CN113813967A - LaFeO3/In2S3Preparation method and application of composite material - Google Patents
LaFeO3/In2S3Preparation method and application of composite material Download PDFInfo
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- 229910002321 LaFeO3 Inorganic materials 0.000 title claims abstract description 78
- 239000002131 composite material Substances 0.000 title claims abstract description 47
- 238000000034 method Methods 0.000 title abstract description 8
- 229910017771 LaFeO Inorganic materials 0.000 claims abstract description 70
- 239000004005 microsphere Substances 0.000 claims abstract description 29
- 239000002243 precursor Substances 0.000 claims abstract description 24
- 238000002360 preparation method Methods 0.000 claims abstract description 23
- 238000003756 stirring Methods 0.000 claims abstract description 23
- 230000001699 photocatalysis Effects 0.000 claims abstract description 22
- 238000006243 chemical reaction Methods 0.000 claims abstract description 17
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims abstract description 13
- -1 polytetrafluoroethylene Polymers 0.000 claims abstract description 13
- 229920001343 polytetrafluoroethylene Polymers 0.000 claims abstract description 13
- 239000004810 polytetrafluoroethylene Substances 0.000 claims abstract description 13
- PSCMQHVBLHHWTO-UHFFFAOYSA-K Indium trichloride Inorganic materials Cl[In](Cl)Cl PSCMQHVBLHHWTO-UHFFFAOYSA-K 0.000 claims abstract description 12
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 12
- 239000000725 suspension Substances 0.000 claims abstract description 12
- 238000007146 photocatalysis Methods 0.000 claims abstract description 9
- 239000002957 persistent organic pollutant Substances 0.000 claims abstract description 6
- 239000000243 solution Substances 0.000 claims description 50
- KRKNYBCHXYNGOX-UHFFFAOYSA-N citric acid Chemical compound OC(=O)CC(O)(C(O)=O)CC(O)=O KRKNYBCHXYNGOX-UHFFFAOYSA-N 0.000 claims description 21
- 238000001035 drying Methods 0.000 claims description 15
- VCJMYUPGQJHHFU-UHFFFAOYSA-N iron(3+);trinitrate Chemical compound [Fe+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O VCJMYUPGQJHHFU-UHFFFAOYSA-N 0.000 claims description 12
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical group [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 claims description 11
- 229940043267 rhodamine b Drugs 0.000 claims description 11
- 238000000137 annealing Methods 0.000 claims description 10
- 239000000463 material Substances 0.000 claims description 9
- 239000002245 particle Substances 0.000 claims description 8
- FYDKNKUEBJQCCN-UHFFFAOYSA-N lanthanum(3+);trinitrate Chemical compound [La+3].[O-][N+]([O-])=O.[O-][N+]([O-])=O.[O-][N+]([O-])=O FYDKNKUEBJQCCN-UHFFFAOYSA-N 0.000 claims description 6
- 239000007864 aqueous solution Substances 0.000 claims description 2
- 239000000356 contaminant Substances 0.000 claims description 2
- 230000035484 reaction time Effects 0.000 claims description 2
- 238000004519 manufacturing process Methods 0.000 claims 1
- 230000009286 beneficial effect Effects 0.000 abstract description 7
- 230000008569 process Effects 0.000 abstract description 6
- 239000000126 substance Substances 0.000 abstract description 6
- 230000000694 effects Effects 0.000 abstract description 5
- 238000013032 photocatalytic reaction Methods 0.000 abstract description 5
- 230000003197 catalytic effect Effects 0.000 abstract description 4
- 239000006185 dispersion Substances 0.000 abstract description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 18
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 15
- 238000005406 washing Methods 0.000 description 14
- 238000006731 degradation reaction Methods 0.000 description 9
- 239000008367 deionised water Substances 0.000 description 9
- 229910021641 deionized water Inorganic materials 0.000 description 9
- 230000015556 catabolic process Effects 0.000 description 8
- 239000004065 semiconductor Substances 0.000 description 8
- 238000005286 illumination Methods 0.000 description 7
- 229910001868 water Inorganic materials 0.000 description 6
- 230000015572 biosynthetic process Effects 0.000 description 5
- 150000001875 compounds Chemical class 0.000 description 5
- 238000005516 engineering process Methods 0.000 description 5
- 238000000227 grinding Methods 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000001816 cooling Methods 0.000 description 4
- 238000007254 oxidation reaction Methods 0.000 description 4
- 239000011941 photocatalyst Substances 0.000 description 4
- 238000003786 synthesis reaction Methods 0.000 description 4
- 238000001132 ultrasonic dispersion Methods 0.000 description 4
- 238000001291 vacuum drying Methods 0.000 description 4
- 231100000053 low toxicity Toxicity 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 238000009210 therapy by ultrasound Methods 0.000 description 3
- 229910052724 xenon Inorganic materials 0.000 description 3
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 231100001240 inorganic pollutant Toxicity 0.000 description 2
- 230000033116 oxidation-reduction process Effects 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000006479 redox reaction Methods 0.000 description 2
- 238000003911 water pollution Methods 0.000 description 2
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 1
- 229910002370 SrTiO3 Inorganic materials 0.000 description 1
- OUUQCZGPVNCOIJ-UHFFFAOYSA-M Superoxide Chemical compound [O-][O] OUUQCZGPVNCOIJ-UHFFFAOYSA-M 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000013543 active substance Substances 0.000 description 1
- 238000005054 agglomeration Methods 0.000 description 1
- 230000002776 aggregation Effects 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 150000004770 chalcogenides Chemical class 0.000 description 1
- 238000002425 crystallisation Methods 0.000 description 1
- 230000008025 crystallization Effects 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002474 experimental method Methods 0.000 description 1
- 229910021389 graphene Inorganic materials 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 231100000086 high toxicity Toxicity 0.000 description 1
- 230000003301 hydrolyzing effect Effects 0.000 description 1
- TUJKJAMUKRIRHC-UHFFFAOYSA-N hydroxyl Chemical compound [OH] TUJKJAMUKRIRHC-UHFFFAOYSA-N 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 230000004298 light response Effects 0.000 description 1
- 230000001089 mineralizing effect Effects 0.000 description 1
- 239000002159 nanocrystal Substances 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
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- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/02—Sulfur, selenium or tellurium; Compounds thereof
- B01J27/04—Sulfides
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J35/00—Catalysts, in general, characterised by their form or physical properties
- B01J35/30—Catalysts, in general, characterised by their form or physical properties characterised by their physical properties
- B01J35/39—Photocatalytic properties
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/30—Treatment of water, waste water, or sewage by irradiation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/725—Treatment of water, waste water, or sewage by oxidation by catalytic oxidation
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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Abstract
The invention relates to the technical field of photocatalysis, and particularly discloses LaFeO3/In2S3The preparation method and the application of the composite material comprise the following steps: s1, preparing LaFeO3Nano-microspheres; s2, preparing LaFeO-containing3In (2) of2S3Precursor solution: LaFeO is added3The nano-microspheres are dispersed in InCl3In the solution to obtain LaFeO-containing3The suspension of (1) is added with Na dropwise under the condition of vigorous stirring2S solution to obtain LaFeO-containing solution3In (2) of2S3Precursor solution; s3, preparing LaFeO3/In2S3The composite material comprises the following components: containing LaFeO3In (2) of2S3The precursor solution is subjected to hydrothermal reaction in a polytetrafluoroethylene reaction kettle to obtain LaFeO3/In2S3A composite material. The preparation method has simple process, easy operation and low cost, and prepares the LaFeO with the Z-type heterostructure3/In2S3The composite material has good photoelectric catalytic performance, good chemical stability and easy dispersion, is beneficial to the photocatalytic reaction, improves the photocatalytic effect, is applied to the field of photocatalytic degradation of organic pollutants, and has good photocatalytic degradation effect.
Description
Technical Field
The invention relates to the technical field of photocatalysis, in particular to LaFeO3/In2S3A preparation method and application of the composite material.
Background
Because the current industry is rapidly developed, the water pollution is increasingly serious, and the serious threat to the human health is caused, the development and the utilization of the high-efficiency water pollution treatment technology are not slow. The semiconductor material directly and effectively utilizes solar energy in the environment to generate electron-hole pairs and a series of active substances with high oxidation-reduction potential to drive surface oxidation-reduction reaction, thereby effectively oxidizing and hydrolyzing various organic or inorganic pollutants in water body, and even completely mineralizing the organic or inorganic pollutants into H2O and CO2. The semiconductor photocatalysis technology has the characteristics of low cost, low toxicity, solar energy utilization, controllability, strong expandability and the like, so that the semiconductor photocatalysis technology is widely concerned by people. However, the existing photocatalytic technology still faces some problems to be solved urgently in the aspect of being applied to sewage treatment, such as low solar energy utilization rate, low quantum efficiency, serious recombination of photo-generated electron-hole pairs and the like.
The redox reactions involved in the photocatalytic process indicate that: the conduction band of the catalyst needs to be higher than the potential of the superoxide radical and the valence band lower than the potential of the hydroxyl radical. The photocatalytic semiconductor material currently involved comprises C3N4CdS, ternary chalcogenides MINxSyTwo-dimensional material graphene, and the like. However, these materials have the disadvantages of difficult preparation, difficult dispersion, high toxicity, insufficient stability, and the like. Commonly used wide band gap semiconductors, e.g. TiO2、ZnO、SrTiO3、WO3Niobate, tantalate and the like, although wide band gap semiconductors have the advantages of good stability, low toxicity and the like, the band gap is too wide, the effective utilization rate of sunlight is low, and the preparation is complex. Therefore, the purpose isThe prior photocatalysis technology has the problems of narrow absorption range, serious recombination of photo-generated charges, insufficient oxidation-reduction capability and the like.
Disclosure of Invention
The invention aims to provide LaFeO against the prior technical situation3/In2S3The preparation method has simple process, easy operation and low cost, and prepares the Z-type heterostructure LaFeO3/In2S3The composite material has good photoelectric catalytic performance, good chemical stability and easy dispersion, is beneficial to the photocatalytic reaction, improves the photocatalytic effect, is applied to the field of photocatalytic degradation of organic pollutants, and has good photocatalytic degradation effect.
In order to achieve the purpose, the invention adopts the following technical scheme:
LaFeO3/In2S3The preparation method of the composite material is characterized by comprising the following steps:
s1, preparing LaFeO3Nano-microspheres;
the invention adopts micron-sized LaFeO3The spherical structure of the nano-microsphere is not easy to agglomerate, compared with the nano-scale small particle LaFeO3Nano material, micron-sized LaFeO3The nano microspheres are less prone to agglomeration and are convenient to compound with other materials to form a heterojunction;
s2, preparing LaFeO-containing3In (2) of2S3Precursor solution: LaFeO is added3The nano-microspheres are dispersed in InCl3In the solution to obtain LaFeO-containing3The suspension of (1) is added with Na dropwise under the condition of vigorous stirring2S solution to obtain LaFeO-containing solution3In (2) of2S3Precursor solution;
s3, preparing LaFeO3/In2S3The composite material comprises the following components: containing LaFeO3In (2) of2S3The precursor solution is subjected to hydrothermal reaction in a polytetrafluoroethylene reaction kettle to obtain LaFeO3/In2S3A composite material.
LaFeO3Is a band gap of2.3eV p-type semiconductor material with wide visible light response range, but LaFeO3Perovskite crystals generally have a small specific surface area and a large grain size, and thus result in a small contact surface with contaminants and low photocatalytic activity. In2S3Is an n-type semiconductor material with a band gap of 2.2eV, has a wide visible light absorption range, good chemical stability and low toxicity, and In2S3Has a high position of a conduction band and has excellent reduction performance In a photocatalytic reaction, but In2S3The crystallinity of the crystal is poor, so that serious photo-generated charge recombination is easy to occur, and the improvement of the photocatalytic activity is seriously restricted.
Compared with single LaFeO3And In2S3In the invention, firstly, the LaFeO synthesized by hydro-thermal synthesis is used3Annealing to enhance LaFeO3The crystallization property of (1) reduces LaFeO3Carrying out grinding treatment on the surface defects of the nanocrystal material to obtain LaFeO with the particle size of 2.5-4 mu m3Nanospheres of LaFeO3The nano-microspheres are fully dispersed in InCl3Suspension, followed by dropwise addition of Na under vigorous stirring2S solution of In2S3Precursor and LaFeO3Fully contacting, and performing hydrothermal reaction on LaFeO3In is grown on the surface of2S3Wherein In2S3The particle diameter of (A) is 100-720 nm, due to LaFeO3Is micron-sized, and when used as a photocatalyst alone, the In of the invention has poor degradation reaction due to the fact that the specific surface area is too small to be In full contact with pollutants to be degraded2S3The grain diameter of the particles is obviously smaller nano-size and can be uniformly dispersed in LaFeO3Uniformly growing on the surface of the nano microsphere to obtain LaFeO with Z-type heterostructure3/In2S3Composite materials, see also LaFeO shown in FIG. 13And In2S3Compared with a position comparison diagram of a conduction valence band of a vacuum energy level, the energy level structure matching of the conduction valence band and the conduction valence band is seen, and the formation of a Z-type heterostructure is facilitated.
LaFeO of the invention3/In2S3The preparation method has simple process, easy operation and low cost, and can ensure In2S3Precursor and LaFeO3Sufficiently contacting to make In of nanometer order2S3In LaFeO3Uniformly growing on the nano-microsphere to obtain LaFeO3/In2S3The composite material is of a Z-type heterostructure, has good photoelectric catalytic performance and chemical stability, is easy to disperse, is beneficial to the photocatalytic reaction and improves the photocatalytic effect.
Preferably, LaFeO in step S23And In2S3The weight ratio of the LaFeO to the LaFeO is 1-8: 1, and more preferably, the LaFeO is obtained in step S23And In2S3The weight ratio of the LaFeO to the LaFeO is 2:1, and tests show that the LaFeO is prepared under the weight ratio3/In2S3The degradation rate of the composite material on rhodamine B is as high as 98%, and the degradation effect is good.
Preferably, step S1 includes the steps of:
adding ferric nitrate, lanthanum nitrate and citric acid into the aqueous solution, stirring and dissolving, transferring into a polytetrafluoroethylene reaction kettle, putting into a constant-temperature drying oven, and reacting for 12h at the temperature of 180 ℃ to obtain LaFeO3The product is then annealed and ground at high temperature to obtain LaFeO3And (4) nano microspheres.
The invention relates to LaFeO3In the hydrothermal synthesis process, milder citric acid is adopted, so that the reaction can be slowed down to be beneficial to the generation of nano particles, and the nano microspheres are further obtained.
Preferably, step S1 further includes the following steps: LaFeO3And (4) alternately centrifuging and washing the product by using ethanol and deionized water, and drying after washing.
Preferably, the LaFeO3The particle size of the nano-microspheres is 2.5-4 mu m, and the In2S3The particle size of (A) is 100 to 720 nm.
Preferably, the high temperature annealing in step S1 is annealing at 800 ℃ for 4h, under which a better annealing effect can be obtained.
Preferably, the reaction temperature of the hydrothermal reaction in step S3 is 180 ℃ and the reaction time is 12 h.
Preferably, Na is dropwise added in step S22And (5) continuing stirring and reacting for 5 hours after the solution S, wherein the stirring speed of the violent stirring is 800-1000 rpm.
Another object of the present invention is to provide the above LaFeO3/In2S3The application of the composite material in photocatalysis provides the LaFeO3/In2S3The use of composite materials in photocatalysis.
Another object of the present invention is to provide LaFeO as described above3/In2S3The application of the composite material in photocatalytic degradation of organic pollutants.
Preferably, the organic pollutant is rhodamine B, and the photocatalytic degradation is carried out under the illumination condition of visible light.
Wherein, the degradation of rhodamine B pollutant belongs to photocatalytic oxidation reaction, and the synthesized LaFeO of the invention3/In2S3The composite material enriches more active sites of the photocatalytic oxidation reaction, is beneficial to the photocatalytic oxidation reaction and is suitable for the application of the photocatalytic oxidation reaction.
The invention has the beneficial effects that:
LaFeO of the invention3/In2S3The preparation method has simple process, easy operation and low cost, and can ensure In2S3Precursor and LaFeO3Sufficiently contacting to make In of nanometer order2S3In LaFeO3Uniformly growing on the nano-microsphere to obtain LaFeO3/In2S3The composite material is of a Z-type heterostructure, has good photoelectric catalytic performance and chemical stability, is easy to disperse, is beneficial to the photocatalytic reaction and improves the photocatalytic effect.
LaFeO prepared by the invention3/In2S3The composite material can be applied to the field of photocatalysis, is particularly suitable for the field of photocatalytic degradation of organic pollutants, and has good degradation effect and good chemical stability.
Drawings
FIG. 1 shows LaFeO3And In2S3Comparison of conduction band position with respect to vacuum level.
FIG. 2 shows LaFeO obtained in examples 1 to 3 of the present invention3/In2S3And comparing the test results of the photocatalytic degradation performance of the composite material.
Detailed Description
The invention is further illustrated by the following examples in conjunction with the accompanying drawings:
example 1
LaFeO3/In2S3The preparation method of the composite material comprises the following steps:
s1, preparing LaFeO3Nano-microspheres:
1) synthesis of LaFeO by hydrothermal method3: adding 0.01M ferric nitrate, 0.01M lanthanum nitrate and 0.025M citric acid into 90ml of water solution, stirring and dissolving, transferring into a 100ml polytetrafluoroethylene reaction kettle, putting into a constant temperature drying box, and reacting for 12h at the temperature of 180 ℃ to obtain LaFeO3A product;
2) naturally cooling to room temperature, then alternately centrifugally washing for three times by using ethanol and deionized water, drying at the temperature of 80 ℃ after washing, annealing for 4 hours at the temperature of 800 ℃, and grinding to obtain LaFeO3Nano-microspheres;
s2, preparing LaFeO-containing3In (2) of2S3Precursor solution:
1) preparation of InCl3A solution;
2) 0.6g of LaFeO prepared as described above was weighed3Nano microsphere, ultrasonic dispersion in InCl3In the solution to obtain LaFeO-containing3The suspension of (4);
3) dropwise adding Na into the suspension under the condition of violent stirring (800 rpm-1000 rpm)2The S solution is continuously stirred vigorously for 5 hours to obtain the LaFeO-containing solution3In (2) of2S3Precursor solution;
s3, preparing LaFeO3/In2S3The composite material comprises the following components: containing LaFeO3In (2) of2S3Transferring the precursor solution into a 100ml polytetrafluoroethylene reaction kettle, reacting for 12h at the temperature of 180 ℃, alternately centrifuging and washing the obtained compound for three times by using ethanol and deionized water, and drying for 12h in a vacuum drying oven at the temperature of 50 ℃ to obtain LaFeO3And In2S3The weight portion ratio of the LaFeO to the LaFeO is 8:13/In2S3A composite material.
Testing of photocatalytic degradation performance:
preparing 25mg/L rhodamine B solution, and then adding 20mg of LaFeO prepared above3/In2S3The composite material is photocatalyst, and is taken out after ultrasonic treatment for 5 min. Stirring for 30min under dark condition, and illuminating with xenon lamp simulated sunlight for 30 min; and (3) taking 1ml of sample every 5min from the beginning to the end of the illumination in the illumination period to detect the degradation rate of the rhodamine B, wherein experiments prove that the degradation rate of the rhodamine B is 16% after 30 min.
Example 2
LaFeO3/In2S3The preparation method of the composite material comprises the following steps:
s1, preparing LaFeO3Nano-microspheres:
3) synthesis of LaFeO by hydrothermal method3: adding 0.01M ferric nitrate, 0.01M lanthanum nitrate and 0.025M citric acid into 90ml of water solution, stirring and dissolving, transferring into a 100ml polytetrafluoroethylene reaction kettle, putting into a constant temperature drying box, and reacting for 12h at the temperature of 180 ℃ to obtain LaFeO3A product;
4) naturally cooling to room temperature, then alternately centrifugally washing for three times by using ethanol and deionized water, drying at the temperature of 80 ℃ after washing, annealing for 4 hours at the temperature of 800 ℃, and grinding to obtain LaFeO3Nano-microspheres;
s2, preparing LaFeO-containing3In (2) of2S3Precursor solution:
4) preparation of InCl3A solution;
5) 0.15g of LaFeO prepared as described above was weighed3Nano microsphere, ultrasonic dispersion in InCl3Solutions ofTo obtain the LaFeO-containing3The suspension of (4);
6) dropwise adding Na into the suspension under the condition of violent stirring (800-1000 rpm)2The S solution is continuously stirred vigorously for 5 hours to obtain the LaFeO-containing solution3In (2) of2S3Precursor solution;
s3, preparing LaFeO3/In2S3The composite material comprises the following components: containing LaFeO3In (2) of2S3Transferring the precursor solution into a 100ml polytetrafluoroethylene reaction kettle, reacting for 12h at the temperature of 180 ℃, alternately centrifuging and washing the obtained compound for three times by using ethanol and deionized water, and drying for 12h in a vacuum drying oven at the temperature of 50 ℃ to obtain LaFeO3And In2S3The weight portion ratio of the LaFeO to the LaFeO is 2:13/In2S3A composite material.
Testing of photocatalytic degradation performance: firstly preparing 25mg/L rhodamine B solution, and then adding 20mg of the LaFeO prepared above3/In2S3The composite material is photocatalyst, and is taken out after ultrasonic treatment for 5 min. Stirring for 30min under dark condition, and illuminating with xenon lamp simulated sunlight for 30 min; a1 ml sample is taken every 5min from the beginning to the end of the illumination in the illumination period to detect the degradation rate of the rhodamine B to be 98%.
Example 3
LaFeO3/In2S3The preparation method of the composite material comprises the following steps:
s1, preparing LaFeO3Nano-microspheres:
5) synthesis of LaFeO by hydrothermal method3: adding 0.01M ferric nitrate, 0.01M lanthanum nitrate and 0.025M citric acid into 90ml of water solution, stirring and dissolving, transferring into a 100ml polytetrafluoroethylene reaction kettle, putting into a constant temperature drying box, and reacting for 12h at the temperature of 180 ℃ to obtain LaFeO3A product;
6) naturally cooling to room temperature, then alternately centrifugally washing for three times by using ethanol and deionized water, drying at the temperature of 80 ℃ after washing, annealing for 4 hours at the temperature of 800 ℃, and grinding to obtain LaFeO3Nano-microspheres;
s2, preparing LaFeO-containing3In (2) of2S3Precursor solution:
7) preparation of InCl3A solution;
8) 0.075g of LaFeO prepared above was weighed out3Nano microsphere, ultrasonic dispersion in InCl3In the solution to obtain LaFeO-containing3The suspension of (4);
9) dropwise adding Na into the suspension under the condition of violent stirring (800 rpm-1000 rpm)2The S solution is continuously stirred vigorously for 5 hours to obtain the LaFeO-containing solution3In (2) of2S3Precursor solution;
s3, preparing LaFeO3/In2S3The composite material comprises the following components: containing LaFeO3In (2) of2S3Transferring the precursor solution into a 100ml polytetrafluoroethylene reaction kettle, reacting for 12h at the temperature of 180 ℃, alternately centrifuging and washing the obtained compound for three times by using ethanol and deionized water, and drying for 12h in a vacuum drying oven at the temperature of 50 ℃ to obtain LaFeO3And In2S3The weight portion ratio of the LaFeO to the LaFeO is 1:13/In2S3A composite material.
Testing of photocatalytic degradation performance: firstly preparing 25mg/L rhodamine B solution, and then adding 20mg of the LaFeO prepared above3/In2S3The composite material is photocatalyst, and is taken out after ultrasonic treatment for 5 min. Stirring for 30min under dark condition, and illuminating with xenon lamp simulated sunlight for 30 min; a1 ml sample is taken every 5min from the beginning to the end of the illumination in the illumination period to detect that the degradation rate of rhodamine B is 56%.
Example 4
LaFeO3/In2S3The preparation method of the composite material comprises the following steps:
s1, preparing LaFeO3Nano-microspheres:
7) synthesis of LaFeO by hydrothermal method3: adding 0.01M ferric nitrate, 0.01M lanthanum nitrate and 0.025M citric acid into 90ml of water solution, stirring for dissolving, transferring into a 100ml polytetrafluoroethylene reaction kettle, placing into a constant temperature drying box, and strip-forming at 180 DEG CReacting for 12 hours under the condition of the reaction to obtain LaFeO3；
8) Naturally cooling to room temperature, then alternately centrifugally washing for three times by using ethanol and deionized water, drying at the temperature of 80 ℃ after washing, annealing for 4 hours at the temperature of 800 ℃, and grinding to obtain LaFeO3Nano-microspheres;
s2, preparing LaFeO-containing3In (2) of2S3Precursor solution:
10) preparation of InCl3A solution;
11) weighing appropriate amount of the prepared LaFeO3Nano microsphere, ultrasonic dispersion in InCl3In the solution to obtain LaFeO-containing3The suspension of (4);
12) dropwise adding Na into the suspension under the condition of vigorous stirring2The S solution is continuously stirred vigorously for 5 hours to obtain the LaFeO-containing solution3In (2) of2S3Precursor solution;
s3, preparing LaFeO3/In2S3The composite material comprises the following components: containing LaFeO3In (2) of2S3Transferring the precursor solution into a 100ml polytetrafluoroethylene reaction kettle, reacting for 12h at the temperature of 180 ℃, alternately centrifuging and washing the obtained compound for three times by using ethanol and deionized water, and drying for 12h in a vacuum drying oven at the temperature of 50 ℃ to obtain LaFeO3And In2S3The weight portion ratio of the LaFeO to the LaFeO is 4:13/In2S3A composite material.
The technical principles of the present invention have been described above in connection with specific embodiments. The description is made for the purpose of illustrating the principles of the invention and should not be construed in any way as limiting the scope of the invention. Based on the explanations herein, those skilled in the art will be able to conceive of other embodiments of the present invention without any inventive step, which shall fall within the scope of the present invention.
Claims (10)
1. LaFeO3/In2S3The preparation method of the composite material is characterized by comprising the following steps:
s1, preparing LaFeO3Nano-microspheres;
s2, preparing LaFeO-containing3In (2) of2S3Precursor solution: LaFeO is added3The nano-microspheres are dispersed in InCl3In the solution to obtain LaFeO-containing3The suspension of (1) is added with Na dropwise under the condition of vigorous stirring2S solution to obtain LaFeO-containing solution3In (2) of2S3Precursor solution;
s3, preparing LaFeO3/In2S3The composite material comprises the following components: containing LaFeO3In (2) of2S3The precursor solution is subjected to hydrothermal reaction in a polytetrafluoroethylene reaction kettle to obtain LaFeO3/In2S3A composite material.
2. LaFeO according to claim 13/In2S3The preparation method of the composite material is characterized in that LaFeO in the step S23And In2S3The weight ratio of the components is 1-8: 1.
3. LaFeO according to claim 13/In2S3The preparation method of the composite material is characterized in that the step S1 comprises the following steps:
adding ferric nitrate, lanthanum nitrate and citric acid into the aqueous solution, stirring and dissolving, transferring into a polytetrafluoroethylene reaction kettle, putting into a constant-temperature drying oven, and reacting for 12h at the temperature of 180 ℃ to obtain LaFeO3The product is then annealed and ground at high temperature to obtain LaFeO3And (4) nano microspheres.
4. LaFeO according to claim 23/In2S3The preparation method of the composite material is characterized in that the LaFeO3The particle size of the nano-microspheres is 2.5-4 mu m, and the In2S3The particle size of (A) is 100 to 720 nm.
5. LaFeO according to claim 13/In2S3Composite materialThe preparation method of the material is characterized in that the high-temperature annealing in the step S1 is annealing for 4 hours under the temperature condition of 800 ℃.
6. LaFeO according to claim 13/In2S3The preparation method of the composite material is characterized in that the reaction temperature of the hydrothermal reaction in the step S3 is 180 ℃, and the reaction time is 12 h.
7. LaFeO according to any of claims 1 to 63/In2S3A method for producing a composite material, characterized in that Na is dropwise added in step S22And (5) continuing stirring and reacting for 5 hours after the solution S, wherein the stirring speed of the violent stirring is 800-1000 rpm.
8. LaFeO according to any one of claims 1 to 63/In2S3The use of composite materials in photocatalysis.
9. LaFeO according to any one of claims 1 to 63/In2S3The application of the composite material in photocatalytic degradation of organic pollutants.
10. The use according to claim 9, wherein the organic contaminant is rhodamine B and the photocatalytic degradation is carried out under visible light.
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| CN116586081A (en) * | 2023-03-24 | 2023-08-15 | 清华大学深圳国际研究生院 | LaFeO 3 Base heterojunction composite photocatalysis nano material, preparation method and application |
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