CN114160165A - High-entropy alloy/NiIn2S4Preparation method of composite photocatalyst - Google Patents
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Abstract
本发明公开了一种高熵合金/NiIn2S4复合光催化剂制备方法，包括以下步骤：S1、称取包括5种金属离子的金属源、表面活性剂、还原剂，加入到溶剂A中，充分搅拌溶解，形成高熵合金前驱体溶液；S2、采用超声辅助法，对上述高熵合金前驱体溶液进行超声还原，得到高熵合金；S3、称取镍盐、铟盐、硫源，加入到溶剂B中，充分搅拌溶解，形成NiIn2S4的前驱体溶液；S4、在上述NiIn2S4的前驱体溶液中加入高熵合金，在高压反应釜中反应，反应结束后清洗干燥，得到NiIn2S4/高熵合金复合物。本发明相较于现有技术，合成过程简单，易于批量制备，所得复合材料具有Z‑型异质结结构，提高了光生载流子的分离效率，对污水中多种抗生素和有机污染物具有较高的催化效率。The invention discloses a preparation method of high-entropy alloy/NiIn 2 S 4 composite photocatalyst. Fully stirring and dissolving to form a high-entropy alloy precursor solution; S2, ultrasonically reducing the above-mentioned high-entropy alloy precursor solution by an ultrasonic-assisted method to obtain a high-entropy alloy; S3, weighing nickel salt, indium salt, and sulfur source, adding into the solvent B, fully stirring and dissolving to form a precursor solution of NiIn 2 S 4 ; S4, adding a high-entropy alloy to the precursor solution of the above-mentioned NiIn 2 S 4 , reacting in an autoclave, washing and drying after the reaction is completed, A NiIn 2 S 4 /HEA composite was obtained. Compared with the prior art, the invention has the advantages of simple synthesis process, easy batch preparation, and the obtained composite material has a Z-type heterojunction structure, which improves the separation efficiency of photogenerated carriers, and has good effects on various antibiotics and organic pollutants in sewage. higher catalytic efficiency.
Description
Technical Field
The invention belongs to the technical field of photocatalytic materials, and particularly relates to a high-entropy alloy/NiIn for photodegradation of water antibiotics and organic pollutants2S4A preparation method of a composite photocatalyst.
Background
With the rapid development of society, organic dyes and antibiotics cause serious water and soil pollution, seriously threaten the health of human bodies, animals and plants, effectively treat the pollution of the organic pollutants and the antibiotics and protect the living environment of human beings, and is a long-term important problem to be solved. Under the carbon neutralization background, the solar photocatalytic degradation technology is considered to be a key green and environment-friendly means for solving the major problem. So far, expert scholars have explored various semiconductor materials, including metal oxides, sulfides, oxyhalides, oxynitrides, organometallic framework materials, etc., for photocatalytic degradation. Of all the reported photocatalysts, metal sulfides are considered to be good candidates for photocatalysis due to their strong absorption in the visible region. Sulfur spinel (A), an important ternary transition metal sulfideIIBIII 2SVI 4E.g. ZnIn2S4、CoIn2S4、NiIn2S4、FeIn2S4Etc.) have shown the feasibility of photocatalysis and in lightPotential applications in electronics, light modulators and photodetectors. Wherein, NiIn2S4Has narrow band gap and excellent photocatalytic activity, and has wide application in the field of solar cells.
Ag. The reason why nano ions such as Au have remarkable photocatalytic activity is that: 1) the electron conduction of the metal nano-particles can obtain irradiation energy, so that high-energy electrons are generated on the surfaces of the metal nano-particles, and the organic pollutant molecules adsorbed on the surfaces of the metal nano-particles are activated to be oxidized. 2) The metal nanoparticles have better affinity for organic contaminant molecules than semiconductors; 3) the electron density of the surface of the metal nano particle is far higher than that of a semiconductor, so that the reaction of organic pollutant molecules on the surface of the metal nano particle is enhanced. Common Au and Ag nanoparticles are often used as a cocatalyst for photocatalysis. The high-entropy alloy containing various metal elements has the advantages of excellent catalytic activity, high strength, good corrosion resistance and the like due to coordination, geometric effect and the like.
Xia et al (In situ growth NiIn)2S4nanosheets as counter electrode for bipolar-state-induced solar cells) by hydrothermal growth method2S4Interconnected network-shaped nanosheets for use in solar cells.
Fu et al (Superior Oxygen Electrocatalysis on Nickel Indium sulfide for Rechargeable Zn-Air Batteries) hydrothermally grow Niln with carbon nano-fiber as carrier2S4The nano sheet shows better catalytic activity in a Zn-Air battery.
The invention patent CN 113181922A adopts high-entropy CoMgNiZnCuOxThe Ag quantum dots are deposited and loaded on the surface of the carrier, so that the efficiency of photodegrading dye wastewater is improved.
Invention patent CN 111573775A adopts AIxEyFezNiuGvThe dye (rhodamine B) is degraded by photochemical-electrochemical bonding as an electrode.
Wang et al (Development of a novel (Ni)40Fe30Co20Al10)90Ti10high-entropy alloy with excellent (Ni) is prepared by high-energy ball milling-high-temperature calcination40Fe30Co20Al10)90Ti10The high-entropy alloy has the advantages that the interface between different phases promotes electron transfer and generates lattice distortion, so that the high-entropy alloy has high-efficiency degradation performance on methyl blue in visible light.
Liu and the like use activated carbon as a carrier, synthesize a high-entropy CoCrFeMnNi/C composite material through impregnation, adsorption and calcination, and show excellent catalytic performance on the degradation of methylene blue without adding any peroxide.
No use of NiIn in the prior art2S4The high-entropy alloy composite photocatalytic material is used for photodegrading antibiotics, and the separation efficiency of a photon-generated carrier of the existing photocatalytic material is low.
Disclosure of Invention
The invention aims to: provides a high-entropy alloy/NiIn2S4A preparation method of a composite photocatalyst.
In order to achieve the purpose, the invention adopts the following technical scheme: high-entropy alloy/NiIn2S4The preparation method of the composite photocatalyst comprises the following steps:
s1, weighing a metal source comprising 5 metal ions, a surfactant and a reducing agent, adding the metal source, the surfactant and the reducing agent into the solvent A, and fully stirring and dissolving to form a high-entropy alloy precursor solution;
s2, carrying out ultrasonic reduction on the high-entropy alloy precursor solution by adopting an ultrasonic auxiliary method under the ultrasonic power of 300-1500W, wherein the ultrasonic time is 5-60min, and the temperature is 20-60 ℃, so as to obtain the high-entropy alloy;
s3, weighing nickel salt, indium salt and sulfur source, adding into solvent B, wherein the molar ratio of nickel salt, indium salt and sulfur source is 1: 2: 4, fully stirring and dissolving to form NiIn2S4The precursor solution of (1);
s4, in the NiIn2S4Adding high-entropy alloy into the precursor solution, reacting for 6-48h in a high-pressure reaction kettle at the temperature of 160-220 ℃, and cleaning and drying after the reaction is finished to obtain NiIn2S4High-entropy alloy composite。
As a further description of the above technical solution:
in step S1, the metal sources are five of hydrochloride, nitrate, sulfate and acetate of Co, Fe, Ni, Cu, Mn, Cr, Au, Ag, Pt, Pd, Ir and Rh, the molar ratio of 5 metal ions is 1: 1, and the molar concentration of the total metal ions is 1-1000 mmol/L.
As a further description of the above technical solution:
in step S1, the surfactant is one or two of CTAB, PVP, SDS, P123, F127.
As a further description of the above technical solution:
in step S1, the reducing agent is one of ethylene glycol, ethylenediamine, ascorbic acid, sodium borohydride, and triethylamine.
As a further description of the above technical solution:
in step S1, the solvent a is one or two of water, ethanol, ethylene glycol, glycerol, and isopropanol.
As a further description of the above technical solution:
in step S3, the nickel salt is one of hydrochloride, sulfate, nitrate, oxalate, and acetate of nickel.
As a further description of the above technical solution:
in step S3, the indium salt is one of hydrochloride, nitrate, sulfate, and acetate of indium.
As a further description of the above technical solution:
in step S3, the sulfur source is one of thiourea, thioacetamide, sodium sulfide, ethylenediamine, thiosemicarbazide, sodium thiosulfate, ammonium thiosulfate, thioacetic acid, dithioacetamide, and dithiobiuret.
As a further description of the above technical solution:
in step S3, the solvent B is one or two of water, ethanol, ethylene glycol, N-dimethylformamide, and N, N-dimethylacetamide, and the mass ratio of the nickel salt to the solvent B is 1: 50-200.
As a further description of the above technical solution:
in step S4, the high-entropy alloy and NiIn2S4The theoretical mass ratio of (A) is 10: 1-1: 10.
In summary, due to the adoption of the technical scheme, the invention has the beneficial effects that:
1. in the invention, the high-entropy alloy with narrow particle size range and uniform size can be prepared by adopting the acoustic cavitation effect of ultrasonic irradiation, and the method has the advantages of high synthesis speed, easiness in mass production and the like;
2. in the invention, the high-entropy alloy has the advantages of good visible light transmission, strong light absorption capacity, good heat resistance, corrosion resistance and the like, and the surface effect and the quantum effect of the high-entropy alloy improve the catalytic activity of the composite material;
3. in the invention, NiIn is coated or grown on the surface of the high-entropy alloy by hydrothermal synthesis2S4The nano material and the nano material can form a compact Z-type heterojunction structure between the two, which is beneficial to the separation of photon-generated carriers and improves the photocatalytic activity.
Detailed Description
The above description is only for the preferred embodiment of the present invention, but the scope of the present invention is not limited thereto, and any person skilled in the art should be considered to be within the technical scope of the present invention, and the technical solutions and the inventive concepts thereof according to the present invention should be equivalent or changed within the scope of the present invention.
Example one
S1, respectively weighing precursors of silver chloride, cobalt chloride, nickel chloride, copper chloride and palladium chloride according to the molar ratio of Ag to Co, Ni, Cu and Pd of 1: 1, dissolving the precursors in ethylene glycol (the molar concentration of total metal ions is 5mmol/L), adding a surfactant CTAB, and fully stirring and dissolving to obtain a high-entropy alloy precursor solution;
s2, carrying out ultrasonic reduction on the solution in a cell crusher at the room temperature and the power of 750W for 30 minutes, and cleaning and drying to obtain the high-entropy AgCoNiCuPd alloy;
s3, weighing 1.0mmol of nickel chloride hexahydrate, 2.0mmol of indium trichloride and 8.0mmol of thiourea, adding the nickel chloride hexahydrate, the indium trichloride and the thiourea into 70ml of mixed solvent of N, N-dimethylformamide and ethylene glycol (volume ratio is 1: 1), and fully stirring and dissolving to form NiIn2S4The precursor solution of (1);
s4, transferring the solution into a high-pressure reaction kettle, adding 0.1g of high-entropy AgCoNiCuPd alloy, carrying out hydrothermal reaction at 180 ℃ for 12h, cleaning and drying to obtain NiIn2S4the/AgCoNiCuPd composite material.
For the prepared NiIn2S4And carrying out a photodegradability test on the/AgCoNiCuPd composite material.
Example two
S1, respectively weighing precursors of silver nitrate, cobalt nitrate, nickel nitrate, copper nitrate and palladium nitrate according to the molar ratio of Ag to Co, Ni, Cu and Pd of 1: 1, dissolving the precursors in ethylene glycol (the molar concentration of total metal ions is 5mmol/L), adding a surfactant SDS, and fully stirring and dissolving to obtain a high-entropy alloy precursor solution;
s2, carrying out ultrasonic reduction on the solution in a cell crusher at the power of 800W and room temperature for 40 minutes, and cleaning and drying to obtain the high-entropy AgCoNiCuPd alloy;
s3, weighing 1.0mmol of nickel chloride hexahydrate, 2.0mmol of indium trichloride and 8.0mmol of thiourea, adding the nickel chloride hexahydrate, the indium trichloride and the thiourea into 70ml of mixed solvent of N, N-dimethylformamide and ethylene glycol (volume ratio is 1: 1), and fully stirring and dissolving to form NiIn2S4The precursor solution of (1);
s4, transferring the solution into a high-pressure reaction kettle, adding 0.1g of high-entropy AgCoNiCuPd alloy, carrying out hydrothermal reaction at 180 ℃ for 12h, cleaning and drying to obtain NiIn2S4the/AgCoNiCuPd composite material.
For the prepared NiIn2S4And carrying out a photodegradability test on the/AgCoNiCuPd composite material.
EXAMPLE III
S1, respectively weighing precursors of cobalt chloride, chromium chloride, ferric chloride, manganese chloride and nickel chloride according to the molar ratio of Co to Cr, Fe, Mn and Ni of 1: 1, dissolving the precursors in ethylene glycol (the molar concentration of total metal ions is 5mmol/L), adding a surfactant CTAB, and fully stirring and dissolving to obtain a high-entropy alloy precursor solution;
s2, carrying out ultrasonic reduction on the solution in a cell crusher at the power of 750W and room temperature for 30 minutes, and cleaning and drying to obtain a high-entropy CoCrFeMnNi alloy;
s3, weighing 1.0mmol of nickel chloride hexahydrate, 2.0mmol of indium trichloride and 8.0mmol of thiourea, adding the nickel chloride hexahydrate, the indium trichloride and the thiourea into 70ml of mixed solvent of N, N-dimethylformamide and ethylene glycol (volume ratio is 1: 1), and fully stirring and dissolving to form NiIn2S4The precursor solution of (1);
s4, transferring the solution into a high-pressure reaction kettle, adding 0.1g of high-entropy CoCrFeMnNi alloy, carrying out hydrothermal reaction at 180 ℃ for 12h, cleaning and drying to obtain NiIn2S4a/CoCrFeMnNi composite material.
For the prepared NiIn2S4the/CoCrFeMnNi composite material is subjected to a photodegradability test.
And (3) testing the photodegradability: the synthesized composite material is added into sewage containing organic dye, the adding amount of the catalyst is 0.1-1g/L, a 300W xenon lamp is used as a light source, an optical filter is used for filtering out the ultraviolet part, and the used light source is visible light with the wavelength of more than 420 nm. When the catalyst is used, the concentration of the catalyst can be adjusted according to specific conditions.
The initial concentration of the organic dye is 5-50 mg/L.
After the reaction is finished, the calculation method of the degradation rate comprises the following steps:
the degradation rate is [ (C)0-Ct)/C0]*100％
Wherein, C0Is the initial concentration of organic dye, CtThe organic dye concentration measured after the reaction is in mg/L.
| Degradation rate of methylene blue after 1h of illumination | |
| Example 1 | 99.1％ |
| Example 2 | 98.9％ |
| Example 3 | 99.5％ |
| COMPARATIVE EXAMPLE 1 (not added to the Sewage) | 56.3％ |
| Comparative example 2 | 43.8％ |
Note: the photodegradability test performed in comparative example 1 was the same as the photodegradability test performed in example 1 except that no synthetic composite material was added to the wastewater.
The photodegradability test performed in comparative example 2 was the same as the photodegradability test performed in example 2 except that no synthetic composite material was added to the wastewater.
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| CN115518659A (en) * | 2022-11-02 | 2022-12-27 | 江苏大学 | A preparation method of SnIn4S8 photocatalyst loaded with copper-gold alloy |
| CN116139894A (en) * | 2023-02-10 | 2023-05-23 | 中山大学 | Preparation of palladium-based high-entropy compound nano material and application of palladium-based high-entropy compound nano material in electrocatalytic and photocatalytic fields |
| CN116474784A (en) * | 2023-04-07 | 2023-07-25 | 重庆三峡学院 | A kind of preparation method of aluminate/high entropy alloy composite photocatalyst |
| CN116832848A (en) * | 2023-07-07 | 2023-10-03 | 山东理工大学 | Preparation method of a medium-entropy alloy/Bi3O4Br/CNNs composite photocatalyst |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN115518659A (en) * | 2022-11-02 | 2022-12-27 | 江苏大学 | A preparation method of SnIn4S8 photocatalyst loaded with copper-gold alloy |
| CN116139894A (en) * | 2023-02-10 | 2023-05-23 | 中山大学 | Preparation of palladium-based high-entropy compound nano material and application of palladium-based high-entropy compound nano material in electrocatalytic and photocatalytic fields |
| CN116139894B (en) * | 2023-02-10 | 2024-06-04 | 中山大学 | Preparation of palladium-based high-entropy compound nano material and application of palladium-based high-entropy compound nano material in electrocatalytic and photocatalytic fields |
| CN116474784A (en) * | 2023-04-07 | 2023-07-25 | 重庆三峡学院 | A kind of preparation method of aluminate/high entropy alloy composite photocatalyst |
| CN116474784B (en) * | 2023-04-07 | 2025-04-04 | 重庆三峡学院 | A method for preparing aluminate/high entropy alloy composite photocatalyst |
| CN116832848A (en) * | 2023-07-07 | 2023-10-03 | 山东理工大学 | Preparation method of a medium-entropy alloy/Bi3O4Br/CNNs composite photocatalyst |
| CN116832848B (en) * | 2023-07-07 | 2025-06-24 | 山东理工大学 | Preparation method of medium-entropy alloy/Bi3O4Br/CNNs composite photocatalyst |
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