Preparation method of photochromic material based on boron cluster anions

A photochromic material and anion technology, applied in the field of materials, can solve the problems of low quantum yield, small excitation wavelength, cumbersome synthesis, etc., and achieve the effects of low preparation cost, long free radical life, and high photosensitivity

Active Publication Date: 2021-04-02
WUHAN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The reported organic photochromic materials have a variety of problems, such as cumbersome synthesis, high cost, small excitation wavelength, and low quantum yield.

Method used

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  • Preparation method of photochromic material based on boron cluster anions

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Experimental program
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Effect test

Embodiment 1

[0027] The preparation of several conjugated polypyridine molecules used in the present invention:

[0028] (1) Preparation of 2,4,6-tris(pyridin-4-yl)-1,3,5-triazine (TPT)

[0029] 4-cyanopyridine (6.0 g, 56 mmol) was added into a 100 mL three-necked flask and heated to 150° C. in an oil bath. Powdered NaOH (230mg, 5.6mmol) was added to the resulting liquid, and the mixture was kept at 150°C for 24h. After the reaction was completed, it was cooled to room temperature, and the solid was washed with a large amount of acetone and dissolved in 50mL of 4M hydrochloric acid. Activated carbon was then added and sonicated for 30 min. Filter the suspension with diatomaceous earth, and neutralize it with 2mol / L NaOH solution. At this time, a large amount of white precipitate will be produced. After filtering, wash it with a large amount of water and acetone alternately three times, and dry it in a 60°C oven. The product was obtained as a white solid (3.1 g, 52% yield).

[0030](2) P...

Embodiment 2

[0044] 0.624g (2mmol) of 2,4,6-tris(pyridin-4-yl)-1,3,5-triazine prepared in Example 1 was added into a 250mL round bottom flask containing 100mL ultrapure water, and then Adjust the pH to 0 with dilute hydrochloric acid, and stir ultrasonically at room temperature (25°C) until the solution is completely clear and transparent to obtain solution A; will contain 0.563g (3mmol) Na 2 B 12 h 12 50mL aqueous solution of the solution was added to solution A, and a light yellow precipitate was rapidly formed, and the stirring was continued for 30 minutes, and the precipitate was obtained by filtration, and washed three times with a small amount of water and ethanol respectively. The target product BOFs-TPT-H was obtained by vacuum drying. The excitation wavelength threshold for discoloration of the obtained target product is roughly between 460nm and 520nm, the photoresponse time is 3s, and the lifetime of free radicals is permanent at room temperature, and the free radicals disappe...

Embodiment 3

[0046] 0.624g (2mmol) of 2,4,6-tris(pyridin-3-yl)-1,3,5-triazine prepared in Example 1 was added into a 250mL round bottom flask containing 100mL of ultrapure water, and then Adjust the pH to 0 with dilute hydrochloric acid, and stir ultrasonically at room temperature (25°C) until the solution is completely clear and transparent to obtain solution A; will contain 0.563g (3mmol) Na 2 B 12 h 12 50mL aqueous solution of the solution was added to solution A, and a light yellow precipitate was rapidly formed, and the stirring was continued for 30 minutes, and the precipitate was obtained by filtration, and washed three times with a small amount of water and ethanol respectively. The target product was obtained by vacuum drying. The excitation wavelength threshold for discoloration of the obtained target product is approximately between 460nm and 520nm, the photoresponse time is 10s, and the lifetime of free radicals is permanent at room temperature, and the free radicals disappea...

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Abstract

The invention discloses a preparation method of a photochromic material based on boron cluster anions, which comprises the following steps: adding conjugated polypyridine molecules into ultrapure water, regulating the pH value to -1-7 with an inorganic acid, and carrying out ultrasonic stirring at room temperature until the solution is completely clear and transparent to obtain a solution A; and adding an aqueous solution containing a boron cluster compound into the solution A, continuously stirring for 0.5-24 hours after generating a precipitate, filtering to obtain a precipitate, washing, and carrying out vacuum drying to obtain the photochromic material based on boron cluster anions. The method is mild in reaction condition, simple in process and easy to operate. The absorption spectrumdifference before and after material discoloration is large, and preparation cost is low. The synthesized material has the advantages of higher photosensitivity, quicker discoloration and longer freeradical service life. A reference thought is provided for subsequently utilizing the photochromic material in the application fields of biological treatment, photoelectric conversion and the like, and the photochromic material has a great application prospect in the aspect of photoelectrocatalysis.

Description

technical field [0001] The invention belongs to the technical field of materials, and in particular relates to a method for preparing a boron cluster anion-based photochromic material. Background technique [0002] Organic photochromism refers to the reversible light-induced conversion between two isomer molecules, and the absorption spectra of the two isomers are significantly different before and after illumination. In the reversible process of photoisomerization, some physical properties of photochromic compounds, such as ultraviolet absorption spectrum, degree of molecular conjugation, fluorescence emission spectrum, electrical conductivity, magnetism, coordination, dipole interaction, electrical Chemical properties, refractive index, etc. may vary. This inspires people to apply this kind of compounds in various fields, such as molecular switches, data recording and storage, multi-photon devices, nanoparticle devices, optoelectronics and other fields. [0003] The prin...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C09K9/00C09K9/02C07D401/14C07D213/22C07D471/04C07D403/14C07D213/127B01J31/02
CPCC09K9/00C09K9/02C07D401/14C07D213/22C07D471/04C07D403/14C07D213/127B01J31/0244B01J35/0033B01J35/004C09K2211/1029C09K2211/1044C09K2211/1059
Inventor 张海波杨紫琼范正宇
Owner WUHAN UNIV
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