CN111644173A - Method for improving photocatalytic activity of copper oxide - Google Patents
Method for improving photocatalytic activity of copper oxide Download PDFInfo
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- CN111644173A CN111644173A CN202010114440.5A CN202010114440A CN111644173A CN 111644173 A CN111644173 A CN 111644173A CN 202010114440 A CN202010114440 A CN 202010114440A CN 111644173 A CN111644173 A CN 111644173A
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- copper oxide
- oxygen vacancies
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- ethyl alcohol
- absolute ethyl
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- QPLDLSVMHZLSFG-UHFFFAOYSA-N Copper oxide Chemical compound [Cu]=O QPLDLSVMHZLSFG-UHFFFAOYSA-N 0.000 title claims abstract description 101
- 239000005751 Copper oxide Substances 0.000 title claims abstract description 94
- 229910000431 copper oxide Inorganic materials 0.000 title claims abstract description 93
- 230000001699 photocatalysis Effects 0.000 title claims abstract description 25
- 238000000034 method Methods 0.000 title claims abstract description 18
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 claims abstract description 28
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims abstract description 26
- 239000001301 oxygen Substances 0.000 claims abstract description 26
- 229910052760 oxygen Inorganic materials 0.000 claims abstract description 26
- 238000010791 quenching Methods 0.000 claims abstract description 11
- 230000000171 quenching effect Effects 0.000 claims abstract description 11
- 238000010438 heat treatment Methods 0.000 claims abstract description 5
- 125000004430 oxygen atom Chemical group O* 0.000 claims abstract description 5
- 238000001035 drying Methods 0.000 claims abstract description 4
- 238000001914 filtration Methods 0.000 claims abstract description 4
- 238000002791 soaking Methods 0.000 claims abstract description 4
- 238000005245 sintering Methods 0.000 claims description 6
- 239000002245 particle Substances 0.000 claims description 3
- 238000007654 immersion Methods 0.000 claims 1
- 230000015556 catabolic process Effects 0.000 abstract description 7
- 238000006731 degradation reaction Methods 0.000 abstract description 7
- 239000002957 persistent organic pollutant Substances 0.000 abstract description 6
- 239000000463 material Substances 0.000 abstract description 4
- 230000000694 effects Effects 0.000 abstract description 3
- 230000003197 catalytic effect Effects 0.000 abstract description 2
- 239000002105 nanoparticle Substances 0.000 description 11
- 239000000243 solution Substances 0.000 description 8
- -1 TiO2 and ZnO Chemical class 0.000 description 4
- 230000015572 biosynthetic process Effects 0.000 description 4
- 239000003054 catalyst Substances 0.000 description 4
- 238000006243 chemical reaction Methods 0.000 description 4
- 239000000356 contaminant Substances 0.000 description 4
- 239000000975 dye Substances 0.000 description 4
- 238000012360 testing method Methods 0.000 description 4
- 239000007864 aqueous solution Substances 0.000 description 3
- QSHDDOUJBYECFT-UHFFFAOYSA-N mercury Chemical compound [Hg] QSHDDOUJBYECFT-UHFFFAOYSA-N 0.000 description 3
- 229910052753 mercury Inorganic materials 0.000 description 3
- 239000011941 photocatalyst Substances 0.000 description 3
- 238000001179 sorption measurement Methods 0.000 description 3
- GWEVSGVZZGPLCZ-UHFFFAOYSA-N Titan oxide Chemical compound O=[Ti]=O GWEVSGVZZGPLCZ-UHFFFAOYSA-N 0.000 description 2
- 238000010521 absorption reaction Methods 0.000 description 2
- 239000013078 crystal Substances 0.000 description 2
- 238000002474 experimental method Methods 0.000 description 2
- 238000012986 modification Methods 0.000 description 2
- 230000004048 modification Effects 0.000 description 2
- 238000007146 photocatalysis Methods 0.000 description 2
- 238000013033 photocatalytic degradation reaction Methods 0.000 description 2
- 238000001782 photodegradation Methods 0.000 description 2
- 239000004065 semiconductor Substances 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 230000007704 transition Effects 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- MHAJPDPJQMAIIY-UHFFFAOYSA-N Hydrogen peroxide Chemical compound OO MHAJPDPJQMAIIY-UHFFFAOYSA-N 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000004458 analytical method Methods 0.000 description 1
- 238000006555 catalytic reaction Methods 0.000 description 1
- 238000011109 contamination Methods 0.000 description 1
- 238000001816 cooling Methods 0.000 description 1
- 239000010949 copper Substances 0.000 description 1
- 238000000354 decomposition reaction Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000002848 electrochemical method Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000002708 enhancing effect Effects 0.000 description 1
- 235000019441 ethanol Nutrition 0.000 description 1
- 239000011521 glass Substances 0.000 description 1
- 230000036541 health Effects 0.000 description 1
- 229910001385 heavy metal Inorganic materials 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000003760 magnetic stirring Methods 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 230000003278 mimic effect Effects 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 238000012544 monitoring process Methods 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002073 nanorod Substances 0.000 description 1
- 239000002077 nanosphere Substances 0.000 description 1
- 239000002071 nanotube Substances 0.000 description 1
- 230000003287 optical effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000001556 precipitation Methods 0.000 description 1
- 230000001737 promoting effect Effects 0.000 description 1
- 239000010453 quartz Substances 0.000 description 1
- 238000000926 separation method Methods 0.000 description 1
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N silicon dioxide Inorganic materials O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 1
- 238000003980 solgel method Methods 0.000 description 1
- 238000003756 stirring Methods 0.000 description 1
- 238000001308 synthesis method Methods 0.000 description 1
- 238000003786 synthesis reaction Methods 0.000 description 1
- 231100000331 toxic Toxicity 0.000 description 1
- 230000002588 toxic effect Effects 0.000 description 1
- 238000009281 ultraviolet germicidal irradiation Methods 0.000 description 1
- 238000000870 ultraviolet spectroscopy Methods 0.000 description 1
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- B01J35/39—
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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
- B01J23/70—Catalysts comprising metals or metal oxides or hydroxides, not provided for in group B01J21/00 of the iron group metals or copper
- B01J23/72—Copper
-
- 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
- C02F1/32—Treatment of water, waste water, or sewage by irradiation with ultraviolet light
-
- 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
- C02F2101/308—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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
-
- 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
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Health & Medical Sciences (AREA)
- Toxicology (AREA)
- Life Sciences & Earth Sciences (AREA)
- Hydrology & Water Resources (AREA)
- Environmental & Geological Engineering (AREA)
- Water Supply & Treatment (AREA)
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Abstract
A method of increasing the photocatalytic activity of copper oxide comprising the steps of: heating the copper oxide to enable the temperature of the copper oxide to reach 750-850 ℃; putting the copper oxide into absolute ethyl alcohol, completely soaking, and carrying out rapid quenching treatment, wherein the absolute ethyl alcohol consumes oxygen atoms on the surface of the copper oxide, so that oxygen vacancies are formed on the surface of the copper oxide; then filtering and taking out the copper oxide, and drying for 2-4 hours at the temperature of 75-85 ℃ to finish the treatment of the copper oxide, thus obtaining the copper oxide with oxygen vacancies on the surface. The invention adopts absolute ethyl alcohol to carry out rapid quenching treatment on the copper oxide, so that a large number of high-concentration oxygen vacancies are formed on the surface of the copper oxide, the photocatalytic performance of the copper oxide is effectively improved, the surface activity is improved, and the copper oxide can be used as a degradation catalytic material of organic pollutants to effectively degrade the organic pollutants.
Description
Technical Field
The invention relates to treatment of copper oxide, in particular to a method for improving the photocatalytic activity of copper oxide.
Background
In recent years, rapid industrialization has led to the contamination of water bodies with heavy metals, toxic organic pollutants (e.g. dyes) and harmful chemicals to surprising levels, which constitute a serious threat to the environment and human health and have profound effects. In particular, the degradation of organic contaminants remains a great challenge, and photocatalysis is considered as a potential degradation method, and thus efforts to remove organic contaminants by photocatalysis are increasing. Due to their extraordinary properties, copper oxide semiconductor nanomaterials have attracted considerable attention as a technology for photocatalytic degradation of organic dye contaminants under ultraviolet or visible light.
Particularly transition copper oxides such as TiO2 and ZnO, are considered important semiconductor materials. In addition, copper oxide attracts many material scientists' attention by virtue of its excellent optical, chemical, electronic and physical properties and its relatively low cost. CuO is a p-type transition copper oxide with a narrow band gap of 1.59eV, and is widely used in, for example, lithium ion batteries, photocatalysts, supercapacitors and sensors. In recent years, the synthesis of nano CuO with different morphologies has been widely reported, such as nanospheres, nanorods, nanoarrays and nanotubes. In addition, the synthesis method of nano copper oxide is also diversified, such as a precipitation method, a sol-gel method, a hydrothermal synthesis method and an electrochemical method. However, despite the increasing use of CuO to date, its use alone as a photocatalyst is still uncommon due to its relatively low photocatalytic activity.
Disclosure of Invention
The invention aims to provide a method for improving the photocatalytic activity of copper oxide.
In order to solve the technical problems, the invention adopts the following technical scheme:
a method of increasing the photocatalytic activity of copper oxide comprising the steps of:
heating the copper oxide to enable the temperature of the copper oxide to reach 750-850 ℃;
putting the copper oxide into absolute ethyl alcohol, completely soaking, and carrying out rapid quenching treatment, wherein the absolute ethyl alcohol consumes oxygen atoms on the surface of the copper oxide, so that oxygen vacancies are formed on the surface of the copper oxide;
then filtering and taking out the copper oxide, and drying for 2-4 hours at the temperature of 75-85 ℃ to finish the treatment of the copper oxide, thus obtaining the copper oxide with oxygen vacancies on the surface.
The copper oxide is heated to the temperature of 750-850 ℃ and then kept for 20-30 minutes.
The temperature condition of the absolute ethyl alcohol is a room temperature condition which is a temperature environment of 20-35 ℃.
When the copper oxide is heated, the copper oxide is firstly placed in a sintering boat, then the muffle furnace is heated to the temperature of 750-.
The copper oxide is copper oxide nano-particles with the particle size less than 40 nm. The purity is more than 99.6%.
When the copper oxide is put into the absolute ethyl alcohol, the dosage of the absolute ethyl alcohol ensures that the copper oxide can be completely immersed in the absolute ethyl alcohol.
After the copper oxide is heated and placed in absolute ethyl alcohol for rapid quenching treatment, oxygen vacancies are formed on the surface of the copper oxide, and the oxygen vacancies cannot migrate into the copper oxide.
The method adopts the absolute ethyl alcohol to carry out rapid quenching treatment on the copper oxide, so that a large number of high-concentration oxygen vacancies are formed on the surface of the copper oxide, the photocatalytic performance of the copper oxide is effectively improved, the surface activity is improved, the copper oxide can be used as a degradation catalytic material for organic pollutants, the organic pollutants are effectively degraded, and the pollution of the organic pollutants such as dyes to the environment is reduced.
Drawings
FIG. 1 is a schematic diagram of photodegradation of nano-CuO and Q-CuO to RhB aqueous solution under ultraviolet light;
FIG. 2 shows the relationship between-ln (C/C0) of RhB concentration and ultraviolet irradiation time.
Detailed Description
For further understanding of the features and technical means of the present invention, as well as the specific objects and functions attained by the present invention, the present invention will be described in further detail with reference to the accompanying drawings and detailed description.
The invention discloses a method for improving the photocatalytic activity of copper oxide, which comprises the following steps:
heating the copper oxide to make the temperature of the copper oxide reach 750-850 ℃ and maintaining the temperature for 20-30 minutes.
And (2) putting the copper oxide into absolute ethyl alcohol at room temperature, completely soaking, and performing rapid quenching treatment, wherein the absolute ethyl alcohol consumes oxygen atoms on the surface of the copper oxide, so that oxygen vacancies are formed on the surface of the copper oxide, and the room temperature is 20-35 ℃.
Then filtering and taking out the copper oxide, and drying for 2-4 hours at the temperature of 75-85 ℃ to finish the treatment of the copper oxide, thus obtaining the copper oxide with oxygen vacancies on the surface.
The copper oxide is heated to the temperature of 750-850 ℃ and then kept for 20-30 minutes.
When the copper oxide is heated, the copper oxide is firstly placed in a sintering boat, then the muffle furnace is heated to the temperature of 750-.
The copper oxide is copper oxide nano-particles with the particle size less than 40 nm. The purity is more than 99.6%.
After the copper oxide is heated and placed in absolute ethyl alcohol for rapid quenching treatment, oxygen vacancies are formed on the surface of the copper oxide, and the oxygen vacancies cannot migrate into the copper oxide.
Example one
2 g of copper oxide nanoparticles were weighed and placed in a sintering boat (length 6 cm, width 3 cm, height 1.5 cm). The sintered boat containing the copper oxide nanoparticles was transferred to the muffle furnace for 20 minutes while the muffle furnace was heated to 800 ℃. After the muffle furnace is opened, the sintering boat is immediately taken out, and the copper oxide nano-particles are immersed in 40mL of absolute ethyl alcohol at room temperature for rapid quenching. Finally, the quenched copper oxide nanoparticles were filtered and then dried at 800 ℃ for 3 hours to obtain treated copper oxide nanoparticles.
To verify whether the treated copper oxide nanoparticles have good photocatalytic performance, the following test can be performed.
Photocatalytic testing
RhB is a red organic dye that is widely used as a mimic contaminant in photocatalytic tests. The photocatalytic activity of the prepared samples was evaluated by monitoring the decomposition of RhB in an aqueous solution under the irradiation of ultraviolet light from a 500W mercury lamp. The lamp was placed in a cylindrical heat-resistant glass vessel, and the reaction temperature was maintained at about 27 ℃ by cooling with circulating water. The quartz tube was used as a photocatalytic reactor. The catalyst (0.03 g) was mixed with an aqueous RhB solution (40 mL, 2X10-5 mol/L). After stirring in the dark for 30 minutes to reach the adsorption equilibrium between the catalyst and the RhB solution, the mercury lamp was turned on and the mixture was exposed to uv light. Vigorous magnetic stirring was maintained to suspend the catalyst in the RhB solution. The concentration of the aqueous solution was determined by measuring the absorption peak intensity of the centrifuged RhB solution at 553nm (absorption peak of RhB) by an ultraviolet-visible spectrophotometer every 20 minutes.
Anhydrous ethanol is an anoxic environment. When nano-CuO is quenched in absolute ethanol, the absolute ethanol consumes oxygen atoms on the surface of CuO crystals, thereby causing oxygen vacancies to occur on the crystal surface. Using the standard Kroger-Vink notation, the formation of oxygen vacancies at high temperatures can be described by the following equilibrium: o isO⟷ VO+1/2O2(g) +2 e. Wherein, OORepresents lattice oxygen, VORepresenting an oxygen vacancy. At the same time, Cu is accompanied in order to maintain the local charge balance in the copper oxide2And (4) generating O.
Photocatalytic degradation test
And carrying out photocatalytic activity analysis on the prepared copper oxide nanoparticles. In the experiment, a dark adsorption experiment was performed for 30 minutes before the mercury lamp was turned on to ensure the adsorption equilibrium of the RhB solution on the catalyst surface. The results are shown in FIG. 1, where T, C and C0The exposure time, instantaneous RhB concentration, and RhB concentration before exposure are indicated, respectively. C/C0For describing the degradation rate, it means the concentration ratio of the initial solution to the reaction after a certain time. It can be seen that the prepared copper oxide Q-CuO shows stronger ultraviolet light catalysis than the non-prepared copper oxide Nano-particles Nano-CuO. For the prepared copper oxide and the crudeThe prepared copper oxide nanoparticles, RhB, were degraded for 230 minutes to leave about 8% and 23%, respectively.
To quantitatively analyze the reaction kinetics of RhB degradation, the experimental data in fig. 1 were fitted by langmuir-hounsfield kinetic model (-ln (C/C0) = kT), as shown in fig. 2, where k is the pseudo first order rate constant. Of two samples-ln (C/C)0) Has good linear correlation with the time T. The corresponding k values of Nano-CuO and Q-CuO were calculated to be 4.97x10-3 min, respectively-1And 9.98x10-3 min-1. These results indicate that Q-CuO exhibits photocatalytic activity superior to nano-CuO.
The prepared Q-CuO shows relatively higher photocatalytic performance than the original Nano-CuO, which is not prepared, probably due to the high concentration of oxygen vacancies formed at the surface of the Q-CuO. It is well known that the formation of superoxide ions is a key step in the formation of intermediate reactive species, such as hydrogen peroxide (H2O 2) and.oh, during the initial stages of the photoreaction. These intermediate active species play an important role in the photodegradation of organic molecules, since oxygen vacancies in the photocatalyst produce more reaction with O2 to form superoxide ions, the photogenerated holes of O2, and therefore, the number of oxygen vacancies on the oxide surface will greatly affect the production of superoxide ions. Thus, the enhanced photocatalytic activity can be attributed to oxygen vacancies generated on the surface of Q — CuO.
From the above, it can be seen that the surface-modified copper oxide shows higher photocatalytic activity for degradation of RhB solution under uv irradiation than the unmodified copper oxide. After the quenching of the rapid ethanol, high-concentration oxygen vacancies are formed on the surface of Q-CuO, thereby promoting the charge hole separation, enhancing the photocatalytic activity, and the oxygen vacancies formed on the surface can not migrate to the inside.
Although the present invention has been described in detail with reference to the embodiments, it will be apparent to those skilled in the art that modifications, equivalents, improvements, and the like can be made in the technical solutions of the foregoing embodiments or in some of the technical features of the foregoing embodiments, but those modifications, equivalents, improvements, and the like are all within the spirit and principle of the present invention.
Claims (7)
1. A method of increasing the photocatalytic activity of copper oxide comprising the steps of:
heating the copper oxide to enable the temperature of the copper oxide to reach 750-850 ℃;
putting the copper oxide into absolute ethyl alcohol, completely soaking, and carrying out rapid quenching treatment, wherein the absolute ethyl alcohol consumes oxygen atoms on the surface of the copper oxide, so that oxygen vacancies are formed on the surface of the copper oxide;
then filtering and taking out the copper oxide, and drying for 2-4 hours at the temperature of 75-85 ℃ to finish the treatment of the copper oxide, thus obtaining the copper oxide with oxygen vacancies on the surface.
2. The method of claim 1 wherein the copper oxide is heated to a temperature of about 750 ℃. 850 ℃ and then held for a period of about 20 to about 30 minutes.
3. The method for improving the photocatalytic activity of copper oxide according to claim 2, wherein the temperature condition of the anhydrous ethanol is a room temperature condition, and the room temperature condition is a temperature environment of 20 to 35 ℃.
4. The method as claimed in claim 3, wherein the copper oxide is heated by placing the copper oxide in a sintering boat, heating the muffle furnace to 850 deg.C, placing the sintering boat containing the copper oxide in the muffle furnace, and maintaining the temperature for 20-30 min.
5. The method of claim 4 wherein the copper oxide has a particle size of less than 40nm and a purity of greater than 99.6%.
6. The method of claim 5, wherein the amount of absolute ethanol used to immerse the copper oxide in the absolute ethanol is sufficient to ensure complete immersion of the copper oxide in the absolute ethanol.
7. The method of claim 6, wherein the copper oxide is heated and then placed in anhydrous ethanol for rapid quenching treatment, so that oxygen vacancies are formed on the surface of the copper oxide, and the oxygen vacancies do not migrate into the interior of the copper oxide.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112958089A (en) * | 2021-02-08 | 2021-06-15 | 哈尔滨工业大学 | Preparation method of copper oxide catalyst for catalyzing persulfate to degrade pollutants in water |
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2020
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN112958089A (en) * | 2021-02-08 | 2021-06-15 | 哈尔滨工业大学 | Preparation method of copper oxide catalyst for catalyzing persulfate to degrade pollutants in water |
| CN112958089B (en) * | 2021-02-08 | 2023-09-01 | 哈尔滨工业大学 | Preparation method of copper oxide catalyst for catalyzing persulfate to degrade pollutants in water |
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Application publication date: 20200911 |