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Preparation method for controlling particle size of silver phosphate crystals by using carbon nanotubes

A technology of carbon nanotubes and crystal particle size, which is applied in chemical instruments and methods, physical/chemical process catalysts, chemical/physical processes, etc., can solve the problems that hinder the popularization and application of Ag, irregular shape, large particle size, etc. Achieve excellent visible light catalytic performance, simple preparation method, simple and easy operation

Inactive Publication Date: 2018-11-30
HUNAN UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

But Ag 3 PO 4 The photocatalytic activity is closely related to its crystal size and morphology, and it is very easy to appear Ag in the preparation process. 3 PO 4 Defects with uncontrollable crystal size and irregular morphology, especially tend to generate Ag with large particle size and low photocatalytic activity 3 PO 4 the crystal
This defect directly affects the Ag 3 PO 4 photocatalytic activity, and severely hindered the Ag 3 PO 4 Promoted application of

Method used

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  • Preparation method for controlling particle size of silver phosphate crystals by using carbon nanotubes
  • Preparation method for controlling particle size of silver phosphate crystals by using carbon nanotubes
  • Preparation method for controlling particle size of silver phosphate crystals by using carbon nanotubes

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Embodiment 1

[0026] A preparation method utilizing carbon nanotubes to control the grain size of silver phosphate crystals, the steps are as follows:

[0027] (1) Weigh 1g of multi-walled carbon nanotubes (MWCNTs) in 350mL HNO 3 In the solution, reflux treatment was carried out under the condition of 120° C. while stirring, and the treatment time was 8 hours. After reflux, it was washed with ultrapure water until neutral, and dried in vacuum at 70°C.

[0028] (2) Weigh 0.0012g of MWCNTs obtained by drying into 40mL of ultrapure water, and sonicate for 3h.

[0029] (3) Weigh 1.53g AgNO 3 Dissolve in 30mL ultrapure water, add the solution dropwise to the above solution, and keep stirring in the dark for 12h;

[0030] (4) Weigh 1.074gNa 2 HPO 4 12H 2 O was dissolved in 30 mL of ultrapure water, and the solution was added dropwise to the solution obtained in step (3), and stirred for 6 h in the dark. The solid-liquid mixture was centrifuged, washed with ethanol and ultrapure water for 3...

Embodiment 2

[0036] The prepared Ag 3 PO 4 Monomer and Ag 3 PO4 @0.1%MWCNTs composite photocatalyst was used for the degradation of phenol to evaluate its photocatalytic activity. Accurately weigh 50 mg of the prepared materials into 100 mL of phenol solution with a concentration of 20 mg / L, stir continuously, and carry out the degradation reaction under the irradiation condition of 300W xenon lamp (λ>420nm). The solutions with different reaction times were taken for concentration determination, and the results were as follows: Figure 5 shown. It can be clearly seen that Ag 3 PO 4 The degradation ability of @MWCNTs is significantly better than that of Ag 3 PO 4 monomer. Image 6 for Ag 3 PO 4 and Ag 3 PO 4 The reaction kinetic curve corresponding to the degradation curve of phenol by @MWCNTs. As shown, the rate constant changes from 0.015min -1 Increase to 0.35min -1 , the photocatalytic rate of the composite photocatalyst is 19.4 times that of the monomer.

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Abstract

The invention discloses a reparation method for controlling the particle size of silver phosphate crystals by using carbon nanotubes. The method comprises the following steps: (1) placing the carbon nanotubes in concentrated nitric acid, carrying out heating refluxing treatment for 6-12 h, cooling the obtained product, washing the cooled product with water until the cooled product is neutral, anddrying the product; (2) weighing a certain amount of the dried carbon nanotubes, adding the dried carbon nanotubes into ultrapure water, and carrying out ultrasonic treatment for 2-5 h; (3) dropwise adding a AgNO3 solution into the above obtained solution, and stirring the obtained solution in a shady place for 6-20 h; and (4) dropwise adding a Na2HPO4.12H2O solution into a solution obtained in step (3), stirring the obtained solution in a shady place for 1-6 h, washing the obtained product with water and ethanol multiple times, carrying out centrifugal separation to obtain a solid part, and carrying out vacuum drying to prepare carbon nanotube modified silver phosphate crystals with the particle size of 0.38-1.0 [mu]m. The preparation method is simple, and changes Ag3PO4 crystals with anaverage particle size of 20 [mu]m into small-granule crystals with an average particle size of 0.38-1.0 [mu]m. The prepared small-grain Ag3PO4@MWCNTs composite catalyst has an excellent visible photocatalysis performance.

Description

technical field [0001] The invention belongs to the technical field of preparation of semiconductor photocatalytic materials, and in particular relates to a preparation method for controlling the grain size of silver phosphate crystals by using carbon nanotubes. Background technique [0002] In recent decades, silver phosphate (Ag 3 PO 4 ) has attracted extensive attention due to its excellent ability to degrade organic pollutants. Ag 3 PO 4 The unique energy band position makes the photogenerated holes in the valence band have strong oxidation ability, which can directly oxidize and degrade pollutants. But Ag 3 PO 4 The photocatalytic activity is closely related to its crystal size and morphology, and it is very easy to appear Ag in the preparation process. 3 PO 4 Defects with uncontrollable crystal size and irregular morphology, especially tend to generate Ag with large particle size and low photocatalytic activity 3 PO 4 crystals. This defect directly affects t...

Claims

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Application Information

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IPC IPC(8): B01J27/18B01J35/02
CPCB01J27/1817B01J35/50B01J35/40B01J35/39
Inventor 杨春平林燕李翔吴少华陈明周琦陈玉娟
Owner HUNAN UNIV
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