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Carbon nitride quantum dot/oxide nano fiber composite photocatalytic material and preparation method thereof

A technology of composite photocatalysis and nanofibers, which is applied in the field of preparation of composite photocatalytic materials, can solve the problems of uneven distribution of quantum dots, long time-consuming mechanical mixing method, poor dispersion of quantum dots, etc., and achieves simple and easy method and uniform composite The effect of improved efficiency and low cost of sex and compound

Active Publication Date: 2021-03-19
YANCHENG INST OF TECH
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Problems solved by technology

[0004] The Chinese invention patent with the authorized announcement number CN106268900B discloses a g-C 3 N 4 Quantum dot sensitized AgVO 3 Preparation method of nanowires; literature "Monodisperse g-C 3 N 4 Synthesis of quantum dot-modified one-dimensional rod-like BiPO4 crystallites and its mechanism for enhancing photocatalytic activity” reported a g-C 3 N 4 One-dimensional rod-like BiPO modified with quantum dots 4 Photocatalysts (see ChineseJournal of Inorganic Chemistry 32(2016) 1246-1254), these methods usually first synthesize g-C in the preparation process 3 N 4 Quantum dots, and then prepare the final composite photocatalyst by hydrothermal method, mechanical mixing method and other methods. Among them, the hydrothermal method requires high experimental equipment, the mechanical mixing method takes a long time, the composite efficiency is low, and the distribution of quantum dots after composite uneven, easy to fall off
In addition, the one-dimensional oxides synthesized by these methods are mostly nanowires and nanorods with relatively small length and diameter, which are still powder materials from a macroscopic point of view, and there are problems of difficult separation and recovery during use and high recycling costs.
[0005] Literature "Hybridization of g-C 3 N 4 quantum dots with 1D branched TiO 2 Fiber for efficient visible light-driven photocatalytic hydrogen generation" reported the use of electrospinning technology and alkaline hydrothermal method to prepare branched TiO 2 nanofibers were then deposited on TiO by chemical vapor deposition 2 Nanofiber surface attachment g-C 3 N 4 Quantum dots (see International Journal of HydrogenEnergy 45(2020) 13994-14005), although this method can realize g-C 3 N 4 The preparation and recombination of quantum dots on the surface of nanofibers, but the prepared g-C 3 N 4 Quantum dots have poor dispersion and low loading
In addition, branched TiO was prepared by alkaline hydrothermal method 2 Nanofibers, the reaction conditions are harsh, and the requirements for experimental equipment are high. At the same time, the prepared fibers have problems such as poor continuity and low strength.

Method used

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  • Carbon nitride quantum dot/oxide nano fiber composite photocatalytic material and preparation method thereof
  • Carbon nitride quantum dot/oxide nano fiber composite photocatalytic material and preparation method thereof
  • Carbon nitride quantum dot/oxide nano fiber composite photocatalytic material and preparation method thereof

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preparation example Construction

[0045]Preparation method of a carbon nitride quantum dot / oxide nanofiber composite photocatalytic material of the present invention, including the following steps:

[0046](1) Preparation of precursor solution

[0047]After mixing the polymer and the solvent was stirred for 1 to 6 h (e.g., 1H, 2H, 3H, 4H, 5H, 6H), and then slowly added a metal salt, stirring was continuously stirred at room temperature or ice water bath (for example, 0.5h, 1H, 1.5H, 2H), where the mass ratio of the polymer, solvent and the metal salt is 1: (5 ~ 20): (, 1 to 10) (for example, 1: 5: 1, 1: 20: 10, 1: 12: 5, 1: 8: 2, 1: 10: 4, 1: 12: 6), polymers are polyvinylpyrrolidone, polyacrylonitrile, polyvinyl butyral, polyethylene oxide, polystyrene At least one of the medium, the solvent is water, ethanol, acetic acid, acetone, N, N-dimethylformamide; metal salt is isopropyl titanate, tetrabutyl titanate, titanium tetrachloride , Manganese chloride, manganese sulfate, iron chloride, iron nitrate, cobalt chloride, c...

Embodiment 1

[0059]The method of preparing the carbon nitride quantum dot / oxide nanofiber composite photocatalytic material of the present embodiment includes the following steps:

[0060](1) Preparation of precursor solution

[0061]The polymer polyvinylpyrrolidone was mixed with the solvent ethanol for 1 h, then the metal saline titanate was slowly added, and the precursor solution was stirred for 0.5 h, wherein the mass ratio of the polymer, solvent, and metal salt is 1: 5: 1;

[0062](2) Preparation of oxide nanofibers

[0063]The precursor solution was prepared by electrostatic spinning, followed by calcination under the air atmosphere, to obtain oxide nanofibers, wherein the conditions of electrostatic spinning are: temperature 20 ° C, relative humidity is 20%, The spinning voltage is 50 kV, the perfusion speed is 10 ml / h, the fiber collecting device and the nozzle distance are 40 cm, and the conditions of calcination are: calcination temperature is 0.5 ° C / min, the temperature is 300 min;

[0064]...

Embodiment 2

[0074](1) Preparation of precursor solution

[0075]The polymer polypropylene nitrile was mixed with solvent N, N-dimethylformamide was mixed after 6 h, and then the tetrabutyl titanate titanate was slowly added, and the agitate for 2 h. The precursor solution was continuously stirred, wherein the polymer, solvent, metal The mass ratio of the salt is 1:20:10;

[0076](2) Preparation of oxide nanofibers

[0077]The above precursor solution was prepared by electrostatic spinning, followed by calcination under the air atmosphere, to obtain oxide nanofibers, wherein the conditions of electrostatic spinning: temperature 30 ° C, relative humidity of 70%, The spinning voltage is 10 kV, the perfusion speed is 0.1 ml / h, the fiber collecting device and the nozzle distance are 10 cm; the calcination conditions are: calcination temperature 1000 ° C, the temperature of the temperature is 10 ° C / min, the holding time is 10 min;

[0078](3) Preparation of a carbon nitride nanoflake

[0079]The mixture was mi...

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Abstract

The invention belongs to the technical field of preparation of composite photocatalytic materials, and particularly relates to a carbon nitride quantum dot / oxide nano fiber composite photocatalytic material and a preparation method thereof. The preparation method comprises the following steps: preparing a precursor solution from a polymer, a solvent and a metal salt, carrying out electrostatic spinning and calcining on the precursor solution to obtain oxide nano fibers, preparing carbon nitride nano sheets, respectively placing the oxide nano fibers and the carbon nitride nano sheets at the outlet end and the inlet end of a tubular furnace, and carrying out heat treatment on the inlet end under an inert atmosphere conveying condition to obtain the composite photocatalytic material. The preparation and compounding of the carbon nitride quantum dots are realized in one step by adopting a thermal stripping in-situ deposition method, compared with an existing hydrothermal method and mechanical mixing method, the compounding uniformity and compounding efficiency are obviously improved, the prepared composite material is stable in structure, the problem that the quantum dots are not easyto compound is solved, and the method is simple and easy to implement and low in cost.

Description

Technical field[0001]The present invention belongs to the preparation of composite photocatalytic materials, and in particular, the present invention relates to a carbon nitride quantum dot / oxide nanofiber composite photocatalytic material and a preparation method thereof.Background technique[0002]Semiconductor photocatalytic technology, as a green environmental protection technology, it has an important value in environmental pollution control and clean energy development. In many photocatalytic materials, carbon nitride (G-C3N4) Because of its advantages such as suitable band structure, good stability, low cost, safe and non-toxic, etc., has been widely studied and concerned in recent years. However, a single component G-C3N4There is a problem of low sunlight utilization rate, high carrier composite rate, resulting in G-C3N4The photocatalytic activity is low, thereby limiting its wide application. Therefore, G-C3N4Modification is carried out to improve its photocatalytic perform...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/24B01J37/03
CPCB01J27/24B01J37/031B01J35/39
Inventor 宋骏关荣锋杨秀丽解明华董鹏玉邵荣
Owner YANCHENG INST OF TECH
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