CN111589457A - Photocatalytic material for in-situ growth of three-dimensional copper sulfide on copper mesh, preparation method and application - Google Patents
Photocatalytic material for in-situ growth of three-dimensional copper sulfide on copper mesh, preparation method and application Download PDFInfo
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- CN111589457A CN111589457A CN202010215886.7A CN202010215886A CN111589457A CN 111589457 A CN111589457 A CN 111589457A CN 202010215886 A CN202010215886 A CN 202010215886A CN 111589457 A CN111589457 A CN 111589457A
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- RYGMFSIKBFXOCR-UHFFFAOYSA-N Copper Chemical compound [Cu] RYGMFSIKBFXOCR-UHFFFAOYSA-N 0.000 title claims abstract description 56
- 229910052802 copper Inorganic materials 0.000 title claims abstract description 56
- 239000010949 copper Substances 0.000 title claims abstract description 56
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 title claims abstract description 28
- 239000000463 material Substances 0.000 title claims abstract description 13
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 13
- 238000011065 in-situ storage Methods 0.000 title claims abstract description 10
- 238000002360 preparation method Methods 0.000 title claims abstract description 10
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 17
- 239000008367 deionised water Substances 0.000 claims abstract description 16
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 16
- XKRFYHLGVUSROY-UHFFFAOYSA-N Argon Chemical compound [Ar] XKRFYHLGVUSROY-UHFFFAOYSA-N 0.000 claims abstract description 14
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims abstract description 12
- 238000007254 oxidation reaction Methods 0.000 claims abstract description 11
- 238000000034 method Methods 0.000 claims abstract description 10
- 239000003792 electrolyte Substances 0.000 claims abstract description 9
- 238000000137 annealing Methods 0.000 claims abstract description 8
- 229910052786 argon Inorganic materials 0.000 claims abstract description 7
- 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 claims abstract description 6
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 claims abstract description 6
- 238000001035 drying Methods 0.000 claims abstract description 6
- 239000007789 gas Substances 0.000 claims abstract description 6
- 229910002804 graphite Inorganic materials 0.000 claims abstract description 6
- 239000010439 graphite Substances 0.000 claims abstract description 6
- 229960000907 methylthioninium chloride Drugs 0.000 claims abstract description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims abstract description 6
- 238000013033 photocatalytic degradation reaction Methods 0.000 claims abstract description 6
- 238000005406 washing Methods 0.000 claims abstract description 6
- CSCPPACGZOOCGX-UHFFFAOYSA-N Acetone Chemical compound CC(C)=O CSCPPACGZOOCGX-UHFFFAOYSA-N 0.000 claims description 10
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 8
- 239000013543 active substance Substances 0.000 claims description 6
- 239000002135 nanosheet Substances 0.000 claims description 6
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 6
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 6
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims description 5
- 238000005520 cutting process Methods 0.000 claims description 5
- 238000001962 electrophoresis Methods 0.000 claims description 5
- 238000002791 soaking Methods 0.000 claims description 5
- 238000009210 therapy by ultrasound Methods 0.000 claims description 5
- 238000007743 anodising Methods 0.000 claims description 2
- 238000002156 mixing Methods 0.000 claims description 2
- 239000011734 sodium Substances 0.000 claims 2
- JPVYNHNXODAKFH-UHFFFAOYSA-N Cu2+ Chemical compound [Cu+2] JPVYNHNXODAKFH-UHFFFAOYSA-N 0.000 claims 1
- BQCADISMDOOEFD-UHFFFAOYSA-N Silver Chemical compound [Ag] BQCADISMDOOEFD-UHFFFAOYSA-N 0.000 claims 1
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 claims 1
- 229910001431 copper ion Inorganic materials 0.000 claims 1
- BWFPGXWASODCHM-UHFFFAOYSA-N copper monosulfide Chemical class [Cu]=S BWFPGXWASODCHM-UHFFFAOYSA-N 0.000 claims 1
- 239000002245 particle Substances 0.000 claims 1
- 229910052709 silver Inorganic materials 0.000 claims 1
- 239000004332 silver Substances 0.000 claims 1
- 229910052717 sulfur Inorganic materials 0.000 claims 1
- 239000011593 sulfur Substances 0.000 claims 1
- 230000003647 oxidation Effects 0.000 abstract description 9
- 239000011941 photocatalyst Substances 0.000 abstract description 5
- 239000003054 catalyst Substances 0.000 abstract 1
- 230000015556 catabolic process Effects 0.000 description 5
- 238000006731 degradation reaction Methods 0.000 description 5
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 3
- 238000010438 heat treatment Methods 0.000 description 3
- 239000005416 organic matter Substances 0.000 description 3
- 230000001590 oxidative effect Effects 0.000 description 3
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 2
- 230000006866 deterioration Effects 0.000 description 2
- 239000003344 environmental pollutant Substances 0.000 description 2
- 239000001257 hydrogen Substances 0.000 description 2
- 229910052739 hydrogen Inorganic materials 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 231100000719 pollutant Toxicity 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005336 cracking Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000003487 electrochemical reaction Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003912 environmental pollution Methods 0.000 description 1
- 239000002803 fossil fuel Substances 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000002904 solvent Substances 0.000 description 1
- 238000002371 ultraviolet--visible spectrum Methods 0.000 description 1
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Classifications
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- B01J35/39—
-
- 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
- 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
-
- 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
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
-
- 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
-
- 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
-
- 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
- C02F2101/40—Organic compounds containing sulfur
-
- 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
A copper mesh in-situ growth three-dimensional copper sulfide photocatalytic material, a preparation method and application thereof are disclosed, wherein the material is prepared by carrying out anodic oxidation on graphite serving as a cathode, a copper mesh serving as an anode and a solution A serving as an electrolyte with a constant output current, repeatedly washing the copper mesh subjected to anodic oxidation by deionized water, and drying the copper mesh by nitrogen to obtain a product A; placing the product A in argon gas for annealing to obtain a product B; directly taking the product B as a photocatalytic film material. The catalyst directly grows on the carrier in situ is easy to collect, clean and repeatedly use. The method is simple and convenient to prepare, is less influenced by external factors, can be used for large-area uniform preparation, enables the photocatalyst to be easily recycled, and enables the prepared photocatalyst to have high sunlight utilization rate. The copper sulfide film obtained by the invention can be used for photocatalytic degradation of methylene blue.
Description
Technical Field
The invention relates to the technical field of photocatalysis, in particular to a preparation method and application of three-dimensional copper sulfide by in-situ growth of a copper mesh.
Background
Energy and environment are two major problems faced by the present society, with the increasing shortage of energy and the continuous deterioration of environment, the global embarrassment of energy shortage and environmental deterioration, the development of new energy and the management of environment are in the forefront, so the development of environment-friendly energy and the management of pollutants are very important subjects. Hydrogen gas is a clean, sustainable new energy source that is one of the candidates for fossil fuel hot substitutes. The photocatalysis technology utilizes clean solar energy to degrade pollutants and produce clean energy hydrogen while cracking water. How to improve the photocatalytic performance is an effective way to solve the current problems of environmental pollution and energy shortage.
In recent years, copper sulfide is favored in the fields of lithium ion batteries, sensors, supercapacitors, photocatalytic hydrogen production and the like, which is mainly due to excellent physicochemical stability, besides, the copper sulfide has a narrow band gap width and a wide photoresponse range, compared with common oxide photocatalysts, the utilization rate of the copper sulfide to sunlight is higher, the conductivity of the copper sulfide is higher by several orders of magnitude than that of corresponding oxides, and the copper sulfide shows higher electron transmission speed in the electrochemical reaction process; copper sulfide is one of the more desirable photocatalysts.
Disclosure of Invention
In order to improve and simplify the repeated utilization rate of the photocatalyst, the invention aims to provide a preparation method of a photocatalytic material for in-situ growth of three-dimensional copper sulfide on a copper mesh.
In order to achieve the purpose, the invention adopts the technical scheme that:
a preparation method of a photocatalytic material for in-situ growth of three-dimensional copper sulfide on a copper mesh comprises the following steps:
the method comprises the following steps: cutting the copper mesh into a certain size, sequentially putting the copper mesh into absolute ethyl alcohol, acetone and deionized water for ultrasonic treatment, and soaking the copper mesh in dilute hydrochloric acid with a certain concentration. Obtaining a plurality of polished copper meshes;
step two: mixing a certain molar amount of Na2S▪9H2Dissolving O in 200 ml deionized water to obtain a solution A;
step three: adjusting a triple-constant electrophoresis apparatus, outputting the product with a certain constant current, taking graphite as a cathode, a copper net as an anode and a solution A as electrolyte, anodizing for a certain time, repeatedly washing the anodized copper net with deionized water, and drying the anodized copper net with nitrogen to obtain a product A with black active substances attached to the copper net;
step four: and placing the product A in argon gas, and annealing for a certain time at a certain temperature to obtain a product B attached with the copper sulfide nanosheet.
In the second step, the concentration range of the solvent A is 0.5-1.5M.
In the third step, the anodic oxidation current range is 5-25 mA, and the oxidation time range is 5-30 min.
In the fourth step, the annealing temperature is 120-200 ℃, and the reaction lasts for 2-4 h.
The copper sulfide film prepared by the invention is used for photocatalytic degradation of organic matters containing hydrogen peroxide.
The copper sheet in-situ grown copper sulfide film provided by the invention is in a nano scale, and the copper sulfide nanosheets grown on the copper sheet vertically and uniformly grow on the copper mesh bottom; copper sulfide materials grown in situ on the copper mesh are in a micron scale, copper sulfide grown on the copper mesh is in a sheet structure and smooth in surface, and sheets are mutually connected and vertically and uniformly grow on a copper mesh line.
The preparation method has the advantages of low requirement on preparation equipment, small influence from the outside, simple method, low cost and high controllability, and is suitable for large-scale industrial production.
Drawings
FIG. 1 (a) is a simple schematic diagram of an anodic oxidation apparatus, (B) optical photographs of a product B of example 1 (c and d) scanning electron micrographs before and after oxidation of a copper mesh.
FIG. 2 is a UV-VIS absorption spectrum of a copper sulfide degradation methylene blue degradation liquid in example 1.
Detailed Description
The present invention will be described in further detail below.
Example 1
(1) Cutting 325 mesh copper net into 2 × 3 cm, sequentially adding into anhydrous ethanol, acetone and deionized water, respectively performing ultrasonic treatment for 3min, and soaking in certain 1.0M hydrochloric acid for 5 min to obtain several polished copper nets;
(2) adding 1.5M of Na2S▪9H2Dissolving O in 200 ml deionized water to obtain a solution A;
(3) adjusting a triple-constant electrophoresis apparatus, outputting current of 15 mA constantly, oxidizing the anode for 10 min by using graphite as a cathode, a copper net as an anode and solution A as electrolyte, repeatedly washing the copper net subjected to anodic oxidation by deionized water, and drying the copper net by nitrogen to obtain a product A with black active substances attached to the copper net;
(4) and placing the product A in argon gas at 200 ℃, annealing, heating for 1 h to 200 ℃, and keeping for 2 h to obtain a product B attached with the copper sulfide nanosheet.
The copper sulfide film prepared by the invention is used for photocatalytic degradation of methylene blue.
The concentration of the degraded organic matter is 10 mg/L, and the area of the film is 4 cm250 mL of the degradation solution contained 5 mLH2O2。
Example 2
(1) Cutting 325 mesh copper net into 2 × 3 cm, sequentially adding into anhydrous ethanol, acetone and deionized water, respectively performing ultrasonic treatment for 3min, and soaking in certain 1.0M hydrochloric acid for 5 min to obtain several polished copper nets;
(2) adding 1.5M of Na2S▪9H2Dissolving O in 200 ml deionized water to obtain a solution A;
(3) adjusting a triple-constant electrophoresis apparatus, outputting the current of 17 mA constantly, oxidizing the anode for 10 min by using graphite as a cathode, a copper net as an anode and the solution A as electrolyte, repeatedly washing the copper net subjected to the anodic oxidation by deionized water, and drying the copper net by nitrogen to obtain a product A with black active substances attached to the copper net;
(4) putting the product A in argon gas at 200 ℃, annealing and heating for 1 h to 200 ℃ for 2 h to obtain a product B attached with the copper sulfide nanosheet.
The copper sulfide film prepared by the invention is used for photocatalytic degradation of methylene blue.
The concentration of the degraded organic matter is 10 mg/L, and the area of the film is 4 cm250 mL of the degradation solution contained 5 mLH2O2。
Example 3
(1) Cutting 325 mesh copper net into 2 × 3 cm, sequentially adding into anhydrous ethanol, acetone and deionized water, respectively performing ultrasonic treatment for 3min, and soaking in certain 1.0M hydrochloric acid for 5 min to obtain several polished copper nets;
(2) adding 1.0M of Na2S▪9H2Dissolving O in 200 ml deionized water to obtain a solution A;
(3) adjusting a triple-constant electrophoresis apparatus, outputting the current of 20 mA constantly, oxidizing the anode for 10 min by using graphite as a cathode, a copper net as an anode and the solution A as electrolyte, repeatedly washing the copper net subjected to the anodic oxidation by using deionized water, and drying the copper net by using nitrogen to obtain a product A with black active substances attached to the copper net;
(4) and placing the product A in argon gas at 200 ℃, annealing, heating for 1 h to 200 ℃, and keeping for 2 h to obtain a product B attached with the copper sulfide nanosheet.
The copper sulfide film prepared by the invention is used for photocatalytic degradation of methylene blue.
The concentration of the degraded organic matter is 10 mg/L, and the area of the film is 4 cm250 mL of the degradation solution contained 5 mLH2O2。
Claims (7)
1. A preparation method of a photocatalytic material for in-situ growth of three-dimensional copper sulfide on a copper mesh is characterized by comprising the following steps:
immersing the cleaned copper mesh base material in a solution containing Na2In the electrolyte of S, taking the bottom of a copper mesh as an anode, introducing 5-30 mA current to carry out anodic oxidation reaction, and attaching a black active substance to the bottom surface of the copper mesh to obtain a product A; and annealing the product at 120-200 ℃ in an inert atmosphere to obtain a copper mesh photocatalytic material product B attached with copper sulfide.
2. The method of claim 1, wherein the sodium sulfide provides a sulfur source for the electrolyte; the bottom of the copper net is an anode and provides a copper ion source; na (Na)2The concentration of the S electrolyte is 0.5-1.5M.
3. The method according to claim 1, wherein the anodic oxidation reaction is performed for 5-30 min under a constant output of 5-30 mA current.
4. The method of claim 1, wherein the inert atmosphere is argon.
5. The method according to claim 1, characterized in that the specific steps comprise:
the method comprises the following steps: cutting a copper mesh into a certain size, sequentially putting the copper mesh into absolute ethyl alcohol, acetone and deionized water for ultrasonic treatment, and soaking the copper mesh in dilute hydrochloric acid with a certain concentration to obtain a plurality of polished copper meshes;
step two: mixing a certain molar amount of Na2S▪9H2Dissolving O in 200 ml deionized water to obtain a solution A;
step three: adjusting a triple-constant electrophoresis apparatus, outputting the product with a certain constant current, taking graphite as a cathode, a copper net as an anode and a solution A as electrolyte, anodizing for a certain time, repeatedly washing the anodized copper net with deionized water, and drying the anodized copper net with nitrogen to obtain a product A with black active substances attached to the copper net;
step four: and placing the product A in argon gas, and annealing at a certain temperature for a certain time to obtain a product B of the silver particle modified copper sulfide nanosheet.
6. A photocatalytic material prepared by the method according to any one of claims 1 to 5.
7. Use of the material according to claim 6 for the photocatalytic degradation of methylene blue.
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| Application Number | Priority Date | Filing Date | Title |
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| CN202010215886.7A CN111589457A (en) | 2020-03-25 | 2020-03-25 | Photocatalytic material for in-situ growth of three-dimensional copper sulfide on copper mesh, preparation method and application |
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| CN202010215886.7A CN111589457A (en) | 2020-03-25 | 2020-03-25 | Photocatalytic material for in-situ growth of three-dimensional copper sulfide on copper mesh, preparation method and application |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111974415A (en) * | 2020-08-31 | 2020-11-24 | 北京化工大学 | Copper sulfide/brass mesh electrode material with nanosheet array structure and preparation method and application thereof |
| CN112206664A (en) * | 2020-10-22 | 2021-01-12 | 西北师范大学 | One-step anodic oxidation preparation process of inorganic flexible super-hydrophobic super-oleophylic copper mesh |
| CN115212897A (en) * | 2022-07-26 | 2022-10-21 | 河北工业大学 | Self-standing nano porous copper-loaded nonacopper pentasulfide nanosheet composite material and preparation method and application thereof |
-
2020
- 2020-03-25 CN CN202010215886.7A patent/CN111589457A/en active Pending
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| 和茹梅: "阳极氧化法可控制备硫化铜三维纳米结构薄膜及其场致电子发射性能研究", 《中国优秀博硕士学位论文全文数据库(硕士)基础科学辑》 * |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111974415A (en) * | 2020-08-31 | 2020-11-24 | 北京化工大学 | Copper sulfide/brass mesh electrode material with nanosheet array structure and preparation method and application thereof |
| CN112206664A (en) * | 2020-10-22 | 2021-01-12 | 西北师范大学 | One-step anodic oxidation preparation process of inorganic flexible super-hydrophobic super-oleophylic copper mesh |
| CN115212897A (en) * | 2022-07-26 | 2022-10-21 | 河北工业大学 | Self-standing nano porous copper-loaded nonacopper pentasulfide nanosheet composite material and preparation method and application thereof |
| CN115212897B (en) * | 2022-07-26 | 2023-07-14 | 河北工业大学 | Self-supporting nano porous copper loaded nine copper pentasulfide nano sheet composite material and preparation method and application thereof |
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