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Method for one-pot synthesis of regular-morphology sulfide-TiO2 composite nanostructure by solvothermal method and application thereof

A technology of composite nanostructure and solvothermal method, applied in chemical instruments and methods, catalyst activation/preparation, chemical/physical processes, etc. There are many factors affecting the method, so as to achieve the effect of improving photocatalytic performance, regular product morphology, and easy large-scale production

Active Publication Date: 2020-05-08
SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

There are many factors affecting the electrospinning method, and it is easily affected by the environment and reaction conditions, so it is difficult to be used in industrial production
[0008] 4) Chemical bath deposition method: Chinese invention patent application CN 102024572 A first prepares porous TiO 2 materials, and then prepared PbS quantum dot co-sensitized porous TiO by chemical bath deposition 2 Composite material, its shape is irregular, the stability of the composite nanostructure is poor, and it is synthesized by a two-step method
The chemical bath deposition method is mainly used for solution growth, controlled precipitation or simple chemical deposition, but its chemical reaction process is relatively slow

Method used

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  • Method for one-pot synthesis of regular-morphology sulfide-TiO2 composite nanostructure by solvothermal method and application thereof
  • Method for one-pot synthesis of regular-morphology sulfide-TiO2 composite nanostructure by solvothermal method and application thereof
  • Method for one-pot synthesis of regular-morphology sulfide-TiO2 composite nanostructure by solvothermal method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0049] Example 1: One-pot synthesis of regular shape sulfide-TiO with a mass percentage of 1% by solvothermal method 2 Composite nano solid spheres, the specific steps are as follows:

[0050] 1g of titanium compound (this experiment is TiS 2 ) into 50mL of ethylene glycol solution containing 0.0117g metal salt (this experiment is cadmium nitrate ethylene glycol solution), and then add a certain amount of ammonium fluoride to it to make the solution pH ≈ 3-4, and magnetically stir for 0.5h Finally, the mixed solution was transferred to a 100mL autoclave liner, sealed and placed in an oven at 200°C for 12 hours. After the reaction was completed, it was naturally cooled to room temperature, and the obtained precipitate was washed with absolute ethanol and deionized water several times until the eluate was neutral (pH=7). % sulfide-TiO 2 One-component composite nano-solid sphere CdS-TiO 2 , denoted as S1, where 1% by mass is sulfide and TiO 2 The mass ratio of the specific e...

Embodiment 2

[0057] Example 2: Solvothermal one-pot synthesis of regular shape sulfide-TiO with a mass percentage of 2% 2 Composite nano solid spheres are prepared by the following method:

[0058] 1g TiS 3 Add 50mL of ethylene glycol solution containing 0.0177g of cadmium acetate into a polytetrafluoroethylene beaker, and then add a certain amount of ammonium chloride to it to make the solution pH ≈ 3-4. After magnetic stirring for 0.5h, transfer the mixed solution to 100mL In the liner of the high-pressure reactor, after sealing, place it in an oven at 200°C for 12 hours. After the reaction was completed, it was naturally cooled to room temperature, and the obtained precipitate was washed several times with absolute ethanol and deionized water until the eluate was neutral (pH=7). After vacuum drying at 60°C for 12 hours, a mass percent of % sulfide-TiO 2 One-component composite nano-solid sphere CdS-TiO 2 , denoted as S6.

[0059] The ethylene glycol solution of above-mentioned cadm...

Embodiment 3

[0063]Example 3: One-pot synthesis of regular shape sulfide-TiO with a mass percentage of 3% by solvothermal method 2 Nano hollow sphere / hollow box is prepared by the following method:

[0064] 1g TiS 2 Add 50mL of ethylene glycol solution containing 0.0273g of cadmium chloride into a polytetrafluoroethylene beaker, and then add a certain amount of ammonium chloride to it to make the solution pH ≈ 3-4, and after magnetic stirring for 0.5h, transfer the mixed solution to Place in a 100mL autoclave liner, seal and place in an oven at 200°C for 12 hours. After the reaction was completed, it was naturally cooled to room temperature, and the obtained precipitate was washed with absolute ethanol and deionized water several times until the eluate was neutral (pH=7). After vacuum drying at 60° C. for 12 hours, the obtained precipitate was 3% by mass. The composite nano-solid box CdS-TiO 2 , denoted as S11.

[0065] The ethylene glycol solution of the above-mentioned cadmium chlori...

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Abstract

The invention relates to the technical field of photocatalyst preparation and pesticide degradation, in particular to a method for synthesizing a regular-morphology unitary, binary or ternary sulfide-TiO2 composite nanostructure in a one-pot mode through a solvothermal method and application thereof in photocatalytic degradation of organic pesticides. Because the raw materials not only can providea titanium source, but also can provide a sulfur source, the sulphide-TiO2 composite nanostructure with regular morphology is prepared by adopting a solvothermal method one-pot synthesis technology.The sulphide-TiO2 composite nano-structure prepared by the preparation method disclosed by the invention has the advantages that active species are generated through optical excitation; toxic pesticides such as .OH and .O2- and the like can be decomposed into small molecules or non-toxic compounds, residues of the toxic pesticides are effectively reduced, the production safety is improved, variousorganic pesticides can be degraded, the broad spectrum property is high, the effect is good, and good application prospects are achieved in the aspects of pesticide greening, low residues and the like.

Description

technical field [0001] The invention relates to the technical field of photocatalyst preparation and pesticide degradation, in particular to a one-pot synthesis of regular-shaped sulfide-TiO by solvothermal method 2 Methods of composite nanostructures and their application in photocatalytic degradation of organic pesticides. Background technique [0002] TiO 2 As a semiconductor material, it has the advantages of non-toxicity, good chemical stability, and high oxidation activity. It is currently mostly used in organic wastewater treatment, carbon dioxide reduction, hydrogen production, and solar cells. TiO 2 As a photocatalyst, ultraviolet light can be used as a light source to perform photocatalytic degradation reactions with organic pollutants. TiO 2 The photocatalyst is excited to form electron-hole pairs, and the photogenerated holes interact with H 2 O, OH － The action produces highly oxidizing OH, photogenerated electrons and O 2 form superoxide radicals, which e...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): B01J27/04B01J35/08B01J37/08C02F1/30C02F101/30
CPCB01J27/04B01J37/08C02F1/30C02F2305/10C02F2101/306B01J35/51B01J35/39B01J35/40
Inventor 陈连清韦晓珊
Owner SOUTH CENTRAL UNIVERSITY FOR NATIONALITIES
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