CN111558389B - BiVO4Protonated g-C3N4AgI ternary composite photocatalyst and preparation method thereof - Google Patents

BiVO4Protonated g-C3N4AgI ternary composite photocatalyst and preparation method thereof Download PDF

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CN111558389B
CN111558389B CN202010403360.1A CN202010403360A CN111558389B CN 111558389 B CN111558389 B CN 111558389B CN 202010403360 A CN202010403360 A CN 202010403360A CN 111558389 B CN111558389 B CN 111558389B
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杨静凯
许敏
梁波
孙朝阳
赵洪力
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Abstract

The invention discloses a BiVO4Protonated g-C3N4Firstly, BiVO is respectively prepared by a hydrothermal method and a calcination method4And protonation of g-C3N4Then preparing BiVO by an electrostatic self-assembly method4Protonated g-C3N4Composite material, and further BiVO prepared by in-situ precipitation method4Protonated g-C3N4the/AgI ternary composite photocatalyst. The ternary composite photocatalyst prepared by the invention can rapidly separate photoproduction electrons and holes, improve the service life of photoelectrons, reduce the recombination rate of the photoproduction electrons and the holes, has good response to visible light, has a degradation rate of rhodamine B solution reaching 94.7 percent after catalytic reaction for 60min, can be used for degrading water pollutant organic dyes under visible light, and has important significance on environmental management.

Description

BiVO4Protonated g-C3N4AgI ternary composite photocatalyst and preparation method thereof
Technical Field
The invention relates to the technical field of photocatalysts, in particular to BiVO4Protonated g-C3N4a/AgI ternary composite photocatalyst and a preparation method thereof.
Background
The photocatalysis technology using semiconductor oxide as main body is characterized by that it has no pollution and can implement workThe method has the advantages of simple process, capability of directly utilizing solar energy as a reaction light source, capability of producing clean energy and the like, and becomes an effective technology for treating environmental pollutants at present. BiVO4As a novel semiconductor material, the photocatalyst has a narrow band gap (about 2.40 eV), excellent visible light response and proper conduction band and valence band positions (compared with a standard hydrogen electrode), and is an effective semiconductor photocatalyst with the capabilities of photolyzing water to generate oxygen, reducing and degrading pollutants. However, BiVO4The photocatalyst has the characteristics of poor charge transport capacity, fast combination, poor adsorptivity and the like, and the photocatalytic activity of the photocatalyst is limited. BiVO4Constructing a suitable heterojunction photocatalytic system with other semiconductors is considered an effective strategy to further enhance photocatalytic activity. In addition, research has proved that the preparation of a proper ternary heterojunction is more beneficial to enhancing the visible light response capability and charge carrier separation, so that the heterojunction has higher photocatalytic activity.
The two-dimensional material (2D) has various excellent characteristics such as high charge mobility and tunable electronic characteristics. In recent years, carbon nitride (g-C)3N4) As a new member of the 2D family, the advantages of high chemical stability, low production cost and the like are attracted by wide attention due to a highly delocalized conjugated system. For example, WO of Tingting Xiao obtained by precise control of in situ hydrolysis and continuous polymerization3/g-C3N4，WO3And g-C3N4The synergistic effect between the two increases the interface charge transmission efficiency and the number of oxidation-reduction active sites, thereby effectively increasing the catalytic activity of the photocatalyst (appl.Catal.B.220(2018) 417-. In addition, researchers are working on g-C3N4Modified BiVO4The research is carried out, Ying Wang et al obtain BiVO by an ultrasonic dispersion method4/g-C3N4The photocatalyst has good photocatalytic degradation activity on rhodamine B in sewage (Appl. Catal. B.234(2018) 37-49). Silver iodide (AgI) having excellent redox ability at the same time has been widely used in the field of photocatalysis. However, AgI tends to be irregular spherical particles and tends to agglomerate, preventing its high catalytic activity. Compounding AgI with other semiconductorsHeterojunction is an effective strategy to solve this problem. Fei Chen et al demonstrate BiVO4Heterostructure-promoted photoelectron transfer and enhanced photocatalytic activity in AgI photocatalyst systems (ACS appl. Mater. Inter.8(2016) 32887-32900).
BiVO prepared according to previous studies4/g-C3N4And BiVO4the/AgI composites have all shown a significantly enhanced photocatalytic activity. In particular, g-C3N4AgI has strong reducing power and BiVO4Has strong oxidizing ability and the band structures of the two materials are matched with each other. Taking into account g-C3N4And AgI, we believe that they together modify BiVO4May be an effective strategy to build a good photocatalyst. So far, BiVO has not yet been provided4And g-C3N4Research and public report on constructing photocatalyst by compounding with AgI, so that BiVO is prepared4Protonated g-C3N4the/AgI ternary composite photocatalyst improves the performance of photocatalytic degradation of water pollutant organic dye by visible light.
Disclosure of Invention
The invention aims to provide a heterojunction photocatalyst which can promote efficient charge separation and has high photocatalytic activity and a preparation method thereof. The method has the advantages of simple operation, short reaction time, mild reaction conditions and prepared BiVO4Protonated g-C3N4The AgI ternary composite photocatalyst has high degradation activity under the irradiation of visible light, and has wide application prospects in the fields of environmental pollution control, energy sources and the like.
In order to achieve the purpose, the technical scheme of the invention is as follows:
the invention provides a BiVO4Protonated g-C3N4the/AgI ternary composite photocatalyst comprises BiVO4Protonated g-C3N4And AgI, wherein the composite photocatalyst is prepared by the following steps:
(1) preparation of BiVO4Powder: adding Bi (NO)3)3·5H2Dissolving O in deionized water, and fully stirring to form solution A; reacting NH4VO3Dissolving in deionized water, and fully stirring to form a solution B; slowly pouring the solution B into the solution A, continuously stirring to form a yellow mixture suspension, adjusting the pH value to 7-9 by using ammonia water, and fully stirring to obtain BiVO4A precursor solution of BiVO4Pouring the precursor solution into a hydrothermal reaction kettle with the filling degree of 70%, heating to 180 ℃, carrying out heat preservation reaction for 12 hours, cooling the reaction kettle to room temperature, washing and drying to obtain BiVO4Powder;
(2) preparation of protonated g-C3N4Powder: putting melamine into a muffle furnace, calcining at the heating rate of 4 ℃/min to 550 ℃, calcining for 4 hours, cooling to room temperature, grinding to obtain g-C3N4(ii) a The g-C obtained3N4Dispersing in 37% hydrochloric acid solution, ultrasonic treating for 60min, stirring for 60min, washing, and drying to obtain protonated g-C3N4；
(3) BiVO with a certain mass ratio4And protonation of g-C3N4Dissolving in ethanol, performing ultrasonic dispersion at room temperature, and stirring in a fume hood for 24 h; after ethanol volatilization, drying the obtained product at 60 ℃ for 12h to obtain BiVO4Protonated g-C3N4A composite material;
(4) BiVO (bismuth oxide) is added4Protonated g-C3N4Dissolving the composite material in deionized water, performing ultrasonic treatment at room temperature for 10min, and adding AgNO3Stirring the solution for 1h in the dark, dropwise adding a KI solution in the stirring process, continuously stirring for 1h, washing and drying to obtain BiVO4Protonated g-C3N4the/AgI ternary composite photocatalyst.
Preferably, Bi (NO) is used in the step (1)3)3·5H2O and NH4VO3Is 1: 1.
Preferably, in the step (2), the g-C3N4The dosage ratio of the hydrochloric acid solution to the hydrochloric acid solution is 1-4 g: 50-100 ml.
Preferably, in the step (3),the BiVO4Protonated g-C3N4The dosage ratio of the alcohol to the ethanol is 0.1-0.2 g:0.1g:100ml, and the ultrasonic dispersion time is 1-4 h.
Preferably, in the step (4), the BiVO4Protonated g-C3N4Composite material, deionized water and AgNO3The dosage ratio of the solution to the KI solution is 0.1g: 50 ml: 0.0851 mmol: 0.0851mmol of said AgNO3The concentration of the solution is 0.1mol/L, and the concentration of the KI solution is 0.1 mol/L.
Preferably, BiVO4Protonated g-C3N4The application of the AgI ternary composite photocatalyst in organic dye treatment.
The invention has the following effects:
1) the invention successfully prepares BiVO for the first time by adopting an electrostatic self-assembly method and an in-situ precipitation method4Protonated g-C3N4/AgI ternary composite photocatalyst and BiVO prepared by using same4Protonated g-C3N4AgI ternary composite photocatalyst and pure BiVO4Compared with the prior art, the photocatalyst has higher photoproduction electron-hole separation effect and electron migration capacity, thereby showing more efficient photocatalytic activity;
2) BiVO prepared by the invention4Protonated g-C3N4The AgI ternary composite photocatalyst can realize high-efficiency degradation of organic dye under visible light, and the degradation rate of the organic dye (rhodamine B) can reach more than 94% within 60min of illumination time;
3) BiVO provided by the invention4Protonated g-C3N4The preparation method of the AgI ternary composite photocatalyst is simple and easy to operate, low in cost and environment-friendly.
Drawings
FIG. 1 shows BiVO prepared in example 1 of the present invention4Protonated g-C3N4(pCN), AgI and BiVO4Protonated g-C3N4、BiVO4AgI and BiVO4Protonated g-C3N4XRD spectrum of the/AgI ternary composite material;
FIG. 2Is BiVO prepared in the embodiment 1 of the invention4Protonated g-C3N4TEM image of (pCN)/AgI ternary composite; and
FIG. 3 shows BiVO prepared in example 1 of the present invention4Protonated g-C3N4(pCN)、AgI、 BiVO4/pCN、BiVO4AgI and BiVO4And the effect diagram of the/pCN/AgI ternary composite material for degrading rhodamine B under the irradiation of visible light.
Detailed Description
Example 1:
(1) preparation of BiVO4Powder: weighing 10mmol of bismuth nitrate Bi (NO)3)3·5H2Dissolving O in 40ml deionized water, and fully stirring for 30min to form solution A; weighing 10mmol of ammonium metavanadate NH4VO3Dissolved in 40ml of deionized water and stirred well for 30min to form a solution B. Slowly pouring the solution B into the solution A, continuously stirring to form a yellow mixture suspension, adjusting the pH value to 7 by using ammonia water, and fully stirring for 30min to obtain BiVO4Precursor solution, prepared BiVO4Pouring the precursor solution into a hydrothermal reaction kettle with the filling degree of 70%, heating at 180 ℃ for 12h, cooling the reaction kettle to room temperature, washing and drying to obtain BiVO4；
(2) Preparation of protonated g-C3N4Powder: first of all 15g of melamine C will be charged3N3(NH2)3The crucible is put into a muffle furnace, calcined to 550 ℃ at the heating rate of 4 ℃/min, calcined for 4 hours, cooled to room temperature, and ground to obtain a sample of g-C3N4. Weighing 4g of g-C3N4Dissolving in 500ml of 37% hydrochloric acid solution, performing ultrasonic treatment for 60min, stirring for 60min, washing, and drying to obtain protonated g-C3N4；
(3) 0.1g of BiVO4And 0.1g protonated g-C3N4Dissolved in 100mL ethanol, sonicated for 1h at room temperature and stirred in a fume hood for 24 h. After ethanol volatilization, collecting the obtained product and drying at 60 ℃ for 12h to obtain BiVO4Protonated g-C3N4Composite material；
(4) 0.1g of BiVO4Protonated g-C3N4Dissolved in 50ml of deionized water and sonicated at room temperature for 10 min. Adding 851 mu L of 0.1mol/L AgNO3The solution was stirred in the dark for 1h, then 851. mu.L of 0.1mol/L KI solution was added dropwise during stirring, and stirring was continued for 1 h. After washing and drying, BiVO is obtained4Protonated g-C3N4the/AgI ternary composite material photocatalyst.
FIG. 1 is BiVO prepared in example 14Protonated g-C3N4(pCN)、AgI、BiVO4/pCN、 BiVO4AgI and BiVO4XRD pattern of/pCN/AgI, BiVO in the pattern4Diffraction peak and BiVO4The monoclinic phase (JCPDS No.14-0688) is corresponding to the crystal phase, and the characteristic diffraction peak is sharp, which shows that the sample prepared by the method is monoclinic phase BiVO with good crystallinity4. Protonation in the spectrum g-C3N4The two diffraction peaks at 27.46 DEG and 21.60 DEG are respectively assigned to g-C3N4(JCPDS No.87-1526) which is a layer-by-layer stacking of carbon nitride and a regular arrangement in the plane of the triazine ring. AgI diffraction peaks in the spectra correspond to AgI (JCPDS 09-0374). For the prepared BiVO4Protonated g-C3N4An XRD (X-ray diffraction) pattern of the/AgI ternary composite photocatalyst, wherein the pattern contains monoclinic phase BiVO4And all diffraction peaks of AgI, no protonated g-C detected3N4The diffraction peak of (2) is due to poor crystallization effect and small intensity after recombination.
FIG. 2 is BiVO prepared in example 14Protonated g-C3N4TEM atlas of (pCN)/AgI ternary composite photocatalyst, BiVO is observed4And AgI distribution in protonated g-C3N4The above.
FIG. 3 is BiVO prepared in example 14Protonated g-C3N4(pCN)、AgI、BiVO4/pCN、 BiVO4AgI and BiVO4And the effect diagram of the/pCN/AgI ternary composite photocatalyst for degrading rhodamine B under the irradiation of visible light is shown. BiVO4Protonated g-C3N4After the/AgI ternary composite photocatalyst is subjected to catalytic reaction for 60min, the degradation rate of the rhodamine B solution reaches 94.7%, which indicates that the prepared ternary composite photocatalyst has excellent photocatalytic activity under visible light.
Example 2:
(1) preparation of BiVO4Powder: weighing 10mmol of bismuth nitrate Bi (NO)3)3·5H2Dissolving O in 40ml of deionized water, and fully stirring for 30min to form solution A; weighing 10mmol of ammonium metavanadate NH4VO3Dissolved in 40ml of deionized water and stirred well for 30min to form a solution B. Slowly pouring the solution B into the solution A, continuously stirring to form a yellow mixture suspension, adjusting the pH value to 7 by using ammonia water, then fully stirring for 30min, and adding the prepared BiVO4Pouring the precursor solution into a hydrothermal kettle with the filling degree of 70%, heating at 180 ℃ for 12h, cooling the reaction kettle to room temperature, washing and drying to obtain BiVO4；
(2) Preparation of protonated g-C3N4Powder: first of all 15g of melamine C will be charged3N3(NH2)3The crucible is put into a muffle furnace, calcined to 550 ℃ at the heating rate of 4 ℃/min, calcined for 4 hours, cooled to room temperature, ground, and the obtained sample is g-C3N4. Weighing 4g of g-C3N4Dissolving in 500ml of 37% hydrochloric acid solution, performing ultrasonic treatment for 60min, stirring for 60min, washing, and drying to obtain protonated g-C3N4；
(3) 0.15g of BiVO4And 0.1g protonated g-C3N4Dispersed in 100mL of ethanol and sonicated for 1h at room temperature. After which it was stirred in a fume hood for 24 h. After ethanol volatilization, collecting the obtained product and drying at 60 ℃ for 12h to obtain BiVO4Protonated g-C3N4A composite material;
(4) 0.1g of BiVO4Protonated g-C3N4Sonication was carried out for 10min at room temperature, dispersed in 50ml of deionized water. Adding 851 mu L0.1mol/L AgNO3Stirring the solution for 1h in the dark, and then dropwise adding the solution during stirring851 mu L of a 0.1mol/L KI solution and stirring was continued for 1 h. After washing and drying, BiVO is obtained4Protonated g-C3N4the/AgI ternary composite photocatalyst.
After the catalyst obtained in the example 2 is subjected to catalytic reaction for 60min, the degradation rate of the rhodamine B solution reaches 92.5%.
Example 3:
(1) preparation of BiVO4Powder: weighing 10mmol of bismuth nitrate Bi (NO)3)3·5H2Dissolving O in 40ml of deionized water, and fully stirring for 30min to form solution A; weighing 10mmol of ammonium metavanadate NH4VO3Dissolved in 40ml of deionized water and stirred well for 30min to form a solution B. Slowly pouring the solution B into the solution A, continuously stirring to form a yellow mixture suspension, adjusting the pH value to 7 by using ammonia water, then fully stirring for 30min, and adding the prepared BiVO4Pouring the precursor solution into a hydrothermal kettle with the filling degree of 70%, heating at 180 ℃ for 12h, cooling the reaction kettle to room temperature, washing and drying to obtain BiVO4；
(2) Preparation of protonated g-C3N4Powder, first of all 15g of melamine C3N3(NH2)3The crucible is put into a muffle furnace, calcined to 550 ℃ at the heating rate of 4 ℃/min, calcined for 4 hours, cooled to room temperature, ground, and the obtained sample is g-C3N4. Weighing 4g of g-C3N4Dissolving in 500ml of 37% hydrochloric acid solution, performing ultrasonic treatment for 60min, stirring for 60min, washing, and drying to obtain protonated g-C3N4；
(3) 0.2g of BiVO4And 0.1g protonated g-C3N4Dispersed in 100ml ethanol and sonicated for 1h at room temperature. After which it was stirred in a fume hood for 24 h. After ethanol volatilization, collecting the obtained product and drying at 60 ℃ for 12h to obtain BiVO4Protonated g-C3N4A composite material;
(4) 0.1g of BiVO4Protonated g-C3N4Sonication was carried out for 10min at room temperature with dispersion in 50mL of deionized water. Adding 851 mu L0.1mol/L ofAgNO3The solution was stirred in the dark for 1h, then 851. mu. L of 0.1mol/L KI solution was added dropwise during stirring, and stirring was continued for 1 h. After washing and drying, BiVO is obtained4Protonated g-C3N4the/AgI ternary composite photocatalyst.
After the catalyst obtained in example 3 is subjected to catalytic reaction for 60min, the degradation rate of the rhodamine B solution reaches 90.3%.
The above-mentioned embodiments are merely illustrative of the preferred embodiments of the present invention, and do not limit the scope of the present invention, and various modifications and improvements made to the technical solution of the present invention by those skilled in the art without departing from the spirit of the present invention shall fall within the protection scope defined by the claims of the present invention.

Claims (3)

1. BiVO4Protonated g-C3N4the/AgI ternary composite photocatalyst is characterized in that: the composite photocatalyst comprises BiVO4Protonated g-C3N4And AgI, wherein the composite photocatalyst is prepared by the following steps:
(1) preparation of BiVO4Powder: adding Bi (NO)3)3·5H2Dissolving O in deionized water, and fully stirring to form solution A; reacting NH4VO3Dissolving in deionized water, and fully stirring to form a solution B; slowly pouring the solution B into the solution A, continuously stirring to form a yellow mixture suspension, adjusting the pH value to 7-9 by using ammonia water, and fully stirring to obtain BiVO4A precursor solution of BiVO4Pouring the precursor solution into a hydrothermal reaction kettle with the filling degree of 70%, heating to 180 ℃, carrying out heat preservation reaction for 12 hours, cooling the reaction kettle to room temperature, washing and drying to obtain BiVO4Powder, BiVO prepared therefrom4Is monoclinic phase BiVO with good crystallinity4；
Bi (NO) in the step (1)3)3·5H2O and NH4VO3In a molar ratio of 1: 1;
(2) preparation of protonated g-C3N4Powder: putting melamine into muffleCalcining in a furnace at the heating rate of 4 ℃/min to 550 ℃ for 4h, cooling to room temperature, and grinding to obtain g-C3N4(ii) a The g-C obtained3N4Dispersing in 37% hydrochloric acid solution, ultrasonic treating for 60min, stirring for 60min, washing, and drying to obtain protonated g-C3N4Said g-C3N4The dosage ratio of the hydrochloric acid solution to the hydrochloric acid solution is 1-4 g: 50-100 mL;
(3) BiVO with a certain mass ratio4And protonation of g-C3N4Dissolving in ethanol, performing ultrasonic dispersion at room temperature, and stirring in a fume hood for 24 h; after ethanol volatilization, drying the obtained product at 60 ℃ for 12h to obtain BiVO4Protonated g-C3N4A composite material of said BiVO4Protonated g-C3N4The dosage ratio of the ethanol to the ethanol is 0.1-0.2 g:0.1g:100 mL;
(4) BiVO (bismuth oxide) is added4Protonated g-C3N4Dissolving the composite material in deionized water, performing ultrasonic treatment at room temperature for 10min, and adding AgNO3Stirring the solution for 1h in the dark, dropwise adding a KI solution in the stirring process, continuously stirring for 1h, washing and drying to obtain BiVO4Protonated g-C3N4a/AgI ternary composite photocatalyst;
the BiVO4Protonated g-C3N4Composite material, deionized water and AgNO3The dosage ratio of the solution to the KI solution is 0.1g: 50mL of: 0.0851 mmol: 0.0851mmol of said AgNO3The concentration of the solution is 0.1mol/L, and the concentration of the KI solution is 0.1 mol/L.
2. BiVO according to claim 14Protonated g-C3N4the/AgI ternary composite photocatalyst is characterized in that in the step (3), the ultrasonic dispersion time is 1-4 h.
3. BiVO according to any of claims 1-24Protonated g-C3N4The application of the AgI ternary composite photocatalyst in organic dye treatment.
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