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Hybrid material based on macrocyclic compound photosensitive dye and titanium dioxide and preparation method thereof, and application of hybrid material to photocatalysis

A technology of macrocyclic compounds and photosensitizing dyes, which is applied in the field of hybrid materials based on macrocyclic compound photosensitizing dyes and titanium dioxide and its preparation and application in photocatalysis, which can solve the problem of photocatalyst catalytic activity and stability reduction, competitive adsorption , Occupying active sites and other issues, achieving excellent hydrogen production performance, reducing recombination probability, and excellent stability

Active Publication Date: 2018-04-13
SUN YAT SEN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, the common solution is surface modification or ion doping. However, surface modification is likely to cause problems such as competitive adsorption and occupation of active sites. Ion doping introduces a large number of electron-hole recombination centers, resulting in the catalytic Reduced activity and stability

Method used

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  • Hybrid material based on macrocyclic compound photosensitive dye and titanium dioxide and preparation method thereof, and application of hybrid material to photocatalysis
  • Hybrid material based on macrocyclic compound photosensitive dye and titanium dioxide and preparation method thereof, and application of hybrid material to photocatalysis
  • Hybrid material based on macrocyclic compound photosensitive dye and titanium dioxide and preparation method thereof, and application of hybrid material to photocatalysis

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preparation example Construction

[0054] A method for preparing a hybrid material based on a macrocyclic compound photosensitizing dye and titanium dioxide, comprising the following steps:

[0055] 1) Preparation of dye solution: dissolve the above-mentioned macrocyclic compound photosensitive dye in an organic solvent to prepare a dye solution;

[0056] 2) Dye-TiO 2 Preparation of gel: Mix tetrabutyl titanate, chelating agent, water and dye solution, heat the mixture until it solidifies to form a translucent colloidal solid, and obtain the dye-TiO 2 gel;

[0057] 3) Post-processing of the gel: extraction dye-TiO 2 Gel, dry, and crystallize to obtain a hybrid material based on a macrocyclic compound photosensitive dye and titanium dioxide.

[0058] Preferably, in step 1) of the preparation method of the hybrid material, the organic solvent is at least one of THF, DMF, DMSO, and acetone; the concentration of the macrocyclic photosensitive dye in the dye solution is (5-10) μmol / L.

[0059] Preferably, in ste...

Embodiment 1

[0079] 1. Synthesis of calixarene dye HO-TPA

[0080] The synthetic route of calixarene dye HO-TPA is shown as attached figure 1 shown. This schematic diagram shows only an example of the synthesis method, and the method of the present invention is not limited to the related substances shown in the figure. Concrete synthetic steps are as follows:

[0081] 1. Synthesis of compound 1-2

[0082]

[0083] Synthesis steps: add compound 1-1 (80mg, 0.0727mmol) and 2,2'-bithiophene-5-boronic acid pinacol ester (106.3mg, 0.3635mmol) into a Schlenk bottle, vacuumize and inflate with nitrogen three times each, add Anhydrous potassium carbonate (225mg, 1.628mmol) aqueous solution, ethylene glycol dimethyl ether (10mL), stirred at room temperature for about 15min, added Pd (pph 3 ) 4 (25mg, 0.02181mmol), mix well, heat up to 90°C, monitor the reaction by TLC, after the reaction product is fully cooled, extract with dichloromethane to obtain the organic phase, wash the organic phase...

Embodiment 2

[0104] 1. Synthesis of zinc porphyrin dyes

[0105] The synthetic route of zinc porphyrin dye is shown as attached Figure 7 shown. This schematic diagram shows only an example of the synthesis method, and the method of the present invention is not limited to the related substances shown in the figure. Concrete synthetic steps are as follows:

[0106] 1. Synthesis of compound 2-1

[0107]

[0108] 4-Hydroxybenzaldehyde (4.9g, 0.04mol), pyrrole (2.8mL, 0.04mol) and propionic acid (100mL) were mixed together and stirred at reflux for 1 hour, filtered, and the filtered solid was washed 5 times with hot water, dried, Washed with dichloromethane and ethyl acetate, the obtained solid was purified by silica gel column, eluting with methanol and ethyl acetate, to obtain purple solid 2-1 with a yield of 7%. 1 H NMR (DMSO-d 6 ):δ9.94(s,4H,Ar-OH),8.86(s,8H,β-pyrrole-H),7.89(d,8H,m-Ar-H,J=6.8Hz),7.20(d, 8H, o-Ar-H, J=6.8Hz). 13 C NMR (DMSO-d 6 ): δ175.55(ArC-OH).157.77(α-pyrrol...

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Abstract

The invention discloses a hybrid material based on a macrocyclic compound photosensitive dye and titanium dioxide and a preparation method thereof, and application of the hybrid material to photocatalysis. The hybrid material comprises the macrocyclic compound photosensitive dye and titanium dioxide, wherein the macrocyclic compound photosensitive dye is a calixarene compound or porphyrin compound. The invention also discloses the preparation method for the hybrid material based on the macrocyclic compound photosensitive dye and titanium dioxide, and application of the hybrid material to photocatalysis. The organic-inorganic hybrid material prepared from the macrocyclic compound photosensitive dye and titanium dioxide has a hierarchical porous structure, and can improve the free diffusionof gas and surface adsorption of CO2, increase the adsorption quantity and activation degree of reactants, reduce the possibility of electron-hole recombination and effectively enhance photocatalysisefficiency. Moreover, the hybrid material of the invention has high stability and is improved in cyclic utilization stability in photocatalysis.

Description

technical field [0001] The invention relates to a hybrid material based on a photosensitive dye of a macrocyclic compound and titanium dioxide, a preparation method thereof and an application in photocatalysis. Background technique [0002] With the consumption of fossil fuels, people are beginning to face the problem of energy depletion, how to provide sufficient renewable energy has attracted widespread attention. Solar energy is clean and pollution-free, with huge reserves, which is an effective way to solve the above problems. Photocatalysis is an effective photoelectric conversion technology in the photolysis of water for hydrogen production and photocatalytic reduction of CO 2 has important application prospects. However, most photocatalysts respond to ultraviolet light at present, and visible light, which accounts for 43% of solar energy, cannot be effectively utilized, and the high recombination rate of photogenerated carriers inside semiconductors also restricts t...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/38B01J35/10C01B3/04C01B32/40
CPCC01B3/042B01J31/38B01J35/39B01J35/61Y02E60/36
Inventor 刘军民苏成勇陈逸凡黄剑锋秦苏黄理渊徐耀维郭靖
Owner SUN YAT SEN UNIV
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