CN110624543A - PtRu-SnNb2O6Preparation method of two-dimensional composite material - Google Patents
PtRu-SnNb2O6Preparation method of two-dimensional composite material Download PDFInfo
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- 239000002131 composite material Substances 0.000 title claims abstract description 21
- 238000000034 method Methods 0.000 title abstract description 12
- 238000006243 chemical reaction Methods 0.000 claims abstract description 41
- 239000002135 nanosheet Substances 0.000 claims abstract description 32
- 239000000463 material Substances 0.000 claims abstract description 22
- 238000002360 preparation method Methods 0.000 claims abstract description 21
- 238000001027 hydrothermal synthesis Methods 0.000 claims abstract description 14
- 239000000243 solution Substances 0.000 claims description 72
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 36
- 239000008367 deionised water Substances 0.000 claims description 30
- 229910021641 deionized water Inorganic materials 0.000 claims description 30
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 30
- 239000011259 mixed solution Substances 0.000 claims description 29
- 238000004321 preservation Methods 0.000 claims description 22
- 229910019891 RuCl3 Inorganic materials 0.000 claims description 21
- 238000003756 stirring Methods 0.000 claims description 20
- ZKATWMILCYLAPD-UHFFFAOYSA-N niobium pentoxide Inorganic materials O=[Nb](=O)O[Nb](=O)=O ZKATWMILCYLAPD-UHFFFAOYSA-N 0.000 claims description 19
- 229910002621 H2PtCl6 Inorganic materials 0.000 claims description 14
- 238000001035 drying Methods 0.000 claims description 14
- 239000007864 aqueous solution Substances 0.000 claims description 12
- 238000003760 magnetic stirring Methods 0.000 claims description 12
- 239000010935 stainless steel Substances 0.000 claims description 12
- 229910001220 stainless steel Inorganic materials 0.000 claims description 12
- 238000005303 weighing Methods 0.000 claims description 8
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 6
- 229910021626 Tin(II) chloride Inorganic materials 0.000 claims description 6
- 239000012295 chemical reaction liquid Substances 0.000 claims description 6
- 238000013329 compounding Methods 0.000 claims description 6
- 238000001914 filtration Methods 0.000 claims description 6
- XLYOFNOQVPJJNP-ZSJDYOACSA-N heavy water Substances [2H]O[2H] XLYOFNOQVPJJNP-ZSJDYOACSA-N 0.000 claims description 6
- 230000001678 irradiating effect Effects 0.000 claims description 6
- 239000007788 liquid Substances 0.000 claims description 6
- 239000002243 precursor Substances 0.000 claims description 6
- 239000006228 supernatant Substances 0.000 claims description 6
- AXZWODMDQAVCJE-UHFFFAOYSA-L tin(II) chloride (anhydrous) Chemical compound [Cl-].[Cl-].[Sn+2] AXZWODMDQAVCJE-UHFFFAOYSA-L 0.000 claims description 6
- 238000005406 washing Methods 0.000 claims description 6
- 229910052724 xenon Inorganic materials 0.000 claims description 6
- FHNFHKCVQCLJFQ-UHFFFAOYSA-N xenon atom Chemical compound [Xe] FHNFHKCVQCLJFQ-UHFFFAOYSA-N 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 2
- YBCAZPLXEGKKFM-UHFFFAOYSA-K ruthenium(iii) chloride Chemical compound [Cl-].[Cl-].[Cl-].[Ru+3] YBCAZPLXEGKKFM-UHFFFAOYSA-K 0.000 claims description 2
- 150000001875 compounds Chemical class 0.000 claims 1
- 230000001699 photocatalysis Effects 0.000 abstract description 16
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 7
- ATJFFYVFTNAWJD-UHFFFAOYSA-N Tin Chemical compound [Sn] ATJFFYVFTNAWJD-UHFFFAOYSA-N 0.000 abstract description 6
- 229910002056 binary alloy Inorganic materials 0.000 abstract description 5
- 230000015556 catabolic process Effects 0.000 abstract description 3
- 238000006731 degradation reaction Methods 0.000 abstract description 3
- 238000000151 deposition Methods 0.000 abstract description 2
- 238000011065 in-situ storage Methods 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 abstract description 2
- 238000007540 photo-reduction reaction Methods 0.000 abstract description 2
- PYWVYCXTNDRMGF-UHFFFAOYSA-N rhodamine B Chemical compound [Cl-].C=12C=CC(=[N+](CC)CC)C=C2OC2=CC(N(CC)CC)=CC=C2C=1C1=CC=CC=C1C(O)=O PYWVYCXTNDRMGF-UHFFFAOYSA-N 0.000 abstract description 2
- 229940043267 rhodamine b Drugs 0.000 abstract description 2
- 238000012360 testing method Methods 0.000 abstract description 2
- 239000002351 wastewater Substances 0.000 abstract description 2
- 239000004065 semiconductor Substances 0.000 description 10
- 239000011941 photocatalyst Substances 0.000 description 6
- 229910000510 noble metal Inorganic materials 0.000 description 4
- 238000005215 recombination Methods 0.000 description 3
- 238000000926 separation method Methods 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 238000001816 cooling Methods 0.000 description 2
- 238000005516 engineering process Methods 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000002082 metal nanoparticle Substances 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 239000002086 nanomaterial Substances 0.000 description 2
- 238000013032 photocatalytic reaction Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- 238000001179 sorption measurement Methods 0.000 description 2
- RBTBFTRPCNLSDE-UHFFFAOYSA-N 3,7-bis(dimethylamino)phenothiazin-5-ium Chemical compound C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 RBTBFTRPCNLSDE-UHFFFAOYSA-N 0.000 description 1
- 241000282414 Homo sapiens Species 0.000 description 1
- 229910002849 PtRu Inorganic materials 0.000 description 1
- 230000009471 action Effects 0.000 description 1
- 230000004888 barrier function Effects 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 239000003054 catalyst Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000010276 construction Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000004925 denaturation Methods 0.000 description 1
- 230000036425 denaturation Effects 0.000 description 1
- 238000011161 development Methods 0.000 description 1
- 230000018109 developmental process Effects 0.000 description 1
- 230000005672 electromagnetic field Effects 0.000 description 1
- 238000010893 electron trap Methods 0.000 description 1
- 229910052737 gold Inorganic materials 0.000 description 1
- 230000006872 improvement Effects 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000007246 mechanism Effects 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229960000907 methylthioninium chloride Drugs 0.000 description 1
- 239000002114 nanocomposite Substances 0.000 description 1
- 229910052763 palladium Inorganic materials 0.000 description 1
- 238000007146 photocatalysis Methods 0.000 description 1
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 1
- 229910052697 platinum Inorganic materials 0.000 description 1
- 239000000047 product Substances 0.000 description 1
- 230000006798 recombination Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000006722 reduction reaction Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 238000002198 surface plasmon resonance spectroscopy Methods 0.000 description 1
- 230000005737 synergistic response Effects 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- 238000003911 water pollution Methods 0.000 description 1
Classifications
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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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/002—Mixed oxides other than spinels, e.g. perovskite
-
- 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
- B01J23/00—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00
- B01J23/38—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals
- B01J23/54—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of noble metals combined with metals, oxides or hydroxides provided for in groups B01J23/02 - B01J23/36
- B01J23/56—Platinum group metals
- B01J23/64—Platinum group metals with arsenic, antimony, bismuth, vanadium, niobium, tantalum, polonium, chromium, molybdenum, tungsten, manganese, technetium or rhenium
- B01J23/648—Vanadium, niobium or tantalum or polonium
- B01J23/6484—Niobium
-
- B01J35/23—
-
- B01J35/39—
-
- 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
-
- 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
- C02F2101/308—Dyes; Colorants; Fluorescent agents
-
- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/10—Photocatalysts
Abstract
The invention discloses a PtRu-SnNb2O6A preparation method of a two-dimensional composite material. Firstly preparing a tin niobate nanosheet in a hydrothermal reaction kettle, and then depositing binary alloy nanoparticles on the tin niobate nanosheet in situ by a photoreduction method to finally obtain the PtRu-SnNb2O6A two-dimensional composite photocatalytic material. The preparation method is simple, easy to operate, mild in reaction condition, easy to control and practical. The prepared two-dimensional composite photocatalytic material can efficiently degrade organic pollutants in wastewater, and tests prove that the degradation rate of the material to rhodamine B organic pollutants is higher than that of single Ru-SnNb2O6The nano sheet is improved by 157%.
Description
Technical Field
The invention belongs to the technical field of material preparation, and particularly relates to PtRu-SnNb2O6A preparation method of a two-dimensional composite material.
Background
As the world's economy has developed rapidly, the negative product water pollution and energy problems have become more severe, and how to treat large quantities of pollutants and how to reduce the production of pollutants has become a major issue for human beings. Therefore, people are in short of a low-pollution or even pollution-free method for purifying the environment. Among the solutions, the photocatalytic technology implemented by using semiconductor materials directly converts solar energy into utilizable chemical energy without generating pollution, which is considered as one of the most ideal methods for treating organic pollutants. Semiconductor photocatalytic technology has been developed to date, and researches and developments on novel photocatalytic materials are the key direction of researchers, with the continuous emphasis on improving photocatalytic efficiency after deeply understanding the principle of semiconductor material photocatalytic reaction.
SnNb2O6Is a novel semiconductor photocatalytic material and has great potential in the field of photocatalysis. SnNb like nano sheet2O6The specific surface area of (A) is large, and the number of unsaturated bonds at the edge is large. These provide a large number of adsorption sites as well as active sites for it. But SnNb2O6The defects of (2) are obvious, the surface area is small, and the self-recombination rate of photogenerated electron holes is high.To compensate for the disadvantages, it is common practice to incorporate materials such as semiconductors or noble metals into the heterojunction, such as Pt/SnNb2O6And CdS/SnNb2O6Etc. are such heterojunctions.
The construction of noble metal-semiconductor composite photocatalysts is considered to be an effective way to increase the photocatalytic activity of semiconductors due to the improvement of visible light adsorption, charge separation and/or redox kinetics. Especially, the Local Surface Plasmon Resonance (LSPR) of metal nano particles such as Pt, Au, Pd and the like can obviously improve the photocatalytic performance of the semiconductor. Due to the localized electromagnetic field enhanced by LSPR or the thermal plasma electrons excited by LSPR, charge can be induced near the metal-semiconductor interface, forming carriers. When a noble metal is in direct contact with an adjacent semiconductor, a schottky barrier is formed, with the result that electron flow of a material with a high fermi level to a lower level causes alignment of the fermi level. The deposited noble metal can be used as an electron trap to assist electron-hole separation, so that charge separation can be effectively forced, and the recombination of electrons and holes is reduced.
Thus, build Metal/SnNb2O6The nano composite material photocatalytic material is an effective method for improving the catalytic efficiency of a photocatalyst. Nano SnNb2O6The photocatalyst has the characteristics of ultrathin property, large specific surface area and strong electron reduction capability, inhibits the self-recombination of photoproduction electrons and photoproduction holes after the metal nano particles are loaded, and further improves the photocatalytic performance of the photocatalyst.
Compared with the tin niobate photocatalyst deposited by single noble metal, the binary alloy supported tin niobate photocatalyst can further improve the photocatalytic activity.
Disclosure of Invention
The invention aims to provide a method for improving the removal rate of organic pollutants, aiming at solving the problems of the prior art; the method is simple, easy to operate, safe and reliable and is PtRu-SnNb2O6A preparation method of a two-dimensional composite material.
The technical scheme for realizing the purpose of the invention is as follows: PtRu-SnNb2O6A method for preparing a two-dimensional composite material, characterized in thatThe method comprises the following steps:
step 1: preparation of SnNb2O6Two-dimensional nanosheet
(1.1) preparing a precursor aqueous solution: mixing 1-5g Nb2O5And 5-20g of KOH are dissolved in 100-200mL of deionized water to obtain a mixed solution, the mixed solution is magnetically stirred for 30 minutes, then the mixed solution is moved into a high-temperature stainless steel reaction kettle for hydrothermal reaction at the temperature of 160-180 ℃, the heat preservation time is 12-48 hours, and the reaction solution is obtained after the reaction and the heat preservation are finished and is cooled to room temperature;
(1.2) dissolving concentrated hydrochloric acid in deionized water to prepare the solution with the concentration of 2 mol. L-1A dilute hydrochloric acid solution of (a); dropwise adding the prepared dilute hydrochloric acid solution into the reaction liquid obtained in the step (1.1), and adjusting the pH value to 7 to obtain Nb2O5·nH2An aqueous solution of O;
(1.3) weighing 1-3g SnCl2·2H2O addition to Nb prepared in step (1.2)2O5·nH2In the O solution, under the magnetic stirring, 2mol/L hydrochloric acid solution is used for adjusting the pH value of the solution to 1.0-3.0, after the magnetic stirring is carried out for 30-60min, the uniformly stirred mixed solution is transferred into a 50ml high-temperature stainless steel reaction kettle for hydrothermal reaction, and after the reaction heat preservation is finished, the mixed solution is naturally cooled to room temperature, the reaction temperature is 180-200 ℃, and the heat preservation time is 24-48 h; removing supernatant, washing with deionized water and anhydrous ethanol, filtering, and drying at 80 deg.C for 8 hr to obtain SnNb2O6Nanosheets;
step 2: preparation of PtRu-SnNb2O6Two-dimensional composite material
(2.1) configuration H2PtCl6And RuCl3Solution: a certain amount of H2PtCl6And RuCl3Dissolving in deionized water to prepare a solution of H2PtCl6 with the molar concentration of 1mM and RuCl3 with the molar concentration of 1 mM;
(2.2) weighing 0.1-0.2g of SnNb prepared in the step (1.3)2O6Placing the nano-sheets in a 100ml beaker, adding 50ml of deionized water, stirring for 30min, and then adding a certain amount of H prepared in the step (2.1)2PtCl6And RuCl3Continuously stirring the solution for 30 min; irradiating with 300W xenon lamp for 30min, and stirring; then the mixed liquid is centrifugally dried to obtain PtRu-SnNb2O6And (3) compounding the nanosheet material.
Further, the H configured in the step (2.1) added in the step (2.2)2PtCl6The amount of the solution is 0.5-5ml, RuCl3The amount of the solution is 0.5-5 ml.
The action mechanism of the invention is as follows: using SnNb2O6The nano-sheet is thin, the carrier transmission rate is high, and the electronic transmission capacity is good. The catalyst has larger specific surface area and more active sites, and can perform high-efficiency photocatalytic reaction. The binary alloy structure is changed to generate a synergistic response, so that the driving force of the directional transfer of the photo-generated charges has adjustable denaturation. Thus, the binary alloy PtRu is photo-deposited onto SnNb2O6In addition, the efficiency of photocatalytic degradation of organic pollutants can be further improved.
Compared with the prior art, the invention has the beneficial effects that:
1. obtained PtRu-SnNb2O6After the two-dimensional nano material is tested by the degraded methylene blue, the degradation rate is 157 percent higher.
2. The PtRu-SnNb prepared by the invention2O6The method for preparing the two-dimensional nano material is simple and easy to operate, has practical feasibility, and the prepared PtRu-SnNb2O6The photocatalytic material has low cost and no pollution.
Drawings
FIG. 1 shows PtRu-SnNb of the present invention2O6Scanning electron micrographs of the composite.
Detailed Description
In order to better understand the present invention, the following examples are further provided to illustrate the present invention, but the present invention is not limited to the following examples. Various changes or modifications may be effected therein by one skilled in the art and such equivalents are intended to be within the scope of the invention as defined by the claims appended hereto.
Example 1
Step 1: preparation of SnNb2O6Two-dimensional nanosheet
(1.1) preparing a precursor aqueous solution: 2.5g of Nb2O5And 11.2g of KOH is dissolved in 100-200mL deionized water to obtain a mixed solution, the mixed solution is magnetically stirred for 30 minutes, then the mixed solution is moved into a high-temperature stainless steel reaction kettle for hydrothermal reaction at the temperature of 160-180 ℃, the heat preservation time is 12-48 hours, and the reaction solution is obtained after the reaction and the heat preservation are finished and is cooled to room temperature.
(1.2) dissolving concentrated hydrochloric acid in deionized water to prepare the solution with the concentration of 2 mol. L-1A dilute hydrochloric acid solution of (a); dropwise adding the prepared dilute hydrochloric acid solution into the reaction liquid obtained in the step (1.1), and adjusting the pH value to 7 to obtain Nb2O5·nH2And (4) O aqueous solution.
(1.3) weighing 2.1g SnCl2·2H2O addition to Nb prepared in step (1.2)2O5·nH2In the O solution, under the magnetic stirring, 2mol/L hydrochloric acid solution is used for adjusting the pH value of the solution to 2.0, after the magnetic stirring is carried out for 30min, the uniformly stirred mixed solution is transferred into a 50ml high-temperature stainless steel reaction kettle for hydrothermal reaction, and after the reaction heat preservation is finished, the mixed solution is naturally cooled to room temperature, the reaction temperature is 200 ℃, and the heat preservation time is 48 hours; removing supernatant, washing with deionized water and anhydrous ethanol, filtering, and drying (drying temperature 80 deg.C, drying time 8h) to obtain SnNb2O6Nanosheets.
Step 2: preparation of PtRu-SnNb2O6Two-dimensional composite material
(2.1) configuration H2PtCl6And RuCl3Solution: a certain amount of H2PtCl6And RuCl3Dissolving in deionized water to prepare H with a molar concentration of 1mM2PtCl6And RuCl at a molar concentration of 1mM3And (3) solution.
(2.2) 0.2g of SnNb prepared in step (1.3) was weighed2O6Placing the nano-sheets in a 100ml beaker, adding 50ml of deionized water, stirring for 30min, and then adding 1ml of H prepared in the step (2.1)2PtCl6Solution and 1ml ofRuCl3Continuously stirring the solution for 30 min; irradiating with 300W xenon lamp for 30min, and stirring; then the mixed liquid is centrifugally dried to obtain PtRu-SnNb2O6And (3) compounding the nanosheet material.
Example 2
Step 1: preparation of SnNb2O6Two-dimensional nanosheet
(1.1) preparing a precursor aqueous solution: 2.5g of Nb2O5And 11.2g of KOH is dissolved in 200mL of deionized water to obtain a mixed solution, the mixed solution is magnetically stirred for 30 minutes, then the mixed solution is transferred into a high-temperature stainless steel reaction kettle for hydrothermal reaction, the reaction temperature is 160 ℃, the heat preservation time is 24 hours, and after the reaction heat preservation is finished, the mixed solution is cooled to room temperature to obtain a reaction solution.
(1.2) dissolving concentrated hydrochloric acid in deionized water to prepare the solution with the concentration of 2 mol. L-1A dilute hydrochloric acid solution of (a); dropwise adding the prepared dilute hydrochloric acid solution into the reaction liquid obtained in the step (1.1), and adjusting the pH value to 7 to obtain Nb2O5·nH2And (4) O aqueous solution.
(1.3) weighing 2.1g SnCl2·2H2O addition to Nb prepared in step (1.2)2O5·nH2In the O solution, under the magnetic stirring, 2mol/L hydrochloric acid solution is used for adjusting the pH value of the solution to 2.0, after the magnetic stirring is carried out for 30min, the uniformly stirred mixed solution is transferred into a 50ml high-temperature stainless steel reaction kettle for hydrothermal reaction, and after the reaction heat preservation is finished, the mixed solution is naturally cooled to room temperature, the reaction temperature is 180 ℃, and the heat preservation time is 48 hours; removing supernatant, washing with deionized water and anhydrous ethanol, filtering, and drying (drying temperature 80 deg.C, drying time 8h) to obtain SnNb2O6Nanosheets.
Step 2: preparation of PtRu-SnNb2O6Two-dimensional composite material
(2.1) configuration H2PtCl6And RuCl3Solution: a certain amount of H2PtCl6And RuCl3Dissolving in deionized water to prepare H with a molar concentration of 1mM2PtCl6And RuCl at a molar concentration of 1mM3And (3) solution.
(2.2) 0.2g of SnNb prepared in step (1.3) was weighed2O6Placing the nano-sheets in a 100ml beaker, adding 50ml of deionized water, stirring for 30min, and then adding 0.5ml of H prepared in the step (2.1)2PtCl6Solution and 1ml of RuCl3Continuously stirring the solution for 30 min; irradiating with 300W xenon lamp for 30min, and stirring; then the mixed liquid is centrifugally dried to obtain PtRu-SnNb2O6And (3) compounding the nanosheet material.
Example 3
Step 1: preparation of SnNb2O6Two-dimensional nanosheet
(1.1) preparing a precursor aqueous solution: 2.5g of Nb2O5Dissolving 11.2g of KOH in 100mL of deionized water to obtain a mixed solution, magnetically stirring for 30 minutes, then transferring the mixed solution into a high-temperature stainless steel reaction kettle for hydrothermal reaction at the reaction temperature of 180 ℃ for 48 hours, and cooling to room temperature after the reaction and heat preservation are finished to obtain a reaction solution;
(1.2) dissolving concentrated hydrochloric acid in deionized water to prepare the solution with the concentration of 2 mol. L-1A dilute hydrochloric acid solution of (a); dropwise adding the prepared dilute hydrochloric acid solution into the reaction liquid obtained in the step (1.1), and adjusting the pH value to 7 to obtain Nb2O5·nH2An aqueous solution of O;
(1.3) weighing 2.1g SnCl2·2H2O addition to Nb prepared in step (1.2)2O5·nH2In the O solution, under the magnetic stirring, 2mol/L hydrochloric acid solution is used for adjusting the pH value of the solution to 2.0, after the magnetic stirring is carried out for 30min, the uniformly stirred mixed solution is transferred into a 50ml high-temperature stainless steel reaction kettle for hydrothermal reaction, and after the reaction heat preservation is finished, the mixed solution is naturally cooled to room temperature, the reaction temperature is 200 ℃, and the heat preservation time is 48 hours; removing supernatant, washing with deionized water and anhydrous ethanol, filtering, and drying (drying temperature 80 deg.C, drying time 8h) to obtain SnNb2O6Nanosheets;
step 2: preparation of PtRu-SnNb2O6Two-dimensional composite material
(2.1) configuration H2PtCl6And RuCl3Solution: a certain amount of H2PtCl6And RuCl3Dissolving in deionized water to prepare H with a molar concentration of 1mM2PtCl6And RuCl at a molar concentration of 1mM3And (3) solution.
(2.2) 0.2g of SnNb prepared in step (1.3) was weighed2O6Placing the nano-sheets in a 100ml beaker, adding 50ml of deionized water, stirring for 30min, and then adding 0.5ml of H prepared in the step (2.1)2PtCl6Solution and 0.5ml of RuCl3Continuously stirring the solution for 30 min; irradiating with 300W xenon lamp for 30min, and stirring; then the mixed liquid is centrifugally dried to obtain PtRu-SnNb2O6And (3) compounding the nanosheet material.
Example 4
Step 1: preparation of SnNb2O6Two-dimensional nanosheet
(1.1) preparing a precursor aqueous solution: 2.5g of Nb2O5Dissolving 11.2g of KOH in 100mL of deionized water to obtain a mixed solution, magnetically stirring for 30 minutes, then transferring the mixed solution into a high-temperature stainless steel reaction kettle for hydrothermal reaction at the reaction temperature of 180 ℃ for 24 hours, and cooling to room temperature after the reaction and heat preservation are finished to obtain a reaction solution;
(1.2) dissolving concentrated hydrochloric acid in deionized water to prepare the solution with the concentration of 2 mol. L-1A dilute hydrochloric acid solution of (a); dropwise adding the prepared dilute hydrochloric acid solution into the reaction liquid obtained in the step (1.1), and adjusting the pH value to 7 to obtain Nb2O5·nH2An aqueous solution of O;
(1.3) weighing 2.1g SnCl2·2H2O addition to Nb prepared in step (1.2)2O5·nH2In the O solution, under the magnetic stirring, 2mol/L hydrochloric acid solution is used for adjusting the pH value of the solution to 2.0, after the magnetic stirring is carried out for 30min, the uniformly stirred mixed solution is transferred into a 50ml high-temperature stainless steel reaction kettle for hydrothermal reaction, and after the reaction heat preservation is finished, the mixed solution is naturally cooled to room temperature, the reaction temperature is 200 ℃, and the heat preservation time is 48 hours; removing supernatant, washing with deionized water and anhydrous ethanol, filtering, and drying (drying temperature 80 deg.C)Drying for 8h) to obtain SnNb2O6Nanosheets;
step 2: preparation of PtRu-SnNb2O6Two-dimensional composite material
(2.1) configuration H2PtCl6And RuCl3Solution: a certain amount of H2PtCl6And RuCl3Dissolving in deionized water to prepare H with a molar concentration of 1mM2PtCl6And RuCl at a molar concentration of 1mM3And (3) solution.
(2.2) 0.2g of SnNb prepared in step (1.3) was weighed2O6Placing the nano-sheets in a 100ml beaker, adding 50ml of deionized water, stirring for 30min, and then adding 1ml of H prepared in the step (2.1)2PtCl6Solution and 0.5ml of RuCl3Continuously stirring the solution for 30 min; irradiating with 300W xenon lamp for 30min, and stirring; then the mixed liquid is centrifugally dried to obtain PtRu-SnNb2O6And (3) compounding the nanosheet material.
The invention discloses PtRu-SnNb2O6A preparation method of a two-dimensional composite material. Firstly preparing a tin niobate nanosheet in a hydrothermal reaction kettle, and then depositing binary alloy nanoparticles on the tin niobate nanosheet in situ by a photoreduction method to finally obtain the PtRu-SnNb2O6A two-dimensional composite photocatalytic material. The preparation method is simple, easy to operate, mild in reaction condition, easy to control and practical. The prepared two-dimensional composite photocatalytic material can efficiently degrade organic pollutants in wastewater, and tests prove that the degradation rate of the material to rhodamine B organic pollutants is higher than that of single Ru-SnNb2O6The nano sheet is improved by 157%.
Finally, it should be noted that the above-mentioned contents are only used for illustrating the technical solutions of the present invention, and not for limiting the protection scope of the present invention, and that the simple modifications or equivalent substitutions of the technical solutions of the present invention by those of ordinary skill in the art can be made without departing from the spirit and scope of the technical solutions of the present invention.
Claims (2)
1. PtRu-SnNb2O6The preparation method of the two-dimensional composite material is characterized by comprising the following steps of:
step 1: preparation of SnNb2O6Two-dimensional nanosheet
(1.1) preparing a precursor aqueous solution: mixing 1-5g Nb2O5And 5-20g of KOH are dissolved in 100-200mL of deionized water to obtain a mixed solution, the mixed solution is magnetically stirred for 30 minutes, then the mixed solution is moved into a high-temperature stainless steel reaction kettle for hydrothermal reaction at the temperature of 160-180 ℃, the heat preservation time is 12-48 hours, and the reaction solution is obtained after the reaction and the heat preservation are finished and is cooled to room temperature;
(1.2) dissolving concentrated hydrochloric acid in deionized water to prepare the solution with the concentration of 2 mol. L-1A dilute hydrochloric acid solution of (a); dropwise adding the prepared dilute hydrochloric acid solution into the reaction liquid obtained in the step (1.1), and adjusting the pH value to 7 to obtain Nb2O5·nH2An aqueous solution of O;
(1.3) weighing 1-3g SnCl2·2H2O addition to Nb prepared in step (1.2)2O5·nH2In the O solution, under the magnetic stirring, 2mol/L hydrochloric acid solution is used for adjusting the pH value of the solution to 1.0-3.0, after the magnetic stirring is carried out for 30-60min, the uniformly stirred mixed solution is transferred into a 50ml high-temperature stainless steel reaction kettle for hydrothermal reaction, and after the reaction heat preservation is finished, the mixed solution is naturally cooled to room temperature, the reaction temperature is 180-200 ℃, and the heat preservation time is 24-48 h; removing supernatant, washing with deionized water and anhydrous ethanol, filtering, and drying at 80 deg.C for 8 hr to obtain SnNb2O6Nanosheets;
step 2: preparation of PtRu-SnNb2O6Two-dimensional composite material
(2.1) configuration H2PtCl6And RuCl3Solution: a certain amount of H2PtCl6And RuCl3Dissolving in deionized water to prepare a solution of H2PtCl6 with the molar concentration of 1mM and RuCl3 with the molar concentration of 1 mM;
(2.2) weighing 0.1-0.2g of SnNb prepared in the step (1.3)2O6Placing the nano-sheets in a 100ml beaker, adding 50ml of deionized water, stirring for 30min, and then adding a certain amount of waterH configured in step (2.1)2PtCl6And RuCl3Continuously stirring the solution for 30 min; irradiating with 300W xenon lamp for 30min, and stirring; then the mixed liquid is centrifugally dried to obtain PtRu-SnNb2O6And (3) compounding the nanosheet material.
2. The PtRu-SnNb compound of claim 12O6The preparation method of the two-dimensional composite material is characterized by comprising the following steps: h added in the step (2.2) and configured in the step (2.1)2PtCl6The amount of the solution is 0.5-5ml, RuCl3The amount of the solution is 0.5-5 ml.
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