CN111111697A - Method for preparing copper sulfide/zinc oxide nano composite photocatalytic material by room-temperature solid-phase chemical method - Google Patents
Method for preparing copper sulfide/zinc oxide nano composite photocatalytic material by room-temperature solid-phase chemical method Download PDFInfo
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- CN111111697A CN111111697A CN202010024982.3A CN202010024982A CN111111697A CN 111111697 A CN111111697 A CN 111111697A CN 202010024982 A CN202010024982 A CN 202010024982A CN 111111697 A CN111111697 A CN 111111697A
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- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 title claims abstract description 70
- 239000011787 zinc oxide Substances 0.000 title claims abstract description 35
- 239000000463 material Substances 0.000 title claims abstract description 29
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 23
- OMZSGWSJDCOLKM-UHFFFAOYSA-N copper(II) sulfide Chemical compound [S-2].[Cu+2] OMZSGWSJDCOLKM-UHFFFAOYSA-N 0.000 title claims abstract description 20
- 239000002114 nanocomposite Substances 0.000 title claims abstract description 17
- 239000007790 solid phase Substances 0.000 title claims abstract description 10
- 239000000126 substance Substances 0.000 title claims abstract description 9
- 238000002360 preparation method Methods 0.000 claims abstract description 8
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- 239000002105 nanoparticle Substances 0.000 claims description 11
- JIAARYAFYJHUJI-UHFFFAOYSA-L zinc dichloride Chemical compound [Cl-].[Cl-].[Zn+2] JIAARYAFYJHUJI-UHFFFAOYSA-L 0.000 claims description 10
- 239000004094 surface-active agent Substances 0.000 claims description 9
- 239000002202 Polyethylene glycol Substances 0.000 claims description 8
- 229920001223 polyethylene glycol Polymers 0.000 claims description 8
- 239000007787 solid Substances 0.000 claims description 8
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 8
- 239000012153 distilled water Substances 0.000 claims description 7
- 150000001879 copper Chemical class 0.000 claims description 6
- 238000000227 grinding Methods 0.000 claims description 6
- 238000002156 mixing Methods 0.000 claims description 6
- 238000001035 drying Methods 0.000 claims description 5
- 239000011592 zinc chloride Substances 0.000 claims description 5
- 235000005074 zinc chloride Nutrition 0.000 claims description 5
- 239000002879 Lewis base Substances 0.000 claims description 4
- 150000007527 lewis bases Chemical class 0.000 claims description 4
- 150000003751 zinc Chemical class 0.000 claims description 4
- 239000002131 composite material Substances 0.000 claims description 3
- XTVVROIMIGLXTD-UHFFFAOYSA-N copper(II) nitrate Chemical compound [Cu+2].[O-][N+]([O-])=O.[O-][N+]([O-])=O XTVVROIMIGLXTD-UHFFFAOYSA-N 0.000 claims description 3
- 229910052979 sodium sulfide Inorganic materials 0.000 claims description 3
- GRVFOGOEDUUMBP-UHFFFAOYSA-N sodium sulfide (anhydrous) Chemical compound [Na+].[Na+].[S-2] GRVFOGOEDUUMBP-UHFFFAOYSA-N 0.000 claims description 3
- 238000000967 suction filtration Methods 0.000 claims description 3
- 238000001914 filtration Methods 0.000 claims description 2
- 230000007613 environmental effect Effects 0.000 abstract description 7
- 229960000907 methylthioninium chloride Drugs 0.000 abstract description 7
- 230000000593 degrading effect Effects 0.000 abstract description 6
- 239000003344 environmental pollutant Substances 0.000 abstract description 6
- 231100000719 pollutant Toxicity 0.000 abstract description 6
- 238000005516 engineering process Methods 0.000 abstract description 4
- 230000015572 biosynthetic process Effects 0.000 abstract description 3
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 3
- 238000003786 synthesis reaction Methods 0.000 abstract description 3
- 238000004065 wastewater treatment Methods 0.000 abstract 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 abstract 2
- 239000004065 semiconductor Substances 0.000 description 11
- CXKWCBBOMKCUKX-UHFFFAOYSA-M methylene blue Chemical compound [Cl-].C1=CC(N(C)C)=CC2=[S+]C3=CC(N(C)C)=CC=C3N=C21 CXKWCBBOMKCUKX-UHFFFAOYSA-M 0.000 description 5
- 238000005265 energy consumption Methods 0.000 description 4
- 239000002086 nanomaterial Substances 0.000 description 4
- 238000007146 photocatalysis Methods 0.000 description 4
- 230000015556 catabolic process Effects 0.000 description 3
- 238000006731 degradation reaction Methods 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 230000006798 recombination Effects 0.000 description 3
- 238000005215 recombination Methods 0.000 description 3
- 229920002565 Polyethylene Glycol 400 Polymers 0.000 description 2
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 2
- 230000009286 beneficial effect Effects 0.000 description 2
- 230000005540 biological transmission Effects 0.000 description 2
- 238000013329 compounding Methods 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 239000004570 mortar (masonry) Substances 0.000 description 2
- JLFNLZLINWHATN-UHFFFAOYSA-N pentaethylene glycol Chemical compound OCCOCCOCCOCCOCCO JLFNLZLINWHATN-UHFFFAOYSA-N 0.000 description 2
- 238000000053 physical method Methods 0.000 description 2
- UFHFLCQGNIYNRP-UHFFFAOYSA-N Hydrogen Chemical compound [H][H] UFHFLCQGNIYNRP-UHFFFAOYSA-N 0.000 description 1
- 206010034972 Photosensitivity reaction Diseases 0.000 description 1
- 238000010521 absorption reaction Methods 0.000 description 1
- 239000000969 carrier Substances 0.000 description 1
- 230000003197 catalytic effect Effects 0.000 description 1
- 238000005285 chemical preparation method Methods 0.000 description 1
- 238000006243 chemical reaction Methods 0.000 description 1
- 238000005229 chemical vapour deposition Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000000151 deposition Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 229910052739 hydrogen Inorganic materials 0.000 description 1
- 239000001257 hydrogen Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 230000031700 light absorption Effects 0.000 description 1
- 238000001755 magnetron sputter deposition Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000011943 nanocatalyst Substances 0.000 description 1
- 231100000956 nontoxicity Toxicity 0.000 description 1
- 230000033116 oxidation-reduction process Effects 0.000 description 1
- 230000036211 photosensitivity Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000006862 quantum yield reaction Methods 0.000 description 1
- 230000001105 regulatory effect Effects 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000010532 solid phase synthesis reaction Methods 0.000 description 1
- 230000001954 sterilising effect Effects 0.000 description 1
- 238000004659 sterilization and disinfection Methods 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000002351 wastewater Substances 0.000 description 1
- 238000003911 water pollution 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
- 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
The invention discloses a novel method for preparing a copper sulfide/zinc oxide nano composite photocatalytic material by a room-temperature solid-phase chemical method, belonging to the technical field of preparation of novel nano photocatalytic materials. The technology prepares the copper sulfide/zinc oxide nano composite material by a simple, green and environment-friendly solid phase chemical method, shows excellent photocatalytic performance in the aspect of degrading organic pollutant methylene blue, and has the efficiency of degrading methylene blue pollutant up to 99.1 percent in 80 minutes. The preparation method disclosed by the invention has the advantages of simple synthesis process, environmental friendliness, high yield, low cost and the like, and has potential application prospects in the aspects of wastewater treatment and environmental protection.
Description
Technical Field
The invention relates to the field of novel nano material preparation, in particular to a copper sulfide/zinc oxide nano composite photocatalytic material and a room-temperature solid-phase chemical preparation method thereof.
Background
In semiconductor materials, the photocatalytic effect is one of effective technologies for efficiently utilizing solar energy resources, and has important significance in solving the global environmental pollution problem and developing new energy. The semiconductor photocatalyst can effectively degrade various pollutants at room temperature, has the advantages of low price, easy obtainment, low energy consumption, high efficiency, environmental protection and the like, and has potential application prospect in the fields of water pollution treatment and renewable resource development and utilization.
The zinc oxide material is an important semiconductor material, is used as a typical semiconductor photocatalyst, has the advantages of higher oxidation-reduction potential and electron mobility, higher photosensitivity, low cost, no toxicity, environmental friendliness and the like, and has wide application value and good application prospect in the aspects of wastewater treatment, hydrogen production by water splitting, biological sterilization and the like. However, the single zinc oxide material can only utilize the defects of easy recombination of ultraviolet part, photogenerated electrons and holes, low quantum yield and the like in sunlight, so that the application of the zinc oxide material in the field of photocatalysis is limited. How to improve the rapid transmission of electrons in zinc oxide, effectively utilize solar energy, reduce the recombination of photo-generated electrons and holes, improve the separation efficiency of electrons and holes, and the like is an important problem to be solved urgently.
The semiconductor composite technology is one of simple and effective methods for improving the catalytic efficiency of the photocatalyst, and can effectively separate photon-generated carriers, regulate and control the forbidden bandwidth of a semiconductor, improve the rapid transmission of electrons, and reduce the recombination of photon-generated electrons and holes, thereby effectively improving the photocatalytic efficiency. Copper sulfide is a semiconductor material with a narrow forbidden band, the forbidden band width of the semiconductor material is 2.2 eV, the semiconductor material has good absorption on visible light, and when photons with proper energy are absorbed, a large number of electrons and holes are generated. By adopting a semiconductor compounding technology, the copper sulfide and the zinc oxide nano material are compounded, so that the light absorption response capability of the material can be improved, the forbidden bandwidth of a semiconductor can be effectively regulated and controlled, the photo-generated electron-hole compounding is reduced, and the photocatalytic activity is effectively improved.
The method for preparing the zinc oxide nano catalyst comprises a physical method and a chemical method, wherein the physical method comprises a magnetron sputtering method, a laser pulse deposition method, a vacuum evaporation method and the like. The chemical method mainly comprises a sol-gel method, a hydrothermal method, a metal organic chemical vapor deposition method, a solid phase chemical method and the like. The solid phase chemical method has the advantages of simple synthesis process, high yield, low energy consumption, environmental protection and the like, and is one of the main methods for preparing zinc oxide nano materials in large scale in industry.
Disclosure of Invention
The invention aims to provide a novel copper sulfide/zinc oxide nano composite photocatalytic material for efficiently degrading pollutants by photocatalysis according to the problem of low photocatalytic efficiency of a single zinc oxide nano material.
The invention also aims to provide a novel method for preparing the copper sulfide/zinc oxide nano composite photocatalytic material, which has the advantages of simple process, environmental protection, low energy consumption and high yield.
In order to realize the aim, the invention provides a method for preparing a copper sulfide/zinc oxide nano composite photocatalytic material by a room-temperature solid-phase method, which comprises the following steps:
adding a proper amount of surfactant polyethylene glycol, mixing and grinding zinc oxide nano particles and copper salt according to a certain molar ratio for 50 minutes, adding sodium sulfide with an equal molar ratio, mixing and grinding for 1 hour, dissolving in distilled water, carrying out suction filtration by using a Buchner funnel, and standing and drying for 12 hours.
The amount of the appropriate amount of the surfactant polyethylene glycol is 1 ml, the molar ratio of the zinc oxide nano-particles to the copper salt is 1:0.005, and the copper salt is copper nitrate.
The zinc oxide nano-particles are characterized in that the preparation method comprises the following steps: adding a proper amount of surfactant polyethylene glycol, mixing and grinding the solid zinc salt and the solid Lewis base in a certain molar ratio, standing for 5 hours in a dark place, dissolving by distilled water, filtering by a Buchner funnel, and standing and drying for 12 hours.
The dosage of the appropriate amount of the surfactant polyethylene glycol is 5 ml, and the certain molar ratio is 1: 4, 0.01 mol of zinc chloride is taken as solid zinc salt, and 0.04 mol of sodium hydroxide is taken as solid Lewis base.
The above zinc chloride was 1.36 g, and sodium hydroxide was 1.60 g.
Compared with the prior art, the invention has the following advantages:
the copper sulfide/zinc oxide nano composite photocatalytic material prepared by the invention has the advantages of simple synthesis process, environmental protection, low energy consumption and the like, is easy to popularize in scientific basic research and actual industrial production, and has good application prospect.
The copper sulfide/zinc oxide nano composite photocatalytic material prepared by the invention has the performance of efficiently degrading methylene blue serving as a pollutant through photocatalysis, is beneficial to treating waste water in the environment, and is beneficial to solving the problem of environmental pollution in China.
Drawings
FIG. 1 is a schematic diagram of the concentration of methylene blue of organic pollutants degraded by the copper sulfide/zinc oxide nano composite photocatalytic material prepared by the invention;
FIG. 2 is a graph of the degradation efficiency of the copper sulfide/zinc oxide nano composite photocatalytic material prepared by the invention for degrading organic pollutant methylene blue within 80 minutes.
Detailed Description
The preparation of the invention is further illustrated by the following examples.
Example 1 Room temperature solid phase preparation of copper sulfide/zinc oxide nano composite photocatalytic material
Preparing a zinc oxide nanoparticle precursor: 0.01 mol of zinc chloride is weighed into an agate mortar, ground into fine powder and mixed with 5 ml of PEG400 for 50 minutes. Then 0.04 mol of sodium hydroxide is added, ground for 1 hour, and the sample is kept standing for 5 hours in the dark to ensure the solid phase chemical reaction is complete. Finally, the surfactant was removed by precipitation twice with 1000 ml of distilled water in a beaker. And (4) carrying out suction filtration by using distilled water, and naturally drying to obtain the zinc oxide nanoparticles.
Preparing a copper sulfide/zinc oxide nano composite photocatalytic material: 0.5 g of zinc oxide nanoparticles was weighed into an agate mortar, 0.5% by mole of copper nitrate was added, and the mixture was ground for 10 minutes and then mixed with 1 ml of PEG400 and ground for 50 minutes. An equimolar amount of sodium sulfide was weighed, mixed and ground for 1 hour. And finally, washing the sample by using distilled water, and naturally airing to obtain the copper sulfide/zinc oxide nano composite photocatalytic material.
A UV-vis ultraviolet analyzer is utilized to test the performance of the copper sulfide/zinc oxide nano composite material for degrading the methylene blue pollutant in a photocatalysis way, the degradation concentration-time of the methylene blue pollutant is shown in figure 1, and the degradation efficiency in 80 minutes is shown in figure 2.
Claims (6)
1. A room-temperature solid-phase chemical method for preparing a copper sulfide/zinc oxide nano composite photocatalytic material is characterized in that the composite photocatalytic material consists of zinc oxide nano particles and copper sulfide nano particles.
2. The composite photocatalytic material according to claim 1, characterized in that said preparation method consists of the following steps: adding a proper amount of surfactant polyethylene glycol, mixing and grinding zinc oxide nano particles and copper salt according to a certain molar ratio for 50 minutes, adding sodium sulfide with an equal molar ratio, mixing and grinding for 1 hour, dissolving in distilled water, carrying out suction filtration by using a Buchner funnel, and standing and drying for 12 hours.
3. A suitable amount of the surfactant of claim 2, polyethylene glycol, in an amount of 1 ml, in a molar ratio of zinc oxide nanoparticles to copper salt of 1:0.005, said copper salt being copper nitrate.
4. The zinc oxide nanoparticles according to claim 3, characterized in that the preparation method consists of the following steps: adding a proper amount of surfactant polyethylene glycol, mixing and grinding the solid zinc salt and the solid Lewis base in a certain molar ratio, standing for 5 hours in a dark place, dissolving by distilled water, filtering by a Buchner funnel, and standing and drying for 12 hours.
5. A proper amount of the surfactant polyethylene glycol according to claim 4 is 5 ml, and the molar ratio is 1: 4, 0.01 mol of zinc chloride is taken as solid zinc salt, and 0.04 mol of sodium hydroxide is taken as solid Lewis base.
6. The zinc chloride of claim 5 is 1.36 grams and the sodium hydroxide is 1.60 grams.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN202010024982.3A CN111111697A (en) | 2020-01-10 | 2020-01-10 | Method for preparing copper sulfide/zinc oxide nano composite photocatalytic material by room-temperature solid-phase chemical method |
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| CN202010024982.3A CN111111697A (en) | 2020-01-10 | 2020-01-10 | Method for preparing copper sulfide/zinc oxide nano composite photocatalytic material by room-temperature solid-phase chemical method |
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| CN111111697A true CN111111697A (en) | 2020-05-08 |
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| CN202010024982.3A Pending CN111111697A (en) | 2020-01-10 | 2020-01-10 | Method for preparing copper sulfide/zinc oxide nano composite photocatalytic material by room-temperature solid-phase chemical method |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112209476A (en) * | 2020-10-21 | 2021-01-12 | 新疆大学 | Method for degrading organic dye by applying low-dimensional zinc oxide nano material through piezoelectric catalysis |
| CN115518658A (en) * | 2022-09-20 | 2022-12-27 | 广州大学 | Preparation method and application of cluster spherical multiphase Fenton catalyst |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112209476A (en) * | 2020-10-21 | 2021-01-12 | 新疆大学 | Method for degrading organic dye by applying low-dimensional zinc oxide nano material through piezoelectric catalysis |
| CN115518658A (en) * | 2022-09-20 | 2022-12-27 | 广州大学 | Preparation method and application of cluster spherical multiphase Fenton catalyst |
| CN115518658B (en) * | 2022-09-20 | 2023-06-20 | 广州大学 | Preparation method and application of flower cluster spherical multiphase Fenton catalyst |
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