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Preparation method and application of viologen complex film

A technology of complexes and viologens, which is applied in the field of preparation of viologen complex films, can solve the problems of difficulty in obtaining complex films, long time consumption, and little research on electrochromism of viologen complexes.

Pending Publication Date: 2022-06-28
UNIV OF SCI & TECH OF CHINA
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0003] In recent years, viologen metal complexes have attracted the attention of many researchers, but the synthesis of viologen complexes reported so far is mostly by solvothermal method, which takes a long time, consumes a lot of energy and is not easy to control. Most importantly, it is difficult to Obtaining complex films greatly limits the application fields of viologen complexes, especially the field of electrochromism, so there are few electrochromic researches on viologen complexes

Method used

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  • Preparation method and application of viologen complex film
  • Preparation method and application of viologen complex film
  • Preparation method and application of viologen complex film

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preparation example Construction

[0030] The invention provides a preparation method of a viologen complex film, comprising:

[0031] A three-electrode system was used to reduce the viologen ligand monomer on the surface of the working electrode to obtain a viologen complex film;

[0032] The electrodeposition solution used in the reduction process includes: a viologen ligand monomer, a metal source, an electrolyte and a solvent.

[0033] In the present invention, the three-electrode system preferably includes: a working electrode, a reference electrode and a counter electrode.

[0034] In the present invention, the working electrode is preferably a conductive substrate, more preferably selected from ITO (indium tin oxide conductive glass), FTO (fluorine-doped SnO) 2 Conductive glass), PET / ITO (indium tin oxide coated PET conductive film).

[0035] In the present invention, the working electrode is preferably washed, dried and trimmed.

[0036] In the present invention, the washing method is preferably ultr...

Embodiment 1

[0079] Example 1 Synthesis of viologen derivative ligand (Oxv)

[0080] The preparation of Oxv ligand was carried out according to the following route:

[0081]

[0082] Into a 250 mL round-bottomed flask were added 4-pyridineboronic acid (1.0 g, 8.1 mmol), 2,5-dibromoanisole (1.2 g, 4.5 mmol), potassium carbonate (1.2 g, 8.6 mmol), tetrakistriphenyl Phosphine palladium (0.28g, 0.20mmol) and a magnetic stirring bar, the bottle was evacuated; 50mL of a mixed solvent of dioxane and water 4:1 was injected into the round-bottomed flask, and the reaction system was protected with argon gas. The reaction system was stirred at 90°C for 48h to carry out the reaction; after the reaction, the obtained reaction product was cooled to room temperature, the solvent was removed by rotary evaporation at 50°C, dissolved in chloroform, the organic phase was extracted, and then the solvent was rotated to dryness to obtain a crude product ; Purify the crude product with ethyl acetate column c...

Embodiment 2

[0085] Example 2 Synthesis of Violet Derivative Ligand (Dioxv)

[0086] The preparation of Dioxv ligands was carried out according to the following route:

[0087]

[0088] The ligand was prepared according to the method of Example 1, and the difference from Example 1 was that 2,5-dibromodimethoxybenzene (1.3 g, 4.5 mmol) was used.

[0089] The product prepared by embodiment 2 is carried out hydrogen nuclear magnetic resonance spectrum detection, and the detection result is such as Image 6 b, the data are: 1HNMR (300MHz, DMSO-d6, ppm): δ9.314-9.264(d,4H), 8.517-8.469(d,4H), 8.055-8.011(d,4H), 7.731-7.687 (d, 4H), 7.538-7.498 (S, 2H), 6.017-5.951 (S, 4H), 3.948-3.900 (S, 6H); it can be seen that the method of Example 2 can prepare the target product.

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Abstract

The invention provides an electrochemical synthesis method of a viologen metal complex film, which utilizes the oxidation-reduction characteristic of a viologen derivative ligand to reduce a viologen ligand on the surface of an electrode to cause local pH value increase of the surface of the electrode, thereby promoting deprotonation of the viologen ligand and finally inducing formation of a metal complex on the surface of the electrode. According to the method provided by the invention, the reduction property of the viologen ligand is directly utilized, some molecules or ions with special reducibility do not need to be additionally used, a sacrificial metal anode does not need to be used, and the complex film can be prepared on various conductive substrates. The method provided by the invention is simple in process and mild in condition, and the prepared viologen complex has various intelligent photoelectric characteristics and has a huge application prospect in the field of intelligent photoelectricity, especially in the field of electrochromism. The invention also provides application of the viologen metal complex film.

Description

technical field [0001] The invention belongs to the technical field of metal complexes, and in particular relates to a preparation method and application of a viologen complex thin film. Background technique [0002] Violet (N,N-disubstituted-4,4-bipyridine) materials have good redox properties and have been widely used in electrochromic fields since their discovery in 1932. The N,N-disubstituted positions of such materials are easy to modify, and they can be designed as functional ligands and metal centers to coordinate to obtain metal complexes. Metal complexes have the characteristics of easily tunable structure, large specific surface area, and high charge mobility, which are beneficial to the realization of electrochromic process, so they are a kind of potential electrochromic materials. [0003] In recent years, viologen metal complexes have attracted the attention of many researchers. However, most of the reported viologen complexes are synthesized by solvothermal me...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C25D9/02C09K9/02
CPCC25D9/02C09K9/02C09K2211/1029C09K2211/1007C09K2211/188
Inventor 徐春叶彭晓函郑建明
Owner UNIV OF SCI & TECH OF CHINA
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