CN115430446B - CePO (CePO) 4 /g-C 3 N 4 Heterojunction material and preparation method and application thereof - Google Patents
CePO (CePO) 4 /g-C 3 N 4 Heterojunction material and preparation method and application thereof Download PDFInfo
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- 230000001699 photocatalysis Effects 0.000 claims abstract description 13
- 238000000034 method Methods 0.000 claims abstract description 12
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- XSQUKJJJFZCRTK-UHFFFAOYSA-N Urea Chemical compound NC(N)=O XSQUKJJJFZCRTK-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000004202 carbamide Substances 0.000 claims abstract description 6
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- 229910052684 Cerium Inorganic materials 0.000 description 3
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- 229910019142 PO4 Inorganic materials 0.000 description 2
- 229910052799 carbon Inorganic materials 0.000 description 2
- VNWKTOKETHGBQD-UHFFFAOYSA-N methane Chemical compound C VNWKTOKETHGBQD-UHFFFAOYSA-N 0.000 description 2
- BDAGIHXWWSANSR-UHFFFAOYSA-N methanoic acid Natural products OC=O BDAGIHXWWSANSR-UHFFFAOYSA-N 0.000 description 2
- 239000010452 phosphate Substances 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 229910052761 rare earth metal Inorganic materials 0.000 description 2
- -1 rare earth phosphate Chemical class 0.000 description 2
- 238000000926 separation method Methods 0.000 description 2
- OSWFIVFLDKOXQC-UHFFFAOYSA-N 4-(3-methoxyphenyl)aniline Chemical compound COC1=CC=CC(C=2C=CC(N)=CC=2)=C1 OSWFIVFLDKOXQC-UHFFFAOYSA-N 0.000 description 1
- UGFAIRIUMAVXCW-UHFFFAOYSA-N Carbon monoxide Chemical class [O+]#[C-] UGFAIRIUMAVXCW-UHFFFAOYSA-N 0.000 description 1
- 238000005033 Fourier transform infrared spectroscopy Methods 0.000 description 1
- 238000001157 Fourier transform infrared spectrum Methods 0.000 description 1
- 229910002367 SrTiO Inorganic materials 0.000 description 1
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- 229910010413 TiO 2 Inorganic materials 0.000 description 1
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- TYAVIWGEVOBWDZ-UHFFFAOYSA-K cerium(3+);phosphate Chemical compound [Ce+3].[O-]P([O-])([O-])=O TYAVIWGEVOBWDZ-UHFFFAOYSA-K 0.000 description 1
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- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
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- B01J27/14—Phosphorus; Compounds thereof
- B01J27/16—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr
- B01J27/18—Phosphorus; Compounds thereof containing oxygen, i.e. acids, anhydrides and their derivates with N, S, B or halogens without carriers or on carriers based on C, Si, Al or Zr; also salts of Si, Al and Zr with metals other than Al or Zr
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Abstract
The application discloses a CePO 4 /g‑C 3 N 4 Heterojunction material, preparation method and application thereof, and belongs to material preparation and photocatalytic reduction of CO 2 The technical field of resource utilization. The application firstly obtains g-C through urea heating calcination 3 N 4 The method comprises the steps of carrying out a first treatment on the surface of the Then at g-C 3 N 4 Ce (NO) is added into the suspension in sequence 3 ) 3 ·6H 2 O and NH 4 H 2 PO 4 After hydrothermal reaction, cooling, water washing and ethanol washing, drying overnight to obtain CePO 4 /g‑C 3 N 4 Heterojunction materials. The preparation process of the application is green and simple, has low cost, environmental protection and strong practicability, and the prepared CePO 4 /g‑C 3 N 4 Heterojunction material, facilitating enhancement of CO 2 The adsorption/activation function of the catalyst has the advantages of high visible light utilization rate, good photogenerated charge transmission effect, strong reducing capability, good economic benefit and environmental protection benefit, and provides guidance for designing a Z-type photocatalytic system.
Description
Technical Field
The application belongs to material preparation and photocatalytic reduction of CO 2 The technical field of resource utilization, in particular to a CePO 4 /g-C 3 N 4 Heterojunction materials, and preparation methods and applications thereof.
Background
In recent years, in order to solve the problems of rapid consumption of fossil fuel and global warming, many methods for reducing carbon emissions have been proposed. Wherein, carbon dioxide emission is reduced or reduced in sustainable solar energySolutions for the conversion of carbon oxides to valuable carbon derivatives (e.g. methane, formic acid, methanol, etc.) have received considerable attention. Thus, photocatalytic CO 2 Reduction technology is one of the fastest growing solutions at present due to its sustainability, environmental friendliness and efficiency.
Currently, various semiconductors such as g-C 3 N 4 、ZnIn 2 S 4 、TiO 2 、WO 3 、MOF、CeO 2 、CdS、 SrTiO 3 Has been widely used in the field of photocatalysis. Wherein cerium phosphate (CePO) 4 ) As one of the most common rare earth phosphate materials, the rare earth phosphate material has the characteristics of special 4f-5d and 4f-4f electronic transition, excellent conductivity, stronger covalent P-O bonding, high chemical stability and the like, and has wide application in the fields of fluorescence, ion exchange, catalytic materials, ceramic composite materials and the like. Graphitized carbon (g-C) 3 N 4 ) The material has the advantages of narrow band gap, good stability and the like, and is considered as a potential visible light catalytic material. However, g-C 3 N 4 There are two major drawbacks: (1) the photo-generated carrier recombination is relatively high; (2) The specific surface area is small, and the photocatalytic efficiency is low.
The heterojunction is constructed, so that the light absorption performance of the composite material and the rapid separation and transfer of the photo-generated electron pair can be effectively improved, and the light reduction/oxidation capability of the composite material can be enhanced. However, to date, for the construction of CePO 4 /g-C 3 N 4 Heterojunction structure and photocatalytic CO thereof 2 There are few reports of reduction properties.
Disclosure of Invention
The first technical problem to be solved by the present application is to provide a CePO 4 /g-C 3 N 4 A heterojunction material; the second technical problem to be solved by the application is to provide a CePO 4 /g-C 3 N 4 A preparation method of a heterojunction material; the third technical problem to be solved by the application is to provide a CePO 4 /g-C 3 N 4 Heterojunction material for photocatalytic reduction of CO 2 Is used in the field of applications.
In order to solve the technical problems, the technical scheme adopted by the application is as follows:
CePO (CePO) 4 /g-C 3 N 4 The preparation method of the heterojunction material comprises the following steps:
1) Slowly adding urea into a crucible at room temperature, introducing air into a muffle furnace, and heating and calcining to obtain g-C 3 N 4 ；
2) According to g-C 3 N 4 The dosage ratio of the ultra-pure water to the ultra-pure water is 0.1-1.5 g/15 mL, and the ultra-pure water is evenly dispersed by ultrasonic to form g-C 3 N 4 A suspension; ce (NO) 3 ) 3 ·6H 2 O and NH 4 H 2 PO 4 Sequentially adding to g-C 3 N 4 Stirring the suspension for 1h, pouring the suspension into a reaction kettle, and carrying out hydrothermal reaction at 100-200 ℃ for 11-13 h; naturally cooling to room temperature, washing with water and ethanol, and oven drying overnight to obtain CePO 4 /g-C 3 N 4 Heterojunction materials.
Further, in the step 1), the dosage of urea is 0-100 mg, the heating speed is 5-10 ℃/min, and the calcining temperature is 500-600 ℃.
Further, in step 2), g-C 3 N 4 And ultrapure water in a ratio of 0.43g to 15mL.
Further, in step 2), ce (NO) 3 ) 3 ·6H 2 O and NH 4 H 2 PO 4 The dosage ratio of (C) is 1.3 g:0.345. 0.345 g.
Further, in the step 2), the ultrasonic reaction time is 0.5-1 h.
Preferably, in step 2), the time of the ultrasonic reaction is 0.5h.
Preferably, in step 2), the temperature of the hydrothermal reaction is 150 ℃ and the time of the hydrothermal reaction is 12 h.
CePO prepared by the method 4 /g-C 3 N 4 Heterojunction materials.
The CePO 4 /g-C 3 N 4 Heterojunction material for photocatalytic reduction of CO 2 Is used in the field of applications.
Compared with the prior art, the application has the beneficial effects that:
(1) CePO of the application 4 /g-C 3 N 4 The preparation process of the heterojunction material is green and simple, low in cost, environment-friendly and high in practicability.
(2) CePO prepared by the application 4 /g-C 3 N 4 Heterojunction material, compared with existing P-CeO 2 /g-C 3 N 4 Material, CO 2 The photocatalytic conversion performance is obviously improved; the heterojunction material has excellent environmental stability and can be used for preparing CO 2 The method has potential application prospect in the aspects of resource utilization and the like.
(3) CePO prepared by the application 4 /g-C 3 N 4 Application of heterojunction material in photocatalytic reduction of CO 2 The method has the advantages of high visible light utilization rate, good photogenerated charge transmission effect and strong reduction capability, and solves the problem of CO 2 Has potential application prospect in the aspects of environmental problems such as greenhouse effect and the like.
Drawings
FIG. 1 is an XRD pattern of a sample prepared in accordance with the present application;
FIG. 2 is a FTIR spectrum of a sample prepared according to the present application;
FIG. 3 is a TEM spectrum of a sample prepared according to the application; in the figure, A, B, C, D, E, F are CePO 4 、Ce/CN、Ce/CN 0.5 、Ce/CN 0.25 、Ce/CN 0.3 And g-C 3 N 4 A sample;
FIG. 4 shows Ce/CN prepared according to the present application 0.3 And CePO (Cepo) 4 P2P XPS (a) and O1s XPS (B) plots of samples;
FIG. 5 is a UV-vis DRS (A) spectrum, photocurrent (B) graph and EIS graph (C) of a sample prepared according to the present application;
FIG. 6 shows a sample prepared according to the present application and P-CeO 2 /g-C 3 N 4 Sample exposure to CO under full spectrum 2 Performance of reduction is compared with a graph.
Detailed Description
The application is further described below in connection with specific embodiments. These examples are only for illustrating the present application and are not intended to limit the scope of the present application. Modifications and substitutions to methods, procedures, or conditions of the present application without departing from the spirit and nature of the application are intended to be within the scope of the present application. In the following examples, unless otherwise indicated, all technical means used in the examples are conventional means well known to those skilled in the art.
Example 1
According to g-C 3 N 4 The dosage ratio of the ultra-pure water to the ultra-pure water is 0.325g to 15mL, and the ultra-pure water is evenly dispersed by ultrasonic to form g-C 3 N 4 A suspension; successively adding Ce (NO) 3 ) 3 ·6H 2 O (1.3 g) and NH 4 H 2 PO 4 (0.345 g) added to the above g-C 3 N 4 Stirring the suspension for 1h, pouring the suspension into a reaction kettle, and carrying out hydrothermal reaction at 150 ℃ for 12h; naturally cooling to room temperature, washing with water and ethanol, and oven drying at 80deg.C overnight to obtain Ce/CN 0.25 Heterojunction materials. Ce/CN 0.3 ，Ce/CN 0.5 Preparation steps of Ce/CN and Ce/CN 0.25 Is similar to the method except g-C 3 N 4 Is a mass of (3). Ce/CN 0.3 ，Ce/CN 0.5 Ce/CN corresponds to g-C respectively 3 N 4 Is characterized by comprising the following components in parts by mass: 0.43g,0.65g,1.3g.
Comparative example 1
Slowly adding 10g of urea into a crucible at room temperature, introducing air into a muffle furnace, and heating and calcining to obtain g-C 3 N 4 The method comprises the steps of carrying out a first treatment on the surface of the The temperature rising rate is 5-10 ℃/min, and the calcining temperature is 500-600 ℃.
Comparative example 2
According to Ce (NO) 3 ) 3 ·6H 2 O、NH 4 H 2 PO 4 And ultrapure water in a ratio of 1.3g to 0.345g to 15mL to give Ce (NO) 3 ) 3 ·6H 2 O and NH 4 H 2 PO 4 Respectively placing into ultrapure water, and ultrasonic dispersing to obtain Ce (NO) 3 ) 3 ·6H 2 O suspension and NH 4 H 2 PO 4 Suspension, NH 4 H 2 PO 4 Slowly adding Ce (NO) into the suspension in a dropwise manner 3 ) 3 ·6H 2 Stirring the O suspension for 1h, pouring the O suspension into a reaction kettle, and carrying out hydrothermal reaction at 150 ℃ for 12h; naturally cooling to room temperature, washing with water and ethanol, and oven drying overnight to obtain CePO 4 。
Comparative example 3
P-CeO 2 /g-C 3 N 4 The preparation method of the composite material comprises the following steps:
(1) Preparation of g-C 3 N 4 And (3) a photocatalyst: weighing 10g of urea, placing into a crucible, covering a crucible cover, horizontally placing into a muffle furnace, calcining in an air atmosphere, heating to 600 ℃, reacting at the temperature for 4h, and cooling to room temperature after calcining is finished to obtain g-C 3 N 4 A sample;
(2) Will be 0.6g g-C 3 N 4 And 0.5g Ce (NO) 3 ) 3 ·6H 2 Adding O into 25mL of ultrapure water, carrying out ultrasonic treatment for 1h, and fully stirring and uniformly mixing to obtain a dispersion E;
(3) Will 0.008g Na 3 PO 4 ·12H 2 Adding O into 25mL of ultrapure water, and fully stirring and uniformly mixing to obtain a dispersion liquid F;
(4) Slowly dripping the dispersion liquid F into the dispersion liquid E dropwise, stirring for 1h, uniformly mixing reactants, transferring the reaction liquid into a 50mL stainless steel autoclave, and performing thermal reaction at a constant temperature of 180 ℃ for 14h;
(5) Naturally cooling to room temperature after the reaction is finished, respectively washing with ultrapure water and absolute ethyl alcohol for 5 times, and drying for 10 hours at the temperature of 60 ℃ in vacuum to obtain the P-CeO 2 /g-C 3 N 4 Heterojunction materials.
FIG. 1 is a Ce/CN 0.25 ，Ce/CN 0.3 ，Ce/CN 0.5 ，Ce/CN，CePO 4 And g-C 3 N 4 X-ray diffraction pattern (XRD) of the sample, as can be seen from FIG. 1, ce/CN 0.25 ，Ce/CN 0.3 ，Ce/CN 0.5 Ce/CN and CePO 4 The samples showed similar diffraction peaks. But with g-C 3 N 4 The input is reduced by 28 DEG and 32 DEGThe diffraction peak at this point showed a trend from weak to strong to weak, and a slight shift of the diffraction peak at 28 ° to a lower angle, indicating a widening of the interlayer distance, and CePO 4 And g-C 3 N 4 There is an interface effect between them.
FIG. 2 is a Ce/CN 0.25 ，Ce/CN 0.3 ，Ce/CN 0.5 ，Ce/CN，CePO 4 And g-C 3 N 4 FTIR patterns of samples, from which Ce/CN is known 0.25 ，Ce/CN 0.3 ，Ce/CN 0.5 CePO appeared in Ce/CN samples 4 And g-C 3 N 4 Is used for successfully preparing CePO 4 /g-C 3 N 4 A composite material.
FIG. 3 is CePO 4 ，Ce/CN，Ce/CN 0.5 ，Ce/CN 0.25 ，Ce/CN 0.3 ，g-C 3 N 4 TEM of sample (A, B, C, D, E, F in FIG. 3), ce/CN is known from the figure 0.25 ，Ce/CN 0.3 ，Ce/CN 0.5 ， Ce/CN，CePO 4 The samples all showed a rod-like CePO 4 g-C loaded on sheet 3 N 4 And (3) upper part.
The XPS results of FIG. 4 indicate the valence of P, O species and CePO in the composite 4 Similar in (a) and (b). The above results all indicate that the CePO was successfully prepared 4 /g-C 3 N 4 A composite material.
Example 2
CO 2 Is carried out in a 50W teflon lined autoclave and irradiated by a 300W Xe lamp. CePO with different proportions 4 /g-C 3 N 4 The heterojunction material (50 mg) was spread uniformly in a quartz reactor, dropped into 1mL of ultrapure water, and CO of high purity was added 2 The gas pressure is up to 4bar. The whole spectrum was irradiated for 8 hours. CO, CH produced 4 Measured by a gas chromatograph. In addition, a cycle experiment was also performed, each cycle being performed for 8 hours. After each cycle, the used samples were washed several times with distilled water and then dried in an oven at 80 ℃.
FIG. 5 is a Ce/CN 0.25 ，Ce/CN 0.3 ，Ce/CN 0.5 ，Ce/CN，CePO 4 And g-C 3 N 4 UV-vis DRS (A) spectra, photocurrent (B) profile and EIS profile (C) of the sample. Ce/CN compared to other samples 0.3 The visible light response of (2) is large, the photocurrent intensity is maximum, the Nyquist circle radius is minimum, indicating Ce/CN 0.3 The method has higher electron-hole separation efficiency, the best electron life and better photocatalysis efficiency.
FIG. 6 is a graph of the CO exposure of the prepared sample under full spectrum irradiation 2 From the reduction effect graph, ce/CN 0.3 Is the highest in CO yield and CH 4 High selectivity with g-C 3 N 4 The input amount is reduced, the catalytic performance of the sample is changed from strong to weak, and the catalyst is used in Ce/CN 0.3 Inflection points are formed at the positions, and the CO yield reaches 3.1 mu mol g -1 ·h -1 . Compared with the previous P-CeO 2 /g-C 3 N 4 The performance of the material, CO yield, is improved by about 6 times. CePO prepared by this patent 4 /g-C 3 N 4 Heterojunction in CO 2 The method has potential application prospect in the aspect of resource utilization.
Claims (6)
1. CePO (CePO) 4 /g-C 3 N 4 The preparation method of the heterojunction material is characterized by comprising the following steps of:
1) Heating and calcining urea in a muffle furnace to obtain g-C 3 N 4 ；
2) According to g-C 3 N 4 The dosage ratio of the ultra-pure water to the ultra-pure water is 0.43g to 15mL, and the ultra-pure water is evenly dispersed by ultrasonic to form g-C 3 N 4 A suspension; ce (NO) in the dosage ratio of 1.3g to 0.345g 3 ) 3 ·6H 2 O and NH 4 H 2 PO 4 Sequentially adding to g-C 3 N 4 Stirring the suspension for 1h, pouring the suspension into a reaction kettle, and carrying out hydrothermal reaction at 150 ℃ for 12h; naturally cooling to room temperature, washing with water and ethanol, and oven drying overnight to obtain CePO 4 /g-C 3 N 4 Heterojunction materials.
2. The CePO according to claim 1 4 /g-C 3 N 4 The preparation method of the heterojunction material is characterized in that in the step 1), the heating rate is 5-10 ℃/min, and the calcining temperature is 500-600 ℃.
3. The CePO according to claim 1 4 /g-C 3 N 4 The preparation method of the heterojunction material is characterized in that in the step 2), the ultrasonic reaction time is 0.5-1 h.
4. A CePO according to claim 3 4 /g-C 3 N 4 The preparation method of the heterojunction material is characterized in that in the step 2), the ultrasonic reaction time is 0.5h.
5. CePO prepared by the method of any one of claims 1 to 4 4 /g-C 3 N 4 Heterojunction materials.
6. The CePO as in claim 5 4 /g-C 3 N 4 Heterojunction material for photocatalytic reduction of CO 2 Is used in the field of applications.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014149993A (en) * | 2013-02-01 | 2014-08-21 | Nippon Shokubai Co Ltd | Zinc negative electrode, battery and electrode base layer |
| CN104289238A (en) * | 2014-09-12 | 2015-01-21 | 山东沁宇环保科技有限公司 | Catalyst used for degrading ozone at normal temperature and preparation method and application thereof |
| CN112023974A (en) * | 2020-09-22 | 2020-12-04 | 南京大学 | P-CeO2/g-C3N4Heterojunction material, preparation method and application thereof |
| CN112473712A (en) * | 2020-11-23 | 2021-03-12 | 南京大学 | CeO treated with different atmospheres2/g-C3N4Heterojunction material, preparation method and application thereof |
| CN114163997A (en) * | 2021-12-06 | 2022-03-11 | 上海交通大学 | Semiconductor composite luminescent material, preparation method and luminescent device |
| CN114653389A (en) * | 2021-12-09 | 2022-06-24 | 淮阴工学院 | g-C with surface defects3N4/LaPO4Preparation method of core-shell structure nanorod |
Family Cites Families (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20070128707A1 (en) * | 2005-11-10 | 2007-06-07 | Oregon State University | Method for making metal oxides |
| WO2012040652A2 (en) * | 2010-09-23 | 2012-03-29 | Molycorp Minerals Llc | Particulate cerium dioxide and an in situ method for making and using the same |
| WO2015002733A2 (en) * | 2013-06-17 | 2015-01-08 | The Curators Of The University Of Missouri | Multifunctional cerium-based nanomaterials and methods for producing the same |
-
2022
- 2022-07-27 CN CN202210902087.6A patent/CN115430446B/en active Active
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP2014149993A (en) * | 2013-02-01 | 2014-08-21 | Nippon Shokubai Co Ltd | Zinc negative electrode, battery and electrode base layer |
| CN104289238A (en) * | 2014-09-12 | 2015-01-21 | 山东沁宇环保科技有限公司 | Catalyst used for degrading ozone at normal temperature and preparation method and application thereof |
| CN112023974A (en) * | 2020-09-22 | 2020-12-04 | 南京大学 | P-CeO2/g-C3N4Heterojunction material, preparation method and application thereof |
| CN112473712A (en) * | 2020-11-23 | 2021-03-12 | 南京大学 | CeO treated with different atmospheres2/g-C3N4Heterojunction material, preparation method and application thereof |
| CN114163997A (en) * | 2021-12-06 | 2022-03-11 | 上海交通大学 | Semiconductor composite luminescent material, preparation method and luminescent device |
| CN114653389A (en) * | 2021-12-09 | 2022-06-24 | 淮阴工学院 | g-C with surface defects3N4/LaPO4Preparation method of core-shell structure nanorod |
Non-Patent Citations (1)
| Title |
|---|
| Core-shell LaPO4/g-C3N4 nanowires for highly active and selective CO2 reduction;Mengli Li et al.;《Applied Catalysis B: Environmental》;第201卷;629-635 * |
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