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Semi-rigid double-imidazole organic-ligand-based transition metal compound containing N-S dicarboxylic acid, as well as synthetic method and application thereof

A technology of organic ligands and transition metals, applied in the field of transition metal complexes and their synthesis, can solve the limitation of the length of organic ligands, the flexibility of ligands, the number of coordination sites and the coordination ability, and the synthesis yield of transition metal functional complexes. There are only problems such as poor catalytic degradation effect of water-soluble organic pollutants, etc., to achieve the effect of good catalytic degradation effect, shortening the synthesis cycle, and increasing coordination adaptability.

Inactive Publication Date: 2013-11-27
BOHAI UNIV
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Problems solved by technology

However, the synthesis of such complexes is restricted by the flexibility of the organic ligands, the length of the ligands, the number of coordination sites, and the coordination ability
Although some complex materials with excellent properties and diverse structures have been synthesized, it is still difficult to synthesize such complex materials.
In addition, the carboxylic acid ligands currently used to synthesize transition metal functional complexes based on organic carboxylic acid and organic amine mixed ligands generally use carboxylic acid derivatives linked by aromatic hydrocarbon structural units. The rigidity and steric position of such derivatives The resistance is relatively large, and it shows certain limitations when coordinating with metal ions, which makes it relatively difficult to crystallize transition metal functional complexes based on such carboxylic acid derivatives, resulting in a synthesis yield of transition metal functional complexes of only 40%. %, the synthesis yield is low, and the cost of synthesis raw materials using multi-acid-based functional complexes as photocatalytic materials is high, the power consumption is large, and it is easy to cause secondary metal pollution of Mo or W; on the other hand, when the After the carboxylic acid derivatives are coordinated with the metal ion, the hydrophobicity of the ligand is increased, which makes the transition metal functional complex constructed by the carboxylic acid poor in affinity to water-soluble organic pollutants. The catalytic degradation effect on water-soluble organic pollutants is poor

Method used

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  • Semi-rigid double-imidazole organic-ligand-based transition metal compound containing N-S dicarboxylic acid, as well as synthetic method and application thereof
  • Semi-rigid double-imidazole organic-ligand-based transition metal compound containing N-S dicarboxylic acid, as well as synthetic method and application thereof
  • Semi-rigid double-imidazole organic-ligand-based transition metal compound containing N-S dicarboxylic acid, as well as synthetic method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0050] Example 1 Synthesis of [Co 2 (L) 2 (2-CMSN) 2 (H 2 O)]·H 2 O, wherein, L is 1,4-two (imidazol-1-methylene) benzene, the structural formula is: , 2-CMSN is 2-carboxymethylenethionicotinate

[0051] 0.1mmol Co(NO 3 ) 2 ·6H 2 O, 0.10mmol 1,4-bis(imidazol-1-methylene)benzene, 0.1mmol 2-carboxymethylenethionicotinic acid (the structural formula is: ) and 7.5mL H 2 Add O to a 50mL beaker in turn, stir at room temperature for 20min, adjust the pH to 6 with 0.1mol / L NaOH solution, pour it into a 25mL autoclave, heat up to 90°C at a heating rate of 15°C / h, and heat Under the condition of heat preservation for 48 h, the temperature was lowered to room temperature at a cooling rate of 5 °C / h to obtain pink blocky crystals, which were washed twice with deionized water and ethanol alternately, and dried naturally at room temperature to obtain [Co 2 (L) 2 (2-CMSN) 2 (H 2 O)]·H 2 O, the yield is 62%, and its coordination environment diagram is as follows Figure 7 As ...

Embodiment 2

[0052] Example 2 Synthesis of [Co 2 (L) 2 (2-CMSN) 2 (H 2 O)]·H 2 O, where L is 1,4-bis(imidazol-1-methylene)benzene, and 2-CMSN is 2-carboxymethylenethionicotinate

[0053] 0.2mmol Co(NO 3 ) 2 ·6H 2 O, 0.10mmol 1,4-bis(imidazol-1-methylene)benzene, 0.14mmol 2-carboxymethylenethionicotinic acid and 12mL H 2 Add O to a 50mL beaker in turn, stir at room temperature for 30min, adjust the pH to 6.1 with 0.5mol / L NaOH solution, pour it into a 25mL autoclave, heat up to 100°C at a heating rate of 10°C / h, and heat Under the condition of heat preservation for 48h, the temperature was lowered to room temperature at a cooling rate of 2.5 °C / h to obtain pink blocky crystals, washed alternately with deionized water and ethanol for 5 times, and dried naturally at room temperature to obtain [Co 2 (L) 2 (2-CMSN) 2 (H 2 O)]·H 2 O, the yield is 84%, and its coordination environment diagram is as follows Figure 7 As shown, its two-dimensional network diagram is shown as Figure 8...

Embodiment 3

[0054] Example 3 Synthesis of [Co 2 (L) 2 (2-CMSN) 2 (H 2 O)]·H 2 O, where L is 1,4-bis(imidazol-1-methylene)benzene, and 2-CMSN is 2-carboxymethylenethionicotinate

[0055] 0.3mmol Co(NO 3 ) 2 ·6H 2 O, 0.10mmol 1,4-bis(imidazol-1-methylene)benzene, 0.2mmol 2-carboxymethylenethionicotinic acid and 14mL H 2 Add O to a 50mL beaker in turn, stir at room temperature for 60min, adjust the pH to 7.0 with 1mol / L NaOH solution, pour it into a 25mL autoclave, and raise the temperature to 105°C at a heating rate of 5°C / h. Keep it warm for 60 hours, lower the temperature to room temperature at a cooling rate of 8°C / h, and obtain pink blocky crystals, wash them alternately with deionized water and ethanol for 3 times, and dry naturally at room temperature to obtain [Co 2 (L) 2 (2-CMSN) 2 (H 2 O)]·H 2 O, the yield is 74%, and its coordination environment diagram is as follows Figure 7 As shown, its two-dimensional network diagram is shown as Figure 8 shown.

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Abstract

The molecular formula of a semi-rigid double-imidazole organic-ligand-based transition metal compound containing N-S dicarboxylic acid is [Co2 (L) 2 (2-CMSN) 2 (H2O)]. H2O; [Cd (L) (2-CMSN) (H2O)]; [Zn (L) (2-CMSN)]. 2 H2O; [Cd (L) (ADTZ) (H2O)]; [Zn (L) (ADTZ)]. H2O, wherein L represents 1, 4-bis ( imidazol-1-methylene ) benzene, 2-CMSN represents 2-carboxylic acid methylene group root, and ADTZ represents 2,2'-(1,3,4-thiadiazol oxazol-2,5-diyl) dithio diethyl dianion root. A synthetic method of the transition metal compound comprises the following steps: adding Co<2+> or Zn<2+> and Cd<2+> nitrate, semi-rigid double-imidazole ligands, dicarboxylic acid containing N and S into deionized water, stirring, using NaOH solution to adjust pH, pouring the mixture into a high-pressure reaction kettle, increasing the temperature to realize hydrothermal reaction, cooling to obtain a bulk crystal, and washing and drying the bulk crystal to obtain the target product. The synthetic method of the compound is simple, the synthesis productivity is high, the cost of synthetic raw materials is low, the synthetic period is short and the electrical energy consumption is low; the compound is high in affiliation capacity of water-soluble pollutants, good in catalysis and degradation effects and environmental-friendly, and can be used as photocatalytic materials.

Description

technical field [0001] The invention belongs to the field of photocatalytic materials and synthesis methods, in particular to a transition metal complex based on a semi-rigid bis-imidazole organic ligand and N-S dicarboxylic acid, and a synthesis method and application thereof. Background technique [0002] Transition metal functional complexes based on mixed ligands of organic carboxylic acids and organic amines are inorganic functional materials with rich and diverse structures, good catalytic performance, and a wide range of applications. However, the synthesis of such complexes is restricted by the flexibility of the organic ligands, the length of the ligands, the number of coordination sites, and the coordination ability. Although some complex materials with excellent properties and diverse structures have been synthesized, it is still difficult to synthesize such complex materials. In addition, the carboxylic acid ligands currently used to synthesize transition metal ...

Claims

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Application Information

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IPC IPC(8): C07F15/06C07F3/06C07F3/08B01J31/22
Inventor 刘国成王秀丽张巨文林宏艳田爱香应俊
Owner BOHAI UNIV
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