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Fullerene carboxylic acid derivative/photosensitizer/titanium dioxide as well as preparation method and application

A technology of fullerene carboxylic acid and titanium dioxide, which is applied to the preparation of carboxylic acid nitrile, the preparation of amino compounds by photochemical reaction, chemical instruments and methods, etc., can solve the problems of low light utilization rate, high active electron and hole separation efficiency, and absorption Issues such as narrow light spectrum range

Inactive Publication Date: 2018-06-05
INST OF CHEM CHINESE ACAD OF SCI +1
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] In view of this, the technical problem to be solved in the present invention is how to provide a novel composite material fullerene carboxylic acid derivative / photosensitizer / titanium dioxide and its preparation method and application. As a catalyst, its structure is novel and can solve technical problems such as low separation efficiency of highly active electrons and holes, narrow spectral range of absorbed light, and low light utilization rate in existing photocatalytic technologies. It not only effectively broadens the absorption range of the spectrum, It increases the utilization efficiency of light, and can increase the separation efficiency of electrons and holes, which contributes to the substantial improvement of photocatalytic performance.

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  • Fullerene carboxylic acid derivative/photosensitizer/titanium dioxide as well as preparation method and application
  • Fullerene carboxylic acid derivative/photosensitizer/titanium dioxide as well as preparation method and application
  • Fullerene carboxylic acid derivative/photosensitizer/titanium dioxide as well as preparation method and application

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Embodiment 1

[0072]In the field of fullerene chemistry, one of the most attractive properties is its low recombination energy in almost all reactions, which is of particular importance for photoinduced charge transfer, because it is the key to control the direction of charge transfer and One of the important factors of efficiency. The unique properties of fullerenes come from their highly spherically symmetric three-dimensional cage structure, which makes the electrons of the whole molecule highly delocalized. Therefore, it can accelerate the light-induced charge separation and slow down the charge recombination in the donor and acceptor system. Fullerene has a high electron affinity (2.6-2.8eV) and a low reduction potential (0.61eV), and has multiple lowest occupied orbital LUMOs at the same time, making it a good choice whether in the ground state or in the excited state. acceptor of electrons or energy.

[0073] At the same time, high-performance photosensitizing dyes can be used to l...

Embodiment 2

[0096] PcZn / TiO 2 / C 60 (C(COOH) 2 ) 3 The photocatalytic reduction of nitrobenzene, the steps are as follows:

[0097] (1) The sample (15mg, 0.1mmol) synthesized in step 3 in Example 1 was added to methanol solution (1ml) containing nitrobenzene (0.05mmol), then 1.5mmol formic acid was added, and 30minN was introduced under dark conditions. 2 Finally, under the condition of stirring, the reaction was irradiated with λ>420nm visible light for 8 hours, and the conversion rate and selectivity of the reaction could be obtained by comparing the changes of the integrated areas of nitrobenzene and aniline before and after the reaction by using gas chromatography. The results are shown in Table 1.

[0098]

[0099] It can be seen from Table 1 that under the irradiation of visible light, the catalyst titanium dioxide does not reduce nitrobenzene, and the conversion rate is 0; Benzene is not reduced. After loaded with fullerene carboxylic acid derivatives and metal phthalocyan...

Embodiment 3

[0107] PcZn / TiO 2 / C 60 (C(COOH) 2 ) 3 Photocatalytic mechanism research, specific steps:

[0108] (1) Photocurrent test: the preparation of the working electrode, the steps are as follows:

[0109] The sample (3 mg) synthesized in Step 3 of Example 1 was sonicated in 0.5 ml ethanol solution for 15 min, and then stirred at room temperature for 12 h. Then take 10 μl of the suspension and drop it on a 1cm*1cm conductive glass, and finally dry the coated conductive glass in a 110 drying oven for 12 hours.

[0110] A platinum sheet (1cm*1cm) was used as a counter electrode, an Ag / AgC electrode was used as a reference electrode, and the working electrode prepared in Step 1 of Example 3 together constituted a three-electrode system, and 0.5M sodium sulfate solution was used as an electrolyte for photocurrent testing. Visible light with λ>420nm is used as the light source, and the test is carried out in constant voltage mode. Test results such as Figure 9 .

[0111] Figure...

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Abstract

The embodiment of the invention relates to fullerene carboxylic acid derivative / photosensitizer / titanium dioxide as well as a preparation method and application. The composite material is prepared from materials including titanium dioxide with -OH on surface, fullerene carboxylic acid derivative and a photosensitizer, wherein the fullerene carboxylic acid derivative is connected with titanium dioxide with -OH on surface by an ester bond, the photosensitizer is physically adsorbed to the surfaces of the fullerene carboxylic acid derivative and titanium dioxide, and the ester bond is formed by -COOH in the fullerene carboxylic acid derivative and -OH on the surface of titanium dioxide. The composite material can be used as a photocatalyst, and when being used as the photocatalyst, the photocatalyst is novel in structure, not only is the spectral absorption scope effectively widened, and light utilization efficiency increased, but also separation efficiency of electrons and holes is increased by fullerene, and great promotion of the photocatalysis performance is facilitated.

Description

technical field [0001] The invention relates to the application of fullerene materials in the field of photocatalysis, in particular to a fullerene carboxylic acid derivative / photosensitizer / titanium dioxide composite material and a preparation method and application thereof. Background technique [0002] Photocatalysis can not only realize many reactions that are difficult or impossible to carry out in ordinary experiments under normal temperature and pressure, but also does not produce secondary pollution in the process of completely mineralizing organic pollutants and has a long service life. These advantages make photocatalysis show out superiority. Using titanium dioxide as a photocatalyst to oxidize and degrade environmental organic matter by photocatalysis is a treatment technology that has received increasing attention in recent years. This process does not require other co-catalysts, can directly use oxygen in the air, and uses a light source with low energy to mak...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J31/38C07C209/80C07C211/46C07C211/47C07C211/45C07C211/52C07C221/00C07C223/06C07C253/30C07C255/58
CPCC07C209/80C07C221/00C07C253/30B01J31/183B01J31/38B01J2531/26B01J2531/025B01J2231/641B01J35/39C07C211/46C07C211/47C07C211/45C07C211/52C07C223/06C07C255/58
Inventor 王春儒吴波田建蕾
Owner INST OF CHEM CHINESE ACAD OF SCI
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