A kind of copper complex with electrocatalytic activity to hydrogen peroxide and preparation method thereof

Abstract

The invention discloses a copper complex and a preparation method thereof, and the copper complex is characterized by having good electrocatalytic activity on hydrogen peroxide, the molecular formula of the copper complex is C46H34N6O14Cu2, the crystal system is clinorhomboidal, the space group is P-1, the cell parameters are as follows: alpha is equal to 99.90 degrees, beta is equal to 101.2 degrees and gamma is equal to 93.69 degrees. The copper complex is prepared from a mixing reaction of a copper salt, 5-(di(carboxymethyl) amino)-2-hydroxybenzoic acid and 1,10-phenanthroline according to a certain proportion, the copper complex has a specific spatial structure and an accurate molecular formula, the synthesis steps are simple, and the yield can reach 30-70%. The copper complex prepared in the invention has good electrocatalytic activity, thereby having a broad application prospect of being used as a potential electrocatalytic active material.

Description

technical field

[0001] The invention relates to the field of material chemistry, in particular to a copper complex having electrocatalytic activity for hydrogen peroxide and a preparation method thereof. Background technique

[0002] Electrocatalysis is a kind of catalysis that accelerates the reaction by charge transfer at the electrode-electrolyte interface. Electrocatalysis covers two aspects of electrode reaction and catalysis, so electrocatalysts must have these two functions at the same time: (1) be able to conduct electricity and transfer electrons relatively freely; (2) be able to effectively catalytically activate the substrate . Mainly used in electrocatalytic treatment of fuel cells and organic sewage; electrocatalytic degradation of chromium-containing wastewater; electrolytic desulfurization of flue gas and raw coal; simultaneous removal of NO by electrocatalysis x and SO 2 ; Electrolytic reduction of carbon dioxide; Electrolytic reduction of formaldehyde, hy...

Examples

Embodiment 1

[0020] Weigh CuSO 4 ·5H 2 O (2.497g, 10mmol), H 4 Add L (0.269g, 1.0mmol) and 1,10-phenanthroline (0.180g, 1.0mmol) to 5.0mL distilled water, stir to dissolve; seal the reaction device and heat at 60°C for 60min, then take it out and cool to Room temperature; then use dilute KOH solution to adjust the mixed solution to be weakly acidic (pH=5); let it stand at room temperature, and slowly evaporate the solvent until crystals are precipitated. The solution was removed, and the massive crystals obtained by natural air drying were copper complexes.

[0021] Wherein, the ligand 5-(bis(carboxymethyl)amino)-2-hydroxybenzoic acid (H 4 L) Preparation method: KOH solution (12M, 20mL) was added dropwise into sodium chloroacetate (13.978g, 0.12mol) aqueous solution (20mL) and stirred, then 5-aminosalicylic acid (4.59g, 0.03mmol) Slowly added to the above mixture, reacted at 85°C for 30h. After the reaction, cool to room temperature, acidify with HCl solution (6mol / L) until precipitat...

Embodiment 2

[0023] Weigh CuCl 2 2H 2 O (0.170g, 1.0mmol), H 4 Add L (2.692g, 10mmol) and 1,10-phenanthroline (1.802g, 10mmol) to 40mL of distilled water, stir to dissolve; seal the reaction device and heat at 90°C for 15min, then take it out and cool to room temperature; Use dilute KOH solution to adjust the mixed solution to be weakly acidic (pH=7); let it stand at room temperature, and slowly evaporate the solvent until crystals are precipitated. The solution was removed, and the massive crystals obtained by natural air drying were copper complexes.

Embodiment 3

[0025] Weigh Cu(NO 3 ) 2 ·3H 2 O (0.483g, 2.0mmol), H 4 Add L (2.692g, 10mmol) and 1,10-phenanthroline (1.802g, 10mmol) to 15mL of distilled water, stir to dissolve; seal the reaction device and heat at 80°C for 30min, then take it out and cool to room temperature; Use dilute KOH solution to adjust the mixed solution to be weakly acidic (pH=6); let it stand at room temperature, and slowly evaporate the solvent until crystals are precipitated. The solution was removed, and the massive crystals obtained by natural air drying were copper complexes.

technical field

[0001] The invention relates to the field of material chemistry, in particular to a copper complex having electrocatalytic activity for hydrogen peroxide and a preparation method thereof. Background technique

[0002] Electrocatalysis is a kind of catalysis that accelerates the reaction by charge transfer at the electrode-electrolyte interface. Electrocatalysis covers two aspects of electrode reaction and catalysis, so electrocatalysts must have these two functions at the same time: (1) be able to conduct electricity and transfer electrons relatively freely; (2) be able to effectively catalytically activate the substrate . Mainly used in electrocatalytic treatment of fuel cells and organic sewage; electrocatalytic degradation of chromium-containing wastewater; electrolytic desulfurization of flue gas and raw coal; simultaneous removal of NO by electrocatalysis x and SO 2 ; Electrolytic reduction of carbon dioxide; Electrolytic reduction of formaldehyde, hy...

Examples

Embodiment 1

[0020] Weigh CuSO 4 ·5H 2 O (2.497g, 10mmol), H 4 Add L (0.269g, 1.0mmol) and 1,10-phenanthroline (0.180g, 1.0mmol) to 5.0mL distilled water, stir to dissolve; seal the reaction device and heat at 60°C for 60min, then take it out and cool to Room temperature; then use dilute KOH solution to adjust the mixed solution to be weakly acidic (pH=5); let it stand at room temperature, and slowly evaporate the solvent until crystals are precipitated. The solution was removed, and the massive crystals obtained by natural air drying were copper complexes.

[0021] Wherein, the ligand 5-(bis(carboxymethyl)amino)-2-hydroxybenzoic acid (H 4 L) Preparation method: KOH solution (12M, 20mL) was added dropwise into sodium chloroacetate (13.978g, 0.12mol) aqueous solution (20mL) and stirred, then 5-aminosalicylic acid (4.59g, 0.03mmol) Slowly added to the above mixture, reacted at 85°C for 30h. After the reaction, cool to room temperature, acidify with HCl solution (6mol / L) until precipitat...

Embodiment 2

[0023] Weigh CuCl 2 2H 2 O (0.170g, 1.0mmol), H 4 Add L (2.692g, 10mmol) and 1,10-phenanthroline (1.802g, 10mmol) to 40mL of distilled water, stir to dissolve; seal the reaction device and heat at 90°C for 15min, then take it out and cool to room temperature; Use dilute KOH solution to adjust the mixed solution to be weakly acidic (pH=7); let it stand at room temperature, and slowly evaporate the solvent until crystals are precipitated. The solution was removed, and the massive crystals obtained by natural air drying were copper complexes.

Embodiment 3

[0025] Weigh Cu(NO 3 ) 2 ·3H 2 O (0.483g, 2.0mmol), H 4 Add L (2.692g, 10mmol) and 1,10-phenanthroline (1.802g, 10mmol) to 15mL of distilled water, stir to dissolve; seal the reaction device and heat at 80°C for 30min, then take it out and cool to room temperature; Use dilute KOH solution to adjust the mixed solution to be weakly acidic (pH=6); let it stand at room temperature, and slowly evaporate the solvent until crystals are precipitated. The solution was removed, and the massive crystals obtained by natural air drying were copper complexes.

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