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Transition metal complex based on semirigid bipyridine bisamide organic ligand and terephthalic acid as well as synthetic method and application of transition metal complex

A technology of bispyridine bisamide and terephthalic acid, applied in the fields of cadmium organic compounds, zinc organic compounds, chemical instruments and methods, etc.

Inactive Publication Date: 2014-04-16
BOHAI UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, there are few studies on the application of zinc and cadmium functional complexes in fluorescence selective molecular recognition and fluorescence sensors, especially the selective recognition and detection of environmental pollutants nitrobenzene has not been reported.

Method used

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  • Transition metal complex based on semirigid bipyridine bisamide organic ligand and terephthalic acid as well as synthetic method and application of transition metal complex
  • Transition metal complex based on semirigid bipyridine bisamide organic ligand and terephthalic acid as well as synthetic method and application of transition metal complex
  • Transition metal complex based on semirigid bipyridine bisamide organic ligand and terephthalic acid as well as synthetic method and application of transition metal complex

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0052] Example 1 Synthesis of [Zn(3-bpah)(1,4-BDC)]·H 2 O, where 3-bpah is N , N '-bis(3-pyridinecarboxamide)-1,2-cyclohexane, the structural formula is: , 1,4-BDC is terephthalate

[0053] 0.3mmol Zn(NO 3 ) 2 2H 2 O, 0.10mmol N , N '-bis(3-pyridinecarboxamide)-1,2-cyclohexane, 0.10 mmol terephthalic acid and 8.0 mL H 2 O was added to a 25mL beaker in turn, stirred at room temperature for 40min, adjusted to pH 6.5 with 0.1mol / L NaOH solution, poured into a 25mL autoclave, heated to 100°C at a heating rate of 5°C / h, and heated with water Under the condition of heat preservation for 48h, the temperature was lowered to room temperature at a cooling rate of 5°C / h to obtain colorless blocky crystals, which were dried naturally at room temperature to obtain [Zn(3-bpah)(1,4-BDC)]·H 2 O, the yield is 48%, and its coordination environment diagram is as follows Figure 4 As shown, its two-dimensional network diagram is shown as Figure 5 As shown, the simplified diagram of i...

Embodiment 2

[0054] Example 2 Synthesis of [Zn(3-bpah)(1,4-BDC)]·H 2 O, where 3-bpah is N , N '-bis(3-pyridinecarboxamide)-1,2-cyclohexane, 1,4-BDC as terephthalate

[0055] 0.2 mmol Zn(NO 3 ) 2 2H 2 O, 0.10mmol N , N '-bis(3-pyridinecarboxamide)-1,2-cyclohexane, 0.15 mmol terephthalic acid and 10.0 mL H 2 Add O to a 25mL beaker in turn, stir at room temperature for 30min, adjust the pH to 6.8 with 1mol / L NaOH solution, pour it into a 25mL autoclave, and raise the temperature to 110°C at a heating rate of 10°C / h. Keep it warm for 36 hours, and lower the temperature to room temperature at a cooling rate of 10 °C / h to obtain colorless blocky crystals, which are naturally dried at room temperature to obtain [Zn(3-bpah)(1,4-BDC)] H 2 O, the yield is 56%, and its coordination environment diagram is as follows Figure 4 As shown, its two-dimensional network diagram is shown as Figure 5 As shown, the simplified diagram of its two-dimensional skeleton structure is shown in Image 6 sho...

Embodiment 3

[0056] Example 3 Synthesis of [Zn(3-bpah)(1,4-BDC)]·H 2 O, where 3-bpah is N , N '-bis(3-pyridinecarboxamide)-1,2-cyclohexane, 1,4-BDC as terephthalate

[0057] 0.2 mmol Zn(NO 3 ) 2 2H 2 O, 0.10mmol N , N '-bis(3-pyridinecarboxamide)-1,2-cyclohexane, 0.15mmol terephthalic acid and 13.0mL H 2 Add O to a 25mL beaker in turn, stir at room temperature for 20min, adjust the pH to 7.2 with 2mol / L NaOH solution, pour it into a 25mL autoclave, and raise the temperature to 120°C at a heating rate of 5°C / h. Keep it warm for 24 hours, and lower the temperature to room temperature at a cooling rate of 10 °C / h to obtain colorless blocky crystals, which are naturally dried at room temperature to obtain [Zn(3-bpah)(1,4-BDC)] H 2 O, the yield is 66%, and its coordination environment diagram is as follows Figure 4 As shown, its two-dimensional network diagram is shown as Figure 5 As shown, the simplified diagram of its two-dimensional skeleton structure is shown in Image 6 shown....

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Abstract

The invention discloses a transition metal complex based on a semirigid bipyridine bisamide organic ligand and terephthalic acid as well as a synthetic method and application of the transition metal complex. The molecular formula of the transition metal complex is as follows: [Zn(3-bpah)(1,4-BDC)).H2O; [Cd(3-bpah)(1,4-BDC)(H2O)], wherein 3-bpah is N,N'-bi(3-pyridine acylamino)-1 2-cyclohexane. The method comprises the steps of mixing Zb<2+> nitrate or Cd<2+> chloride, the semirigid bipyridine bisamide ligand, terephthalic acid and deionized water, adjusting the pH value of the mixture, pouring the mixture into a high-pressure reaction kettle, performing heat preservation in hydrothermal condition, cooling the mixture to room temperature, and airing the mixture, so as to obtain the target complex. The transition metal complex as well as the synthetic method and application of the transition metal complex have the advantages that the synthetic method is simple, the synthetic yield is high, the synthesized complex has high fluorescence-emission property, fluorescent selectivity to different solvent molecules, and fluorescence identification and detection properties for environmental pollutant nitrobenzene, and can be used as fluorescent material.

Description

technical field [0001] The invention belongs to the field of fluorescent material synthesis, in particular to a transition metal complex based on a semi-rigid bispyridine bisamide organic ligand and terephthalic acid, and a synthesis method and application thereof. Background technique [0002] Transition metal functional complexes based on mixed ligands of organic aromatic carboxylic acids and organic amines have rich and diverse structures, and have attracted extensive attention for their potential applications in magnetism, catalysis, adsorption, and fluorescence. Research in this area mainly focuses on the design and synthesis of new complexes and the exploration of the relationship between structure and properties. Although remarkable progress has been made, it is still a great challenge to accurately synthesize complexes with expected structures and properties. . The design of organic amine ligands with specific structures and the selection of appropriate metal ions a...

Claims

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Application Information

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IPC IPC(8): C07F3/06C07F3/08C09K11/06G01N21/64
Inventor 林宏艳王秀丽刘国成栾健田爱香张巨文
Owner BOHAI UNIV
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