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One-step synthesis method of nitrogen-and-sulfur co-doped titanium dioxide/graphene quantum dot heterostructure

A technology of graphene quantum dots and titanium dioxide, applied in chemical instruments and methods, chemical/physical processes, water treatment of special compounds, etc., can solve the problems of multi-energy and consumption, and achieve the effect of small loss rate and favorable catalytic performance

Active Publication Date: 2017-06-20
JILIN UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

However, the tedious preparation and compounding process requires more energy

Method used

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  • One-step synthesis method of nitrogen-and-sulfur co-doped titanium dioxide/graphene quantum dot heterostructure
  • One-step synthesis method of nitrogen-and-sulfur co-doped titanium dioxide/graphene quantum dot heterostructure
  • One-step synthesis method of nitrogen-and-sulfur co-doped titanium dioxide/graphene quantum dot heterostructure

Examples

Experimental program
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Effect test

Embodiment 1

[0026] Preparation of nitrogen, sulfur co-doped titanium dioxide, nitrogen, sulfur co-doped graphene quantum dot composite material NSTG (2:1)

[0027] (1) According to the molar ratio of citric acid and thiourea being 2:1, weigh 0.42g of citric acid and 0.08g of thiourea.

[0028] (2) Add the powder weighed in step 1 into 8ml of dimethylformamide solution in sequence, and stir rapidly until it is completely dissolved.

[0029] (3) Weigh 100 mg of titanium dioxide (P25) powder, slowly add it into the solution obtained in step 2, and stir rapidly until it becomes a suspension.

[0030] (4) Transfer the suspension obtained in step 3 to a 40ml reaction kettle, and react at 180°C for 6 hours.

[0031] (5) Naturally cool to room temperature, remove the reaction kettle, and centrifuge the precipitate at 8500 rpm for 20 minutes to obtain a gray sample.

[0032] (6) The sample obtained in step 5 was washed twice with ethanol at 8500 rpm for 10 minutes, and the supernatant was discar...

Embodiment 2

[0038] In Example 1, change step 1 to: according to the molar ratio of citric acid and thiourea being 1:1, weigh 0.42 g of citric acid and 0.15 g of thiourea. The rest of the steps are consistent with Example 1. Finally, the sample NSTG (1:1) was prepared. The photocatalytic degradation dye performance test process is the same as step 9 of Example 1.

[0039] image 3 It is the TEM picture of the sample prepared in Example 2. Under low magnification, it can be seen that nitrogen-sulfur-doped titanium dioxide exists in the form of nanoparticles, and nitrogen-sulfur-doped graphene quantum dots are tightly attached due to the small size (about 5nm) On the titanium dioxide surface, a heterojunction is formed. At high resolution, the exposed (101) crystal plane of titanium dioxide can be clearly seen. Due to the effect of heterojunction, the (1120) crystal plane of nitrogen-sulfur-doped graphene quantum dots is closely connected, and the two crystal planes cooperate The effect ...

Embodiment 3

[0042]In Example 1, change step 1 to: according to the molar ratio of citric acid and thiourea being 1:3, weigh 0.42 g of citric acid and 0.46 g of thiourea. The rest of the steps are consistent with Example 1. Finally, the sample NSTG (1:3) was prepared. The photocatalytic degradation dye performance test process is the same as step 9 of Example 1.

[0043] Figure 4 It is the N 1s and S 2p high-resolution characterization of the sample prepared in Example 2. Under the high-resolution N 1s, 399.2, 399.7, 400.3, and 401.3 eV correspond to C-N-C, O-Ti-N, N-H, and Ti-O-N bonds, respectively. Under the high resolution of S 2p, 163.6, 164.7, 168.3, 169.6eV correspond to S 2p respectively 3 / 2 , S 2p 1 / 2 , S=O, S-O bonding, side proof, the sample prepared in Example 3 is a heterojunction of nitrogen-sulfur-doped titanium dioxide and nitrogen-sulfur-doped graphene quantum dots, and there is a strong chemical bond between the heterojunctions It is beneficial to improve the stabil...

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Abstract

The invention discloses a one-step synthesis method of nitrogen-and-sulfur co-doped titanium dioxide / graphene quantum dot heterostructure. The preparation method disclosed by the invention can synthesize a co-doped modified binary system through one step, and enable nitrogen-and-sulfur co-doped titanium dioxide and nitrogen-and-sulfur co-doped graphene quantum dots to be closely compounded together through a stronger chemical bond. The one-step synthesis method is mainly applied to the field of photocatalytic degradation; methylene blue is degraded under visible light; the photocatalysis performance of the composite material is detected through a degrading curve. Compared with the photocatalysis performance of single titanium dioxide, the photocatalysis performance of the composite material is substantially improved due to the excellent visible catalysis activity, and the composite material is environmentally friendly, cannot introduce heavy metal ions, cannot lead to secondary pollution to treated water resources, and is high in circulating stability.

Description

technical field [0001] The invention belongs to the technical field of nanomaterial preparation, and in particular relates to a preparation method for one-step synthesis of nitrogen-sulfur co-doped titanium dioxide / nitrogen-sulfur co-doped graphene quantum dot composite material and its photocatalytic degradation application. [0002] technical background [0003] With the development of industrialization, environmental problems have become an important factor restricting economic development. Especially for water pollution, it affects people's lives. Due to the massive discharge of organic dyes in industry, serious water pollution problems are caused. Moreover, there are many kinds of dyes, which are highly polluting and difficult to completely degrade. Therefore, there is an urgent need for a catalyst with wide application range, low raw material cost, wide sources and no secondary pollution. Titanium dioxide is the most widely used catalyst in industry due to its strong...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24C09K11/65B82Y40/00C02F1/30C02F101/30
CPCC09K11/0883C09K11/65B82Y40/00C02F1/30B01J27/24C02F2305/10C02F2101/308B01J35/39
Inventor 田宏伟沈凯郑伟涛
Owner JILIN UNIV
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