metal functional complex based on the mixed ligands of oxygen-containing organic carboxylic acid ligands and nitrogen-containing organic heterocyclic ligands is an inorganic-organic functional hybrid material with rich and diverse structures, good catalytic performance, and a wide range of applications. broad features. Although some transition metal complex materials with excellent properties and novel structures have been synthesized by hydrothermal technology so far, not only transition metal ions will affect the structure and performance of such hybrid materials, but also nitrogen-containing heterocyclic ligands The change of species is also an imp...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F1/08C07F15/04C07F15/06B01J31/22
Inventor 王秀丽林宏艳刘国成栾健田爱香张巨文
Owner BOHAI UNIV
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