Preparation method and application of cobalt (II) coumarin Schiff base complex

A technology of coumarins and Schiff bases, which is applied in the direction of cobalt organic compounds, organic compounds/hydrides/coordination complex catalysts, compounds containing elements of group 8/9/10/18 of the periodic table, etc., can Solve the problems of low reduction efficiency, low overpotential, and high reduction cost, and achieve the effects of less raw material consumption, high catalytic performance, and high selectivity

Active Publication Date: 2021-08-27
ANHUI UNIVERSITY OF TECHNOLOGY
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0006] The purpose of the present invention is to overcome the use of existing photocatalysts to CO 2 In the photocatalytic reduction reaction, there are disadvantages such as high reduction cost and relatively low reduction efficiency. A new method for the preparation and application of cobalt (II) coumarin Schiff base complexes is provided. By using cobalt materials cheap, low toxicity, moderate CO 2 Adsorption strength, excellent electron-mediated function and low overpotential, applied to CO 2 In the process of photocatalytic reduction, as a catalyst with strong activity, it is beneficial to reduce environmental pollution, and it is CO 2 Resource utilization provides an effective way

Method used

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  • Preparation method and application of cobalt (II) coumarin Schiff base complex
  • Preparation method and application of cobalt (II) coumarin Schiff base complex
  • Preparation method and application of cobalt (II) coumarin Schiff base complex

Examples

Experimental program
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Effect test

Embodiment 1

[0047] In a 100mL round bottom flask, add 3.12g (20mmol) 5-chloro salicylaldehyde, 2.34g (20mmol) acetylglycine and 4.92g (60mmol) anhydrous sodium acetate, then add 40mL acetic anhydride, stir until the solid is completely dissolved , heated to reflux at 130°C for 12h, cooled to room temperature, added a large amount of ice water, and a large amount of precipitate was observed. After drying by suction, the product was placed in a mixed solvent of 20mL concentrated hydrochloric acid:ethanol (2:1) at 80 Reflux at ℃ for 5 hours, cool naturally, and adjust the pH to nearly neutral with 30% NaOH, a large amount of precipitates are precipitated, filtered and dried, and then recrystallized with absolute ethanol to obtain the precursor of 3-amino-6-chlorocoumarin;

[0048] Weigh 1.96g of 3-amino-6-chlorocoumarin (10mmol) and 1.56g of 5-chlorosalicylaldehyde (10mmol) and dissolve them in 20mL of absolute ethanol, reflux at 70°C for 6h, a large amount of precipitates are formed, cool A...

Embodiment 2

[0051] Add 3.12g (20mmol) 5-chloro salicylaldehyde, 2.34g (20mmol) acetylglycine and 4.92g (60mmol) anhydrous sodium acetate in a 100mL round bottom flask, then add 45mL acetic anhydride, stir until the solid is completely dissolved , heated to reflux at 135°C for 10 h, cooled to room temperature, added a large amount of ice water, and a large amount of precipitate was observed. After drying by suction, the product was placed in a mixed solvent of 20 mL concentrated hydrochloric acid:ethanol (2:1) at 80 Reflux for 4 hours at ℃, cool naturally, and adjust the pH to near neutral with 30% NaOH, a large amount of precipitate precipitates, filter and dry, and then recrystallize with absolute ethanol to obtain the precursor of 3-amino-6-chlorocoumarin;

[0052] Weigh 1.96g of 3-amino-6-chlorocoumarin (10mmol) and 1.56g of 5-chlorosalicylaldehyde (10mmol) and dissolve them in 20mL of absolute ethanol, reflux at 75°C for 5h, a large amount of precipitates are formed, cool After reachi...

Embodiment 3

[0055] In a 100mL round bottom flask, add 3.12g (20mmol) 5-chloro salicylaldehyde, 2.34g (20mmol) acetylglycine and 4.92g (60mmol) anhydrous sodium acetate, then add 50mL acetic anhydride, stir until the solid is completely dissolved , heated to reflux at 140°C for 9h, cooled to room temperature, added a large amount of ice water, and a large amount of precipitate was observed. Reflux for 3 hours at ℃, cool naturally, and adjust the pH to nearly neutral with 30% NaOH, a large amount of precipitates are precipitated, filtered and dried, and recrystallized with absolute ethanol to obtain the precursor of 3-amino-6-chlorocoumarin; the Shimadzu The UV-2700 UV-visible spectrophotometer produced by the company records the UV-visible light absorption spectrum;

[0056] Weigh 1.96g of 3-amino-6-chlorocoumarin (10mmol) and 1.56g of 5-chlorosalicylaldehyde (10mmol) and dissolve them in 20mL of absolute ethanol, reflux at 80°C for 5h, a large amount of precipitates are formed, cool Afte...

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Abstract

The invention discloses a preparation method and application of a cobalt (II) coumarin Schiff base complex, and belongs to the technical field of inorganic material synthesis. The preparation method specifically comprises the following steps: firstly, synthesizing a 3-amino-6-chlorocoumarin precursor, and then heating and refluxing the 3-amino-6-chlorocoumarin precursor and a 5-chlorosalicylaldehyde ethanol solution to prepare coumarin Schiff base ligand 3-[(2-hydroxy-5-chlorobenzylidene)-amino]-6-chlorocoumarin; and finally, carrying out a coordination reaction to prepare the novel mononuclear ionic metal-organic small molecule cobalt (II) 3-[(2-hydroxy-5-chlorobenzene methylene)-amino]-6-chlorocoumarin complex. When the complex can be used as a catalyst to be applied to photocatalytic CO2 reduction, the turnovernumber (TON) and the turnover frequency (TOF) are 1592 and 159.2 h<-1> respectively, the selectivity is as high as 91%, the stability is relatively high, the complex synthesis method is relatively simple, the synthesis conditions are mild, and particularly, a theoretical foundation is laid for environmental pollution reduction and CO2 resource utilization by deep research of a photocatalytic mechanism.

Description

technical field [0001] The invention belongs to the technical field of inorganic material synthesis, in particular to a method for easily preparing cobalt (II) coumarin Schiff base complexes and the complexes in CO 2 Applications in photocatalytic reduction systems. Background technique [0002] With the rapid development of science and technology, the energy structure has undergone changes, and new energy sources such as wind energy, solar energy, and ocean energy have emerged. However, the proportion of fossil fuel energy is still the highest. With the widespread use of fossil fuels and rapid population growth, CO 2 Excessive emissions directly produce the global "greenhouse effect", which in turn leads to environmental degradation. Therefore, the photocatalytic conversion of CO 2 Conversion to valuable chemicals or fuels for carbon cycling not only reduces CO 2 emission, alleviate the secondary greenhouse effect, and help to solve the energy crisis. Harnessing sustai...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07F15/06C07D311/14B01J31/22C01B32/40
CPCC07F15/065C07D311/14B01J31/2217B01J35/004C01B32/40B01J2531/845B01J2531/0252B01J2231/62Y02A50/30
Inventor 吴芳辉文国强罗祥瑞孙文斌叶明富徐旭东
Owner ANHUI UNIVERSITY OF TECHNOLOGY
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