CN111939956B - Honeycomb FeV 2 O 4 Preparation method and application of composite carbon nitride loaded stainless steel wire mesh composite material - Google Patents

Honeycomb FeV 2 O 4 Preparation method and application of composite carbon nitride loaded stainless steel wire mesh composite material Download PDF

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CN111939956B
CN111939956B CN202010816773.2A CN202010816773A CN111939956B CN 111939956 B CN111939956 B CN 111939956B CN 202010816773 A CN202010816773 A CN 202010816773A CN 111939956 B CN111939956 B CN 111939956B
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fev
stainless steel
steel wire
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CN111939956A (en
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牛利
韩冬雪
赵欣
王伟
秦冬冬
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Guangdong Dingcheng Electronic Technology Co ltd
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    • B01J37/00—Processes, in general, for preparing catalysts; Processes, in general, for activation of catalysts
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Abstract

The invention discloses a honeycomb FeV 2 O 4 A preparation method and application of a composite carbon nitride loaded stainless steel wire mesh composite material. The method comprises the following steps: dissolving ammonium metavanadate and pentahydrate bismuth nitrate in water, putting the solution into a stainless steel screen, and carrying out hydrothermal reaction to obtain three-dimensional FeV 2 O 4 A stainless steel wire mesh; dissolving 2, 4-diamino-6-phenyl-1, 3, 5-triazine and cyanuric acid in water, stirring for reaction, performing solid-liquid separation on the suspension to obtain white solid, drying, grinding into powder, and spreading on three-dimensional FeV 2 O 4 Heating the surface of the stainless steel wire mesh for a period of time under the protection of gas to obtain three-dimensional FeV 2 O 4 /g‑C 3 N 4 Stainless steel wire mesh. The method effectively simplifies the process flow, and has the advantages of simple operation process, low cost and strong feasibility. The photocatalyst prepared by the invention canEffectively solves the problem that the photon-generated carriers are easy to compound, and is very suitable for being applied to the photocatalytic preparation of carbon monoxide in industrialization.

Description

Honeycomb FeV 2 O 4 Preparation method and application of composite carbon nitride loaded stainless steel wire mesh composite material
Technical Field
The invention belongs to the technical field of preparation of photocatalytic materials, and particularly relates to a honeycomb FeV 2 O 4 A preparation method and application of a composite carbon nitride loaded stainless steel wire mesh composite material.
Background
Carbon dioxide (CO) 2 ) Is a major product of combustion of fossil energy, which causes a greenhouse effect as a major greenhouse gas and its content has been continuously increased in recent years due to the continuous acceleration of industrialization. This raises a range of climatic problems such as: glacier melting, sea level rising, etc. Therefore, carbon dioxide capture and conversion technology has been applied and is considered as an effective method to solve the above problems. Among various techniques, artificial photosynthesis inspired by photosynthesis of green plants in nature is an environmentally friendly method. The method is realized through the input of external light energy and the catalytic action of a photocatalyst, and the breaking of C-O bonds in carbon dioxide and the formation of new chemical bonds are accompanied, so that the solar energy is formed. Therefore, the photocatalytic reduction of carbon dioxide can solve the problems of environmental pollution and energy shortage. In order to achieve highly selective photocatalytic reduction of carbon dioxide, various semiconductor photocatalysts have been investigated in recent years. However, the low photocatalytic yields and poor product selectivity have been limiting the further development of catalysts. Recently, spinel oxides have attracted a wide attention due to their excellent light conversion properties. Based on this, spinel oxides have been applied to photocatalytic reduction of carbon dioxide.
However, single spinel has the fatal problem of rapid carrier recombination, which seriously hampers its photocatalytic efficiency. To solve this problem, various strategies (e.g.surface sensitization, metal modification, element doping)Hetero-and building heterojunctions, etc.) have been reported to improve carrier separation efficiency and improve overall efficiency of photocatalytic reduction of carbon dioxide. Among these approaches, building a heterojunction of two different band gap materials is one of the most efficient and intelligent strategies, for example: compounding spinel with graphene, and mixing spinel with graphite phase carbon nitride (g-C) 3 N 4 ) Composite, spinel with organometallic framework compounds (MOFs), and the like. While both type ii and schottky junctions can achieve efficient separation of photogenerated carriers for the construction of the heterojunction, they both come at the expense of a reduced potential for electrons, which is extremely detrimental to the overall performance of the composite catalyst. In sharp contrast, the all-solid Z-type systems not only achieve efficient separation of photogenerated carriers spatially, but also preserve the maximum redox potential of the different catalyst components. This enables a good reduction of carbon dioxide while performing a favorable oxidation reaction. For the Z-type system, it is critical to find two band-matched catalysts and satisfy both efficient and tight interfacial carrier transport.
So far, in the field of photocatalysis, feV 2 O 4 There has not been much research. Therefore, for the study of FeV 2 O 4 The method has important significance in application of photocatalytic carbon dioxide reduction. However, existing FeV 2 O 4 Has the disadvantages of complex preparation process flow, high cost and the like. See, in particular, dohyung Kim, dongyi Zhou, songbai Hu, dieu Hien Thi Nguyen, nagarajan Valanoor, and Jan Seidel; temperature-Dependent Magnetic Domain Evolution in non-ncollicular Ferragnetic FeV 2 O 4 Thin Films,ACS Appl.Electron.Mater.2019,1,817-822,doi: 10.1021/acsaelm.9b00153.
From g to C 3 N 4 Since birth, it has attracted a great deal of interest in the field of photocatalysis due to its easy preparation, low cost, environmental friendliness and appropriate band gap as an organic polymer photocatalyst that absorbs visible light. Furthermore, g-C 3 N 4 Possess a conduction band edge that is more negative with respect to the carbon dioxide reduction potential, which gives it a broad spectrum of additional photocatalytic carbon dioxide reductionC1 compounds and other carbon-containing compounds of values such as: CO, CH 4 And CH 3 COOH, and the like. Although it has a suitable band structure, it also has a characteristic that photogenerated carriers are easily recombined.
Disclosure of Invention
Based on the problems in the prior art, the primary object of the present invention is to provide a honeycomb FeV 2 O 4 A preparation method of a composite carbon nitride loaded stainless steel wire mesh composite material. The invention adopts g-C 3 N 4 Loaded honeycomb FeV 2 O 4 (FeV 2 O 4 /g-C 3 N 4 ) Compared with the existing FeV 2 O 4 The preparation technology can effectively simplify the process flow, and has simple operation process and strong feasibility. In addition, the photocatalyst prepared by the method can effectively solve the problem that a photon-generated carrier is easy to recombine. The preparation method of the composite semiconductor photocatalytic system is simple and convenient, has low cost, and is very suitable for being applied to the photocatalytic preparation of carbon monoxide in industrialization.
Another object of the present invention is to provide a honeycomb FeV prepared by the above method 2 O 4 The composite carbon nitride loaded stainless steel wire mesh composite material.
It is still another object of the present invention to provide the above cellular FeV 2 O 4 Application of the composite carbon nitride loaded stainless steel wire mesh composite material. The spinel-based all-solid-state direct Z-type photocatalyst is used for converting carbon dioxide into carbon monoxide with high selectivity and high efficiency and effectively inhibiting a competitive reaction (hydrogen evolution reaction). FeV 2 O 4 And g-C 3 N 4 As two catalyst components for the construction of the Z-type system. FeV 2 O 4 Is selected for its inherent visible response and is relative to g-C 3 N 4 With a more positive conduction band edge. Therefore, the Z-type photocatalyst can simultaneously solve the problem of single use of FeV 2 O 4 And g-C 3 N 4 The short plate can reasonably utilize the matched staggered energy band structure and can realize the highly selective reduction of carbon dioxide to carbon monoxide under visible light. The Z-type nano composite catalyst prepared by the invention is relativelyIn a single g-C 3 N 4 Exhibits 4.84 times the photoconversion carbon monoxide performance.
The purpose of the invention is realized by the following technical scheme:
honeycomb FeV 2 O 4 The preparation method of the composite carbon nitride loaded stainless steel wire mesh composite material comprises the following steps:
(1) Three-dimensional FeV 2 O 4 Preparation of stainless steel wire mesh: reacting NH 4 VO 3 And Bi (NO) 3 ) 3 ·5H 2 Dissolving O in water, stirring, filling the mixture into a polytetrafluoroethylene lining, and putting the polytetrafluoroethylene lining into a dry and clean stainless steel wire mesh; then, filling the polytetrafluoroethylene lining into a reaction kettle, heating to 150-170 ℃ and reacting for 45-51h to obtain three-dimensional FeV 2 O 4 Stainless steel wire net (FeV) 2 O 4 )；
(2) Three-dimensional FeV 2 O 4 /g-C 3 N 4 Preparation of stainless steel wire mesh: dissolving 2, 4-diamino-6-phenyl-1, 3, 5-triazine and cyanuric acid in water, stirring for reaction for a period of time, separating solid from liquid to obtain white solid, drying the white solid, and grinding into white powder (g-C) 3 N 4 A precursor); uniformly spreading white powder on the three-dimensional FeV prepared in the step (1) 2 O 4 Heating to 480-520 ℃ for 3-5h under the protection of gas to obtain three-dimensional FeV 2 O 4 /g-C 3 N 4 Stainless steel wire net (FeV) 2 O 4 /g- C 3 N 4 )。
Further, in the step (1), the stainless steel screen provides an iron source;
further, in the step (1), NH 4 VO 3 And Bi (NO) 3 ) 3 ·5H 2 The molar ratio of O is (8-12): (4-6). The stainless steel wire mesh provides an excess of iron source.
Further, in the step (1), after the heating reaction is finished, the reaction kettle is naturally cooled to room temperature, and then the FeV is loaded 2 O 4 Taking out the stainless steel wire net, alternately washing with water and ethanol, and then drying in vacuum to obtain the three-dimensional FeV 2 O 4 Stainless steel wire mesh.
Further, the vacuum drying is drying at 60 ℃ for 8h.
Further, in the step (2), the mass ratio of the 2, 4-diamino-6-phenyl-1, 3, 5-triazine to the cyanuric acid is (8-10): (5-8).
Further, in the step (2), 2, 4-diamino-6-phenyl-1, 3, 5-triazine and cyanuric acid are dissolved in water, and then stirred to react for 24 hours.
Further, in the step (2), the white solid is dried for 6-10h at 50-70 ℃.
Further, in the step (2), the three-dimensional FeV prepared in the step (1) is tiled 2 O 4 The mass range of the white powder on the surface of the stainless steel wire mesh is as follows: 1.0-2.0g white powder/(8-12) mmol NH 4 VO 3 The FeV thus obtained 2 O 4 。
Further, in the step (2), the three-dimensional FeV prepared in the step (1) is tiled 2 O 4 The quality range of the white powder on the surface of the stainless steel wire mesh is as follows: 1.0-2.0g white powder/10 mmol NH 4 VO 3 The prepared FeV 2 O 4 。
Further, in the step (2), the three-dimensional FeV prepared in the step (1) is tiled 2 O 4 The quality range of the white powder on the surface of the stainless steel wire mesh is as follows: 1.5g white powder/10 mmol NH 4 VO 3 The FeV thus obtained 2 O 4 。
Further, in the step (2), uniformly spreading the powder on the three-dimensional FeV prepared in the step (1) 2 O 4 Introducing nitrogen after the surface of the stainless steel wire mesh, and heating to 480-520 ℃ at the speed of 2-3 ℃/min.
Further, in the step (2), after the heating is completed, the sample is taken out after being cooled to room temperature and is subjected to ultrasonic treatment in water to remove unstable substances on the surface of the sample.
The above-mentioned honeycomb-shaped FeV 2 O 4 The composite carbon nitride loaded stainless steel wire mesh composite material can be applied to preparing carbon monoxide by photocatalysis of carbon dioxide.
Compared with the prior art, the invention has the following advantages and beneficial effects:
existing FeV 2 O 4 The preparation process has the disadvantages of complex flow, high cost and the like, and the invention adopts g-C 3 N 4 Loaded honeycomb FeV 2 O 4 (FeV 2 O 4 /g-C 3 N 4 ) Compared with the existing FeV 2 O 4 The preparation technology can effectively simplify the process flow, and has simple operation process and strong feasibility. In addition, the photocatalyst prepared by the method can effectively solve the problem that a photon-generated carrier is easy to recombine. The preparation method of the composite semiconductor photocatalytic system is simple and convenient, has low cost, and is very suitable for being applied to the photocatalytic preparation of carbon monoxide in industrialization.
Drawings
FIG. 1 shows FeV as a sample obtained in example 1 2 O 4 、FeV 2 O 4 /g-C 3 N 4 Scanning electron micrograph (c). Wherein (a-c) is FeV of different scale 2 O 4 SEM picture of (1); (d-f) FeV of different scale 2 O 4 /g-C 3 N 4 SEM image of (d).
FIG. 2 shows FeV as a sample obtained in example 1 2 O 4 /g-C 3 N 4 Transmission electron micrograph (c). a. b are TEM images of different scales respectively.
FIG. 3 shows FeV obtained in example 1 2 O 4 、g-C 3 N 4 、FeV 2 O 4 /g-C 3 N 4 Powder X-ray diffraction pattern.
FIG. 4 shows FeV obtained in example 1 2 O 4 /g-C 3 N 4 An X-ray photoelectron spectrum of (a). Wherein (a) the total energy spectrum; (b) high resolution Fe 2 p; (c) a V2 p high resolution map; (d) O1 s high resolution; (e) C1 s high resolution; (f) N1 s high resolution.
FIG. 5 shows FeV obtained in example 1 2 O 4 、g-C 3 N 4 And FeV 2 O 4 /g-C 3 N 4 The ultraviolet-visible diffuse reflectance spectrum of (1). Wherein (a) is an ultraviolet-visible diffuse reflectance spectrum diagram, and (b) is a Tauc diagram.
FIG. 6 shows FeV obtained in example 1 2 O 4 、g-C 3 N 4 And FeV 2 O 4 /g-C 3 N 4 The gas adsorption/desorption analysis of (3). Wherein (a) is BET adsorption-desorption isotherm curve (inset: pore size distribution diagram) of the sample, and (b) is CO of the sample 2 Adsorption profile.
FIG. 7 shows FeV obtained in example 1 2 O 4 、g-C 3 N 4 And FeV 2 O 4 /g-C 3 N 4 The photoelectrochemical test result of (1).
FIG. 8 shows FeV obtained in example 1 2 O 4 、g-C 3 N 4 And FeV 2 O 4 /g-C 3 N 4 The photocatalytic reduction of carbon dioxide test results.
FIG. 9 is a graph of isotope labeled gas chromatography-mass spectrometry detection.
FIG. 10 is a. OH active species detection graph.
FIG. 11 is an in situ Fourier transform infrared detection map.
Detailed Description
The present invention will be described in further detail with reference to examples and drawings, but the embodiments of the present invention are not limited thereto. The raw materials related to the invention can be directly purchased from the market. For process parameters not specifically noted, reference may be made to conventional techniques.
In the following examples: stainless steel wire mesh (500 mesh) was purchased from alfield wire mesh limited; bismuth nitrate pentahydrate, cyanuric acid (> 99%), naphthol (5%) were purchased from alfa aesar chemical ltd; ammonium metavanadate was purchased from Beijing YinoKay science and technology, inc.; sodium hydroxide, hydrochloric acid, nitric acid, ethanol, acetone, barium sulfate, sodium sulfite and terephthalic acid are purchased from Beijing chemical reagent company Limited; 2, 4-diamino-6-phenyl-1, 3, 5-triazines are available from Shanghai Michelin Biochemical Co., ltd.
Using a D8 Advance (Bruker) system X-ray diffractometer (Cu ka,
Figure GDA0003868041900000061
) To study the structure and shape of the sampleAppearance information; analyzing the surface chemical valence state of the sample by a VG ESCALMK II X-ray photoelectron spectrometer (XPS, al Ka: 1486.6 eV); acquiring the surface topography of a sample by using a Philips XL 30 ESEM FEG field emission scanning electron microscope at an accelerating voltage of 15.0 kV; use of Tecnai G 2 Carrying out TEM and HRTEM on a microscope transmission electron microscope under the accelerating voltage of 200.0kV to obtain the appearance and the lattice spacing of the sample; performing ultraviolet visible diffuse reflectance spectroscopy (barium sulfate as reference substance) in Hitachi U-3900 ultraviolet visible spectrophotometer; detecting a sample by using a Quantachrome ASiQwin-Autosorb Station 1 in a nitrogen adsorption and desorption isothermal curve and carbon dioxide adsorption; photoluminescence spectra were acquired using a fluorescence spectrophotometer (Hitachi, F-4600); the photocatalytic reduction product is detected by gas chromatography GC-2014; carbon monoxide isotope labeling was obtained using gas chromatography-mass spectrometry (GC-MS Agilent Technologies 7890B GC system and 5977B MSD); and detecting the in-situ Fourier transform infrared spectrum by a Nicolet IS-50FT-IR spectrometer.
Example 1
1. Preparation of FeV 2 O 4 /g-C 3 N 4
(1) Three-dimensional FeV 2 O 4 Stainless steel wire net (FeV) 2 O 4 ) The preparation of (1): firstly, a stainless steel wire mesh (2 cm multiplied by 2 cm) is sequentially ultrasonically cleaned for 20min by soapy water, acetone, ethanol and deionized water respectively, and then is dried in vacuum for standby application. 20mL of deionized water was added to a clean beaker followed by the sequential addition of 10mmol of NH 4 VO 3 And 5mmol of Bi (NO) 3 ) 3 ·5H 2 And O. The mixed solution is evenly stirred for 1h and then is filled into a polytetrafluoroethylene lining, and then a piece of dry and clean stainless steel wire mesh is arranged. And sealing the lining, putting the lining into a reaction kettle, putting the reaction kettle into an oven, and heating the reaction kettle to 160 ℃ for reaction for 48 hours. After the reaction kettle is naturally cooled to room temperature, the FeV is loaded 2 O 4 Taking out the stainless steel wire net, alternately washing the stainless steel wire net for 3 times by using deionized water and ethanol, and then drying the stainless steel wire net for 8 hours in vacuum at the temperature of 60 ℃ to obtain the target object.
(2) Three-dimensional FeV 2 O 4 /g-C 3 N 4 Stainless steel wire net (FeV) 2 O 4 /g-C 3 N 4 ) The preparation of (1): first, 2, 4-diamino-6-phenyl-1, 3, 5-triazine (9 g) and cyanuric acid (6.5 g) were dissolved in 200mL of deionized water and magnetically stirred at room temperature for 24h. Subsequently, the mixed suspension was subjected to suction filtration to effect solid-liquid separation. The white solid was placed in a 60 ℃ forced air drying cabinet for 8h. The dried white solid was then ground in a mortar to a white powder. Finally, a FeV chip 2 O 4 (the object obtained in step (1)) was placed in the bottom of a 30mL crucible, and the prepared white powder (1.5 g) was uniformly spread over FeV 2 O 4 Covering the surface of the crucible, putting the crucible into a tube furnace, introducing nitrogen, and heating to 500 ℃ at the speed of 2.5 ℃/min for 4 hours. After the tube furnace is naturally cooled to the room temperature, taking out the sample, placing the sample in deionized water, and removing unstable substances on the surface of the sample by ultrasonic treatment for 30min to obtain FeV 2 O 4 /g-C 3 N 4 。
2. Performance testing
(1) The sample was analyzed by Scanning Electron Microscope (SEM), and a scanning electron micrograph thereof was shown in fig. 1. In which (a-c) are FeV of different scales 2 O 4 SEM picture of (1); (d-f) FeV of different scale 2 O 4 /g-C 3 N 4 SEM image of (d).
(2) The sample was analyzed by a Transmission Electron Microscope (TEM) to obtain a transmission electron micrograph thereof. a. b are FeV with different scales 2 O 4 /g-C 3 N 4 A TEM image of (a).
(3) The obtained different samples were analyzed by a powder X-ray diffractometer to obtain the corresponding spectra as shown in fig. 3.
(4) FeV obtained by X-ray photoelectron spectrometer 2 O 4 /g-C 3 N 4 And analyzing to obtain a corresponding map, as shown in figure 4. Wherein (a) the total energy spectrum; (b) high resolution Fe 2 p; (c) a V2 p high resolution map; (d) O1 s high resolution; (e) C1 s high resolution; (f) N1 s high resolution.
(5) Measurement of ultraviolet-visible diffuse reflectance spectrum: adding 40mg of barium sulfate into 200mL of deionized water, performing ultrasonic treatment for 30min,and (3) carrying out suction filtration on the solution by using a suction filtration device, forming a thin layer of barium sulfate on the filter membrane, namely a blank sample, and carrying out sealing, storage and drying on the blank sample by using tinfoil. Adding 40mg of barium sulfate into 200mL of deionized water, performing ultrasonic treatment for 30min, simultaneously adding 5mg of sample into 25mL of deionized water, performing ultrasonic treatment for 30min, performing suction filtration on 200mL of barium sulfate solution by using a suction filtration device, performing suction filtration on 25mL of sample solution, forming a thin-layer sample on a filter membrane, combining the barium sulfate, namely the sample, and performing sealing, storage and drying by using tinfoil. In sequence to FeV 2 O 4 、g-C 3 N 4 And FeV 2 O 4 /g-C 3 N 4 The test was performed to obtain a uv-visible diffuse reflectance spectrum chart as (a) in fig. 5, and converted into a Tauc chart by the Tauc plot method as (b) in fig. 5.
(6) By using nitrogen gas absorption and desorption instrument and CO 2 Adsorption apparatus pair FeV 2 O 4 、g-C 3 N 4 And FeV 2 O 4 /g-C 3 N 4 Analysis was performed, resulting in fig. 6, in which: (a) Sample BET adsorption-desorption isotherm (inset: pore size distribution plot) and (b) sample CO 2 Adsorption profile.
(7) Preparing a photoelectrochemical test electrode and electrolyte: a10 mg sample was triturated and added to 80. Mu.L naphthol and 1.0mL ethanol to form a paste. Indium-doped tin oxide (ITO) electrode is sequentially coated with 1mol L of indium -1 And ultrasonically cleaning the glass substrate by NaOH, acetone, ethanol and deionized water for 20min, and then drying the glass substrate by nitrogen. Applying the paste to a fixed area (1.5 cm) -2 ) And (3) placing the ITO into a culture dish, sealing and storing the ITO by using tinfoil for drying, and then placing the ITO loaded with the catalyst into a 60 ℃ drying oven for drying for 12 hours, so that the catalyst is tightly loaded on the surface of the ITO, namely the preparation of the working electrode is finished. Platinum wire as counter electrode, ag/AgCl (3 mol L) -1 KCl) as reference electrode, 0.5mol L -1 Na 2 SO 4 As an electrolyte.
(8) Transient photocurrent response test: fixing the working electrode on the photocurrent detection device, assembling the photocurrent detection device, and adding 4mL 1mol L -1 Na 2 SO 4 5min nitrogen was introduced, and a platinum wire electrode and Ag/AgCl (3 mol L) were inserted -1 KCl) electrode, standing for 5min, turning on light source (3W)The perfect light-LED100B, with an ultraviolet filter, λ =450 nm) and the electrochemical workstation (CHI 660C) were run for 5min, and after the photocurrent stabilized, the photocurrent was testable by varying the different bias voltages to obtain the photocurrent at different potentials, as shown in fig. 7 (a).
(9) Electrochemical Impedance Spectroscopy (EIS) testing: electrochemical impedance is tested by using a Solartron 1255B Frequency Response Analyzer, a three-electrode system is adopted, a sheet catalyst is directly used as a working electrode, a platinum wire is used as a counter electrode, and Ag/AgCl (3 mol L) -1 KCl) as reference electrode. Impedance spectrum test frequency range: 0.01Hz-100kHz, as shown in (b) of FIG. 7.
(10) Photoluminescence spectrum test: a fluorescence spectrophotometer (Hitachi, F-4600) was used as shown in (c) of fig. 7.
(11) Model schottky test: it is in the range of 0.5mol L -1 Na 2 SO 4 The use of 1500Hz in the potential range from-2.0 to 3.0V, at different potentials, maintaining 10mV AC amplitude, as shown in figure 7 (d).
(12) Photocatalytic reduction of carbon dioxide is a gas-liquid phase reaction that is carried out in an environment of about 230mL reaction system under a 300W xenon lamp. Briefly, a 4cm piece was placed 2 Loading about 10mg of photocatalyst in 25mL of 0.5M Na 2 SO 3 In the reaction chamber. Before the reaction, all the gas in the reaction apparatus was evacuated, and argon gas was introduced into the system and further evacuated for 3 times. High purity carbon dioxide gas (99.999%) was then passed into the reaction chamber and the chamber pressure was reached. Finally, the adsorption was performed for 10h under light saturation in dark conditions, after which the reactor was under xenon illumination. The gas products were detected by gas chromatography (GC-2014, shimadzu, japan) and calibrated with standard gas mixtures. The total gas product was determined by retention time and the gas component concentration calculation was by external standard peak area method. Fig. 8 (a) is a graph of carbon monoxide yield versus time; (b) carbon dioxide reduction product yields for different samples; (c) Is FeV 2 O 4 /g-C 3 N 4 The photocatalytic stability of (3).
(13) Isotope labeling test: 12 c and 13 c-labelled CO 2 Carrying out the gas phaseThe retention time of the generated carbon monoxide was substantially the same by chromatography, as shown in (a) of fig. 9. By mass spectrometric detection, to 12 CO 2 As a carbon source, the product produced 12 CO (m/z = 28); to be provided with 13 CO 2 As a carbon source, the product produced 13 CO (m/z = 29), as shown in (b) of fig. 9. In summary, the photocatalytic product is derived from CO 2 And (4) transformation.
(14) Active species detection: under the irradiation of light, the photocatalyst forms OH on the surface, and the terephthalic acid captures the OH and forms a new product which is verified by photoluminescence spectra. In general, 0.05g of the sample was ultrasonically dispersed in 25mL of a solution containing 0.5mmol L -1 And 2mmol L of terephthalic acid -1 To the sodium hydroxide mixed solution. The dispersion was then placed in the light and sampled every 10min for photoluminescence spectroscopy, the results of which are shown in FIG. 10.
(15) In-situ Fourier transform infrared detection: before experimental testing, the samples were placed in a vacuum oven at 170 ℃ for 6h to remove residues adsorbed on the surface of the material. First, in-situ fourier transform infrared spectroscopy is performed under dark conditions to collect background signals. Then, carbon dioxide is introduced into the system to subtract the background value so as to obtain the in-situ Fourier transform infrared spectrum. The in-situ Fourier transform infrared spectroscopy analysis is carried out in two successive steps. The detection results are shown in fig. 11. Wherein: first, under dark conditions, mixed CO was continuously introduced 2 And steam in FeV 2 O 4 /g-C 3 N 4 Feeding CO 2 And (4) adsorbing. Then, the reactor was illuminated with an LED lamp for 1h.
Example 2
1. Preparation of FeV 2 O 4 /g-C 3 N 4
(1) Three-dimensional FeV 2 O 4 Stainless steel wire net (FeV) 2 O 4 ) The preparation of (1): firstly, a stainless steel wire mesh (2 cm multiplied by 2 cm) is sequentially ultrasonically cleaned for 20min by soapy water, acetone, ethanol and deionized water respectively, and then is dried in vacuum for standby application. 15mL of deionized water was added to a clean beaker followed by the sequential addition of 8mmol of NH 4 VO 3 And 4mmol of Bi (NO) 3 ) 3 ·5H 2 And (O). The mixed solution is evenly stirred for 1h and then is filled into a polytetrafluoroethylene lining, and then a piece of dry and clean stainless steel wire mesh is arranged. And sealing the lining, putting the lining into a reaction kettle, putting the reaction kettle into an oven, and heating the reaction kettle to 150 ℃ for reaction for 45 hours. After the reaction kettle is naturally cooled to room temperature, the FeV is loaded 2 O 4 Taking out the stainless steel wire net, alternately washing the stainless steel wire net for 3 times by using deionized water and ethanol, and then drying the stainless steel wire net for 8 hours in vacuum at the temperature of 60 ℃ to obtain the target object.
(2) Three-dimensional FeV 2 O 4 /g-C 3 N 4 Stainless steel wire net (FeV) 2 O 4 /g-C 3 N 4 ) The preparation of (1): first, 2, 4-diamino-6-phenyl-1, 3, 5-triazine (8 g) and cyanuric acid (5 g) were dissolved in 200mL of deionized water and magnetically stirred at room temperature for 24h. Subsequently, the mixed suspension was subjected to suction filtration to effect solid-liquid separation. The white solid was dried in an air-blast drying oven at 50 ℃ for 6h. The dried white solid was then ground in a mortar to a white powder. Finally, a FeV chip 2 O 4 (the object obtained in step (1)) was placed in a 30mL crucible bottom, and the prepared white powder (1 g) was uniformly spread over FeV 2 O 4 Covering the surface of the crucible, putting the crucible into a tube furnace, introducing nitrogen, and heating to 480 ℃ at the speed of 2 ℃/min for 3 hours. After the tube furnace is naturally cooled to the room temperature, taking out the sample, placing the sample in deionized water, and removing unstable substances on the surface of the sample by ultrasonic treatment for 30min to obtain FeV 2 O 4 /g-C 3 N 4 。
2. Performance testing
After 6h of reaction, the yield of the main product carbon monoxide is as follows: feV 2 O 4 /g-C 3 N 4 (56.72μmol g -1 )> g-C 3 N 4 (11.49μmol g -1 )>FeV 2 O 4 (0.01465μmol g -1 ). In addition, no catalyst, either no light or no carbon dioxide, produces essentially no carbon monoxide.
Average product formation for three materials: feV 2 O 4 /g-C 3 N 4 (carbon monoxide: 9.43. Mu. Mol g) -1 h -1 (ii) a Methane: 0.708μmol g -1 h -1 )>g-C 3 N 4 (carbon monoxide: 1.79. Mu. Mol g -1 h -1 (ii) a Methane: 0.618. Mu. Mol g -1 h -1 )>FeV 2 O 4 (carbon monoxide: 0.0025. Mu. Mol g -1 h -1 (ii) a Methane: 0.0008. Mu. Mol g -1 h -1 )。
FeV 2 O 4 /g-C 3 N 4 After 5 cycles, the yield of the photocatalytic reduction carbon dioxide product is not changed basically (after 1 st cycle: carbon monoxide: 57.03. Mu. Mol g) -1 (ii) a Methane: 4.382. Mu. Mol g -1 . After the end of the 5 th cycle: carbon monoxide: 55.46. Mu. Mol g -1 (ii) a Methane: 3.987. Mu. Mol g -1 . ) Thus, the stability is very good.
Example 3
1. Preparation of FeV 2 O 4 /g-C 3 N 4
(1) Three-dimensional FeV 2 O 4 Stainless steel wire net (FeV) 2 O 4 ) The preparation of (1): firstly, a stainless steel wire mesh (2 cm multiplied by 2 cm) is sequentially and respectively ultrasonically cleaned for 20min by soapy water, acetone, ethanol and deionized water, and then is dried in vacuum for standby. 25mL of deionized water was added to a clean beaker followed by the sequential addition of 12mmol of NH 4 VO 3 And 6mmol of Bi (NO) 3 ) 3 ·5H 2 And O. The mixed solution is evenly stirred for 1h and then is filled into a polytetrafluoroethylene lining, and then a piece of dry and clean stainless steel wire mesh is arranged. And sealing the lining, putting the lining into a reaction kettle, putting the reaction kettle into an oven, and heating the reaction kettle to 170 ℃ for reaction for 51 hours. After the reaction kettle is naturally cooled to room temperature, the FeV is loaded 2 O 4 The stainless steel wire net is taken out, washed for 3 times by deionized water and ethanol alternately, and then dried for 8 hours in vacuum at 60 ℃ to obtain the target object.
(2) Three-dimensional FeV 2 O 4 /g-C 3 N 4 Stainless steel wire net (FeV) 2 O 4 /g-C 3 N 4 ) The preparation of (1): first, 2, 4-diamino-6-phenyl-1, 3, 5-triazine (10 g) and cyanuric acid (8 g) were dissolved in 200mL of deionized water and magnetically stirred at room temperature for 24h. Then, mixedAnd carrying out suction filtration on the suspension to realize solid-liquid separation. The white solid was dried in an air-blast dry box at 70 ℃ for 10h. The dried white solid was then ground in a mortar to a white powder. Finally, a FeV chip 2 O 4 (the object obtained in step (1)) was placed in a 30mL crucible bottom and the prepared white powder (2 g) was uniformly spread over FeV 2 O 4 Covering the surface of the crucible, putting the crucible into a tube furnace, introducing nitrogen, heating to 520 ℃ at the speed of 3 ℃/min, and keeping for 5 hours. After the tube furnace is naturally cooled to the room temperature, taking out the sample, placing the sample in deionized water, and removing unstable substances on the surface of the sample by ultrasonic treatment for 30min to obtain FeV 2 O 4 /g-C 3 N 4 。
2. Performance test
After 6h of reaction, the yield of the main product carbon monoxide is as follows: feV 2 O 4 /g-C 3 N 4 (56.83μmol g -1 )> g-C 3 N 4 (11.54μmol g -1 )>FeV 2 O 4 (0.01491μmol g -1 ). In addition, no catalyst, either no light or no carbon dioxide, produces essentially no carbon monoxide.
Average product formation of three materials: feV 2 O 4 /g-C 3 N 4 (carbon monoxide: 9.48. Mu. Mol g -1 h -1 (ii) a Methane: 0.724. Mu. Mol g -1 h -1 )>g-C 3 N 4 (carbon monoxide: 1.85. Mu. Mol g -1 h -1 (ii) a Methane: 0.654. Mu. Mol g -1 h -1 )>FeV 2 O 4 (carbon monoxide: 0.0029. Mu. Mol g -1 h -1 (ii) a Methane: 0.0011. Mu. Mol g -1 h -1 )。
FeV 2 O 4 /g-C 3 N 4 After 5 cycles, the yield of the photocatalytic reduction carbon dioxide product was not substantially changed (after the end of cycle 1: carbon monoxide: 57.11. Mu. Mol g) -1 (ii) a Methane: 4.394. Mu. Mol g -1 . After the end of the 5 th cycle: carbon monoxide: 55.69 μmol g -1 (ii) a Methane: 4.031. Mu. Mol g -1 . ) Thus, the stability is very good.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.

Claims (8)

1. Honeycomb FeV 2 O 4 The preparation method of the composite carbon nitride loaded stainless steel wire mesh composite material is characterized by comprising the following steps of:
(1) Reacting NH 4 VO 3 And Bi (NO) 3 ) 3 ·5H 2 Dissolving O in water, stirring, filling the mixture into a polytetrafluoroethylene lining, and putting the polytetrafluoroethylene lining into a dry and clean stainless steel screen; then, filling the polytetrafluoroethylene lining into a reaction kettle, heating to 150-170 ℃ and reacting for 45-51h to obtain three-dimensional FeV 2 O 4 A stainless steel wire mesh;
(2) Dissolving 2, 4-diamino-6-phenyl-1, 3, 5-triazine and cyanuric acid in water, stirring for reacting for a period of time, carrying out solid-liquid separation on the suspension to obtain white solid, drying the white solid, and grinding the white solid into white powder; uniformly spreading white powder on the three-dimensional FeV prepared in the step (1) 2 O 4 Heating to 480-520 ℃ for 3-5h under the protection of nitrogen to obtain three-dimensional FeV 2 O 4 /g-C 3 N 4 A stainless steel wire mesh;
wherein the stainless steel wire net in the step (1) provides an iron source;
in the step (2), the mass ratio of the 2, 4-diamino-6-phenyl-1, 3, 5-triazine to the cyanuric acid is (8-10): (5-8);
in the step (2), the three-dimensional FeV prepared in the step (1) is tiled 2 O 4 The mass range of the white powder on the surface of the stainless steel wire mesh is as follows: 1.0-2.0g white powder/(8-12) mmol NH 4 VO 3 The FeV thus obtained 2 O 4 。
2. A honeycomb FeV according to claim 1 2 O 4 Composite nitridingThe preparation method of the carbon-loaded stainless steel wire mesh composite material is characterized in that in the step (1), NH is added 4 VO 3 And Bi (NO) 3 ) 3 ·5H 2 The molar ratio of O is (8-12): (4-6); wherein the stainless steel wire mesh provides an excess of iron source.
3. A cellular FeV according to claim 1 2 O 4 The preparation method of the composite carbon nitride loaded stainless steel wire mesh composite material is characterized in that in the step (1), after the heating reaction is finished, the reaction kettle is naturally cooled to room temperature, and then the loaded FeV is subjected to 2 O 4 Taking out the stainless steel wire net, alternately washing with water and ethanol, and then drying in vacuum to obtain the three-dimensional FeV 2 O 4 Stainless steel wire mesh.
4. A cellular FeV according to claim 1 2 O 4 The preparation method of the composite carbon nitride loaded stainless steel wire mesh composite material is characterized in that in the step (2), 2, 4-diamino-6-phenyl-1, 3, 5-triazine and cyanuric acid are dissolved in water, and then stirred and reacted for 24 hours.
5. A honeycomb FeV according to claim 1 2 O 4 The preparation method of the composite carbon nitride loaded stainless steel wire mesh composite material is characterized in that in the step (2), the white solid is dried for 6-10 hours at the temperature of 50-70 ℃.
6. A cellular FeV according to claim 1 2 O 4 The preparation method of the composite carbon nitride loaded stainless steel wire mesh composite material is characterized in that in the step (2), white powder is uniformly paved on the three-dimensional FeV prepared in the step (1) 2 O 4 Introducing nitrogen after the surface of the stainless steel wire mesh, and heating to 480-520 ℃ at the speed of 2-3 ℃/min.
7. A honeycomb FeV prepared by the method of any one of claims 1 to 6 2 O 4 Composite carbon nitride loaded stainless steel wire mesh composite materialAnd (4) feeding.
8. The honeycomb FeV of claim 7 2 O 4 The composite material of the composite carbon nitride loaded stainless steel wire mesh is applied to the preparation of carbon monoxide by photocatalysis of carbon dioxide.
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