CN107649164B - g-C3N4-xFx/TiO2Coupling heterojunction photocatalyst and preparation method thereof - Google Patents
g-C3N4-xFx/TiO2Coupling heterojunction photocatalyst and preparation method thereof Download PDFInfo
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- 239000011941 photocatalyst Substances 0.000 title claims abstract description 37
- 238000002360 preparation method Methods 0.000 title claims abstract description 11
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N titanium dioxide Inorganic materials O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 claims abstract description 50
- 239000004202 carbamide Substances 0.000 claims abstract description 34
- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000007864 aqueous solution Substances 0.000 claims abstract description 17
- 238000001035 drying Methods 0.000 claims abstract description 17
- 239000011259 mixed solution Substances 0.000 claims abstract description 16
- 238000010168 coupling process Methods 0.000 claims abstract description 9
- 238000005859 coupling reaction Methods 0.000 claims abstract description 9
- 238000000227 grinding Methods 0.000 claims abstract description 9
- 238000011065 in-situ storage Methods 0.000 claims abstract description 8
- 230000008878 coupling Effects 0.000 claims abstract description 7
- 238000003756 stirring Methods 0.000 claims description 20
- 239000000843 powder Substances 0.000 claims description 16
- 238000002156 mixing Methods 0.000 claims description 10
- 238000001132 ultrasonic dispersion Methods 0.000 claims description 10
- 238000006243 chemical reaction Methods 0.000 claims description 9
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 claims description 8
- 239000008367 deionised water Substances 0.000 claims description 8
- 229910021641 deionized water Inorganic materials 0.000 claims description 8
- 238000010438 heat treatment Methods 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 230000015572 biosynthetic process Effects 0.000 claims description 6
- 150000002500 ions Chemical class 0.000 claims description 5
- 230000002194 synthesizing effect Effects 0.000 claims description 2
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 claims description 2
- 230000001699 photocatalysis Effects 0.000 abstract description 9
- 238000001354 calcination Methods 0.000 abstract description 5
- 238000000034 method Methods 0.000 abstract description 5
- 230000035484 reaction time Effects 0.000 abstract description 3
- 239000003054 catalyst Substances 0.000 abstract description 2
- 230000003197 catalytic effect Effects 0.000 abstract 1
- 238000006731 degradation reaction Methods 0.000 description 11
- 230000015556 catabolic process Effects 0.000 description 10
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 description 10
- 229940043267 rhodamine b Drugs 0.000 description 10
- 230000000593 degrading effect Effects 0.000 description 7
- 239000013078 crystal Substances 0.000 description 6
- 230000000694 effects Effects 0.000 description 5
- 239000000463 material Substances 0.000 description 4
- 239000002957 persistent organic pollutant Substances 0.000 description 4
- 239000012071 phase Substances 0.000 description 4
- 239000004065 semiconductor Substances 0.000 description 4
- 238000001179 sorption measurement Methods 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 3
- 238000007146 photocatalysis Methods 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000009286 beneficial effect Effects 0.000 description 2
- 125000000623 heterocyclic group Chemical group 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000003786 synthesis reaction Methods 0.000 description 2
- 238000012719 thermal polymerization Methods 0.000 description 2
- 239000002131 composite material Substances 0.000 description 1
- 238000004070 electrodeposition Methods 0.000 description 1
- 238000005265 energy consumption Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000003344 environmental pollutant Substances 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 125000005842 heteroatom Chemical group 0.000 description 1
- 238000010348 incorporation Methods 0.000 description 1
- 239000008204 material by function Substances 0.000 description 1
- 239000005416 organic matter Substances 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 238000013032 photocatalytic reaction Methods 0.000 description 1
- 231100000719 pollutant Toxicity 0.000 description 1
- 239000002994 raw material Substances 0.000 description 1
- 238000005215 recombination Methods 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003746 solid phase reaction Methods 0.000 description 1
- 239000000243 solution Substances 0.000 description 1
- 230000002269 spontaneous effect Effects 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
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Abstract
The invention discloses a g-C3N4‑xFx/TiO2A coupled heterojunction photocatalyst and a preparation method thereof, (NH)4)2TiF6Adding into urea aqueous solution to obtain mixed solution, drying, grinding, and calcining to obtain g-C3N4‑xFx/TiO2A heterojunction photocatalyst is coupled. The invention adopts an in-situ calcination method to synthesize the g-C in one step3N4‑xFx/TiO2The coupled heterojunction photocatalyst has simple operation, short reaction time and synthesized g-C3N4‑xFx/TiO2The coupling heterojunction photocatalyst has higher photocatalytic activity and improves pure phase g-C3N4The catalytic efficiency of the catalyst has good application prospect.
Description
Technical Field
The invention belongs to the field of functional materials, and particularly relates to g-C3N4-xFx/TiO2A coupled heterojunction photocatalyst and a preparation method thereof.
Background
Environmental pollution and energy shortage are two major problems faced by the contemporary society, and the semiconductor photocatalysis technology has wide application prospects in the aspect of pollutant degradation due to low energy consumption, no secondary pollution and the like.
g-C3N4The graphite-like layered structure has excellent thermal stability and chemical stability, is easy to control in structure and performance, and responds to visible light. The synthesis method mainly comprises the following steps: thermal polymerization, solid-phase reaction, solvothermal, electrochemical deposition. But g-C prepared by conventional thermal polymerization3N4The specific surface area is small, and the photo-generated electron-hole pairs are easy to recombine to cause lower photocatalysis performance, so that the application of the photo-generated electron-hole pairs in the field of photocatalysis is severely restricted.
Therefore, the photocatalytic performance of the material is improved by modifying the material by chemical doping and semiconductor composite modification. After chemical doping, the g-C can be changed3N4Thereby improving the photocatalytic performance. At present, heterocyclic rings, hetero atoms and the like are often used for doping. Introduction of a heterocyclic ring may lead to g-C3N4Redistribute electron potential, separate oxidation-reduction sites and improve photocatalytic activity. Many ions, including B, F, C, O, P, S, etc., can be incorporated into g-C3N4The separation of photo-generated electron-hole pairs can be accelerated; g to C3N4The material is compounded with an oxide semiconductor, fully contacts with the oxide semiconductor and forms a heterojunction, and can also improve the interface transfer rate of a photon-generated carrier and reduce the recombination rate of photon-generated electron-hole pairs, thereby improving the photocatalytic activity of the material.
Disclosure of Invention
The invention aims to provide g-C3N4-xFx/TiO2The coupling heterojunction photocatalyst and the preparation method thereof have the advantages of simple operation, short reaction time and capability of preparing g-C3N4-xFx/TiO2The coupled heterojunction photocatalyst has high rhodamine B degradation activity under visible light, and can be used for degrading organic pollutants.
In order to achieve the above purpose, the preparation method of the invention comprises the following steps:
step 1: adding urea into deionized water, uniformly stirring, and performing ultrasonic dispersion to obtain a urea aqueous solution with the concentration of 0.2-0.5 g/mL;
step 2: conversion of the amount of F to g-C as urea3N4Adding (NH) into the urea aqueous solution with the mass of 1-4%4)2TiF6Mixing and stirring to obtain a mixed solution;
and step 3: drying the mixed solution in an oven, and grinding to obtain white powder; then the white powder is put into an alumina crucible with a cover, heated to 550 ℃ from room temperature at the heating rate of 15 ℃/min, calcined and cooled to room temperature, and then ground to obtain light yellow g-C3N4-xFx/TiO2A heterojunction photocatalyst is coupled.
The stirring and ultrasonic dispersion time in the step 1) is 30 min.
The mixing and stirring time in the step 2) is 60 min.
The drying temperature in the step 3) is 70 ℃.
g-C prepared by the above preparation method3N4-xFx/TiO2F ions in the coupled heterojunction photocatalyst enter g-C3N4Lattice formation g-C3N4-xFxSimultaneously synthesizing anatase TiO with 141/amd space point group in situ2And form g-C3N4-xFx/TiO2A heterojunction.
g-C of the invention3N4-xFx/TiO2The coupling heterojunction photocatalyst has the adsorption characteristic and high degradation activity, and can be used for degrading organic pollutants.
Compared with the prior art, the invention has the beneficial effects that:
the invention uses urea and (NH)4)2TiF6g-C is successfully prepared by one step through an in-situ calcination method as a raw material3N4-xFx/TiO2Coupling of heterojunction photocatalyst to improve pure phase g-C3N4The efficiency of photocatalytic degradation of organic matter. The invention adopts an in-situ calcination method to synthesize the g-C in one step3N4-xFx/TiO2The coupling heterojunction photocatalyst has simple operation, short reaction time and synthesized g-C3N4-xFx/TiO2The coupled heterojunction photocatalyst has higher photocatalytic activity and reaches the g-C ratio3N4The modification is aimed at, and the method has good application prospect. g-C prepared by the invention3N4-xFx/TiO2The preparation method of the coupled heterojunction photocatalyst is an in-situ calcination method, and F ions enter g-C3N4Lattice formation g-C3N4-xFxSimultaneous in situ synthesis of anatase TiO2And form g-C3N4-xFx/TiO2A heterojunction. The photocatalyst has the advantages of adsorption property and high degradation activity, and can be used for degrading organic pollutants.
Drawings
FIG. 1 is g-C prepared according to the present invention3N4-xFx/TiO2XRD patterns of the coupled heterojunction photocatalysts.
FIG. 2 is g-C prepared according to the present invention3N4-xFx/TiO2And (3) degrading the degradation curve of rhodamine B by coupling the heterojunction photocatalyst under visible light.
Detailed Description
The present invention will be described in further detail with reference to the following specific embodiments and the accompanying drawings.
Example 1:
step 1: adding urea into deionized water, stirring for 30min, and then performing ultrasonic dispersion for 30min to obtain a urea aqueous solution with the concentration of 0.2 g/mL;
step 2: conversion of the amount of F to g-C as urea3N4Adding (NH) to the urea aqueous solution at 1% by mass4)2TiF6Mixing and stirring for 60min to obtain a mixed solution;
and step 3: drying the mixed solution in a drying oven at 70 ℃, and grinding to obtain white powder; then the white powder is put into an alumina crucible with a cover, heated to 550 ℃ from room temperature at the heating rate of 15 ℃/min, calcined and cooled to room temperature, and then ground to obtain light yellow g-C3N4-xFx/TiO2A heterojunction photocatalyst is coupled.
Example 2:
step 1: adding urea into deionized water, stirring for 30min, and then performing ultrasonic dispersion for 30min to obtain a urea aqueous solution with the concentration of 0.2 g/mL;
step 2: conversion of the amount of F to g-C as urea3N42% by mass of (NH) is added to the urea aqueous solution4)2TiF6Mixing and stirring for 60min to obtain a mixed solution;
and step 3: drying the mixed solution in a drying oven at 70 ℃, and grinding to obtain white powder; then the white powder is put into an alumina crucible with a cover, heated to 550 ℃ from room temperature at the heating rate of 15 ℃/min, calcined and cooled to room temperature, and then ground to obtain light yellow g-C3N4-xFx/TiO2A heterojunction photocatalyst is coupled.
Example 3:
step 1: adding urea into deionized water, stirring for 30min, and then performing ultrasonic dispersion for 30min to obtain a urea aqueous solution with the concentration of 0.2 g/mL;
step 2: conversion of the amount of F to g-C as urea3N43% by mass of (NH) is added to the urea aqueous solution4)2TiF6Mixing and stirring for 60min to obtain a mixed solution;
and step 3: drying the mixed solution in a drying oven at 70 ℃, and grinding to obtain white powder; then the white powder is put into an alumina crucible with a cover, heated to 550 ℃ from room temperature at the heating rate of 15 ℃/min, calcined and cooled to room temperature, and then ground to obtain light yellow g-C3N4-xFx/TiO2A heterojunction photocatalyst is coupled.
Example 4:
step 1: adding urea into deionized water, stirring for 30min, and then performing ultrasonic dispersion for 30min to obtain a urea aqueous solution with the concentration of 0.2 g/mL;
step 2: conversion of the amount of F to g-C as urea3N44% by mass of (NH) is added to the urea aqueous solution4)2TiF6Mixing and stirring for 60min to obtainMixing the solution;
and step 3: drying the mixed solution in a drying oven at 70 ℃, and grinding to obtain white powder; then the white powder is put into an alumina crucible with a cover, heated to 550 ℃ from room temperature at the heating rate of 15 ℃/min, calcined and cooled to room temperature, and then ground to obtain light yellow g-C3N4-xFx/TiO2A heterojunction photocatalyst is coupled.
Example 5:
step 1: adding urea into deionized water, stirring for 30min, and then performing ultrasonic dispersion for 30min to obtain a urea aqueous solution with the concentration of 0.5 g/mL;
step 2: conversion of the amount of F to g-C as urea3N42.5% by mass of (NH) was added to the urea aqueous solution4)2TiF6Mixing and stirring for 60min to obtain a mixed solution;
and step 3: drying the mixed solution in a drying oven at 70 ℃, and grinding to obtain white powder; then the white powder is put into an alumina crucible with a cover, heated to 550 ℃ from room temperature at the heating rate of 15 ℃/min, calcined and cooled to room temperature, and then ground to obtain light yellow g-C3N4-xFx/TiO2A heterojunction photocatalyst is coupled.
Example 6:
step 1: adding urea into deionized water, stirring for 30min, and then performing ultrasonic dispersion for 30min to obtain a urea aqueous solution with the concentration of 0.3 g/mL;
step 2: conversion of the amount of F to g-C as urea3N43.5% by mass of (NH) was added to the urea aqueous solution4)2TiF6Mixing and stirring for 60min to obtain a mixed solution;
and step 3: drying the mixed solution in a drying oven at 70 ℃, and grinding to obtain white powder; then the white powder is put into an alumina crucible with a cover, heated to 550 ℃ from room temperature at the heating rate of 15 ℃/min, calcined and cooled to room temperature, and then ground to obtain light yellow g-C3N4-xFx/TiO2A heterojunction photocatalyst is coupled.
FIG. 1 is g-C prepared according to the present invention3N4-xFx/TiO2XRD patterns of coupled heterojunction photocatalysts, wherein a to d are respectively embodiment 1 to embodiment 4, wherein figure 1(a) is g-C prepared in embodiment 1 to embodiment 43N4-xFx/TiO2XRD patterns of coupled heterojunction photocatalysts, and FIG. 1(b) shows g-C prepared in examples 1 to 43N4-xFx/TiO2XRD partial magnification of the coupled heterojunction photocatalyst. As can be seen from FIG. 1(a), pure phase g-C3N4Diffraction peaks were evident at diffraction angles 2 θ of about 13.1 ° and 27.7 °, corresponding to g-C, respectively3N4The (100) crystal plane and the (002) crystal plane of (A). Introduction of (NH)4)2TiF6Then g-C is co-present3N4And TiO2Characteristic diffraction peak of (1), wherein TiO2Diffraction peak of and anatase type TiO2Standard cards (JCPDS No.84-1285) were matched, and diffraction peaks at diffraction angles 2 θ of 25.3 ° and 37.8 ° respectively corresponded to TiO2The (101) crystal plane and the (004) crystal plane of (a), and (NH) is followed by (NH)4)2TiF6Increase in the amount of incorporation, TiO2The characteristic diffraction peaks of (a) become more and more pronounced. As can be seen from FIG. 1(b), the (NH) is introduced4)2TiF6Then g-C3N4(002) Diffraction peaks at the crystal planes are shifted to different degrees due to the entry of F ions into g-C3N4Lattice formation g-C3N4-xFxSimultaneous in situ synthesis of TiO2Form g-C3N4-xFx/TiO2Heterojunctions, which distort the crystal lattice.
FIG. 2 is g-C prepared according to the present invention3N4-xFx/TiO2And (3) degrading the degradation curve of rhodamine B by coupling the heterojunction photocatalyst under visible light. Wherein a to d are g-C prepared in examples 1 to 4, respectively3N4-xFx/TiO2Coupled degradation curve of heterojunction photocatalyst, RhB is spontaneous degradation curve of rhodamine B without adding catalyst, g-C3N4"is as in example 1 without addition of (N)H4)2TiF6g-C obtained3N4Degradation curve. C/C of ordinate0The ratio of the concentration of the degraded rhodamine B to the initial concentration of the degraded rhodamine B at a certain time is shown. As can be seen from the figure, the (NH) is introduced4)2TiF6Then the adsorption performance of the sample is improved to a certain extent, and after dark reaction for 60min, pure phase g-C3N4Can adsorb 53 percent of rhodamine B, and the g-C prepared by the embodiment 1 to the embodiment 43N4-xFx/TiO262 percent, 68 percent, 69 percent and 63 percent of rhodamine B can be adsorbed respectively, and the excellent adsorption performance is more beneficial to the photocatalytic reaction. Examples 1 to 4 g-C3N4-xFx/TiO2Coupled heterojunction photocatalyst degradation activity ratio pure phase g-C3N4High, after 20min of visible light irradiation, the degradation rate of example 2 and example 3 on rhodamine B reaches 90 percent, which indicates that g-C3N4-xFx/TiO2The coupled heterojunction photocatalyst has higher degrading activity to rhodamine B and can be used for degrading organic pollutants.
Claims (3)
1. g-C3N4-xFx/TiO2The preparation method of the coupled heterojunction photocatalyst is characterized by comprising the following steps of:
step 1: adding urea into deionized water, uniformly stirring, and performing ultrasonic dispersion to obtain a urea aqueous solution with the concentration of 0.2-0.5 g/mL;
step 2: conversion of the amount of F to g-C as urea3N4Adding (NH) into the urea aqueous solution with the mass of 1-4%4)2TiF6Mixing and stirring to obtain a mixed solution;
and step 3: drying the mixed solution in an oven, and grinding to obtain white powder; then the white powder is put into an alumina crucible with a cover, heated to 550 ℃ from room temperature at the heating rate of 15 ℃/min and calcined, and ground to obtain light yellow g-C3N4-xFx/TiO2Coupling a heterojunction photocatalyst;
the stirring and ultrasonic dispersion time in the step 1) is 30 min;
the mixing and stirring time in the step 2) is 60 min.
2. g-C according to claim 13N4-xFx/TiO2The preparation method of the coupling heterojunction photocatalyst is characterized in that: the drying temperature in the step 3 is 70 ℃.
3. g-C prepared by the preparation method of claim 13N4-xFx/TiO2A coupled heterojunction photocatalyst, characterized in that: g-C3N4-xFx/TiO2F ions in the coupled heterojunction photocatalyst enter g-C3N4Lattice formation g-C3N4-xFxSimultaneously synthesizing anatase TiO with space point group of I41/amd in situ2And form g-C3N4-xFx/TiO2A heterojunction.
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