CN114146720A - photo-Fenton catalyst for degrading organic matters in wastewater and application thereof - Google Patents
photo-Fenton catalyst for degrading organic matters in wastewater and application thereof Download PDFInfo
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- CN114146720A CN114146720A CN202111394662.8A CN202111394662A CN114146720A CN 114146720 A CN114146720 A CN 114146720A CN 202111394662 A CN202111394662 A CN 202111394662A CN 114146720 A CN114146720 A CN 114146720A
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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
- B01J27/00—Catalysts comprising the elements or compounds of halogens, sulfur, selenium, tellurium, phosphorus or nitrogen; Catalysts comprising carbon compounds
- B01J27/24—Nitrogen compounds
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- 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
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- 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
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- 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
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- 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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2209/00—Controlling or monitoring parameters in water treatment
- C02F2209/06—Controlling or monitoring parameters in water treatment pH
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
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- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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- 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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Abstract
The invention relates to the field of photo-Fenton catalytic oxidation, and particularly discloses a photo-Fenton catalyst for degrading organic matters in wastewater and application thereof. The photo-Fenton catalyst for degrading organic matters in wastewater is characterized in that: the photo-Fenton catalyst is metal magnesium doped graphite phase nitrogen carbide, and the appearance of the photo-Fenton catalyst is a two-dimensional nanosheet. The photo-Fenton catalyst can degrade methylene blue and/or tetracycline hydrochloride in wastewater, can be degraded under the irradiation of visible light and at room temperature, and has the advantages of mild reaction conditions, low cost and easy realization.
Description
Technical Field
The invention relates to the field of photo-Fenton catalytic oxidation, in particular to a photo-Fenton catalyst for degrading organic matters in wastewater and application thereof.
Background
The traditional Fenton oxidation system has higher oxidative degradation capability on organic pollutants and is widely applied. However, the reaction must be carried out under an acidic condition, and secondary pollution caused by the generation of a large amount of iron mud seriously restricts the further development of the reaction. The Fenton-like system can better replace a Fenton system. Among these fenton-like catalysts, light fenton-like catalysts are attracting attention as a light fenton-like catalyst that works in visible light (or ultraviolet light) to significantly improve its catalytic degradation performance. However, the existing photo-Fenton catalyst basically contains toxic transition metals, and the popularization and the application of the photo-Fenton catalyst are restricted due to higher use cost and potential loss of the transition metals. The development of efficient and environment-friendly photo-Fenton catalyst is one of the future development directions of Fenton system.
As a semiconductor material responding to visible light, graphite phase nitrogen carbide has good application prospect due to excellent physicochemical property, adjustable photoelectric property, low price and environmental friendliness. The transition metal elements (such as iron, copper and manganese) are doped into the graphite phase nitrogen carbide framework, so that a good photo-Fenton oxidation effect can be obtained. This is because the strong force between the lone pair of nitrogen atoms in the heptazine ring and the metal atom can improve the photo-fenton oxidation ability and reduce the loss of transition metal. In the photo-fenton process, the main active component is hydroxyl radical (. OH), and since the life of the.oh is short, the amount of hydrogen peroxide used in the system is high. Considering the harm caused by the loss of transition metal elements in the catalytic process and the use of more hydrogen peroxide in the catalytic system, the graphite-phase nitrogen carbide photo-Fenton catalyst doped with metal elements, which is low in development cost and environment-friendly, has a good application prospect.
Ge et al in J.Mater.chem.A. 6(2018) 16421-16429: the compound of graphite phase nitrogen carbide and magnesium oxide has a good effect on organic matter degradation in Fenton-like reaction, but the photo-Fenton effect is lower than that of Fenton-like reaction under dark conditions, and the catalytic reaction active component is OH. In addition, some researchers find that magnesium-doped graphite-phase nitrogen carbide has better capability of degrading organic matters through photocatalysis.
Disclosure of Invention
The invention provides a photo-Fenton catalyst for degrading organic matters in wastewater, which has visible light response, low cost, high degradation efficiency and good stability and an application thereof in order to make up for the defects of the prior art.
The invention is realized by the following technical scheme:
the photo-Fenton catalyst for degrading organic matters in wastewater is characterized in that: the photo-Fenton catalyst is metal magnesium doped graphite phase nitrogen carbide, the appearance of the photo-Fenton catalyst is a two-dimensional nanosheet, and the appearance of the photo-Fenton catalyst is doped with magnesium ions, so that the photo-Fenton catalyst has the best catalytic effect.
Preferably, in the photo-Fenton catalyst, the mass fraction of the magnesium element is 0.1-2.0%, and the balance is graphite phase nitrogen carbide.
The application of the photo-Fenton catalyst in degrading methylene blue and tetracycline hydrochloride in wastewater comprises the following specific steps: adding the photo-Fenton catalyst and hydrogen peroxide into wastewater containing methylene blue and/or tetracycline hydrochloride, stirring and reacting for 0.2-2h under the irradiation of a light source with the wavelength of 420-800nm, and filtering the catalyst.
Preferably, the dye content in the wastewater is 5-100mg/L, and the adding amount of the catalyst meets 0.5-1.5g of catalyst per 1L of wastewater, and further preferably 0.8-1.2g of catalyst per 1L of wastewater; the concentration of hydrogen peroxide in the wastewater is 10-70mM, and more preferably 30-50 mM; the pH value of the waste water is 2-12, and the preferable range is 3-10; the stirring reaction is carried out at room temperature, and the reaction time is 0.2-1 h.
The invention is a photo-Fenton catalyst of graphite-phase nitrogen carbide doped with metal magnesium, the metal magnesium is doped in the graphite-phase nitrogen carbide, and the loss of metal Mg can be well inhibited by the Mg-N bond formed by the lone electron pair of nitrogen in the heptazine ring and the metal magnesium, so that the stability of the catalyst is improved; in addition, the metal magnesium is alkaline earth metal, not transition metal, and the loss of metal elements in the catalytic process can not cause toxic heavy metal pollution.
Finally, the lone electron pair of nitrogen in the heptazine ring forms with magnesium metalThe Mg-N bond can improve the decomposition of hydrogen peroxide into active component singlet oxygen1O2) Due to the fact that1O2The service life of the catalyst is far longer than that of OH, so that the consumption of hydrogen peroxide is obviously reduced.
The photo-Fenton catalyst can degrade methylene blue and/or tetracycline hydrochloride in wastewater, can be degraded under the irradiation of visible light and at room temperature, and has the advantages of mild reaction conditions, low cost and easy realization; in addition, the photo-Fenton catalyst is easy to regenerate and use, and has good photo-catalytic performance after being regenerated for many times.
Drawings
The invention will be further described with reference to the accompanying drawings.
FIG. 1 is a trapping experiment of an active component of the photo-Fenton catalyst used in example 1;
FIG. 2 is an XPS plot of the O element of the catalyst before it was operated in example 3;
FIG. 3 is an XPS plot of the Mg element of the catalyst before it was operated in example 3;
FIG. 4 is an XPS plot of the Mg element of the catalyst after four recycles in example 3;
figure 5 is an XRD pattern of the catalyst before non-operation and after four recycles of example 3.
Detailed Description
The present invention will be described in further detail with reference to specific embodiments, but these examples are only illustrative and do not limit the scope of the present invention.
Example 1:
evaluation conditions were as follows: in 40mg/L organic wastewater containing methylene blue, the adding mass of a catalyst is 1.0g/L calculated by the volume of the organic wastewater, the mass fraction of magnesium element in the catalyst is 0.8%, the concentration of hydrogen peroxide in the wastewater is 40mM, the pH value of the wastewater is 7, the wastewater is stirred and reacted at room temperature under the irradiation of a light source with the wavelength of 420-800nm, the reaction time of the photo-Fenton catalytic oxidation is 0.5 hour, and the catalyst is removed by filtration, so that the water body after the methylene blue is removed by degradation is obtained.
The results show that: in the embodiment, the degradation rate of the magnesium-doped graphite-phase nitrogen carbide on methylene blue is 99.9%. In the process of degrading 40mg/L wastewater containing methylene blue, the catalyst needs 40mM hydrogen peroxide; the graphite phase carbon nitride doped with Cu-C needs 400mM hydrogen peroxide [ Applied Surface science.488(2019)728-738] when degrading wastewater with the same concentration; while the graphite phase carbon nitrogen doped with Fe needs 160mM hydrogen peroxide [ Molecular catalysis.435(2017) 156-165 ] for degrading wastewater with the same concentration. This indicates that the amount of hydrogen peroxide used in the present application is much lower than the reported transition metal doped graphite phase nitrogen carbide.
As can be seen from FIG. 1, the catalyst can degrade 99,9% in 0.5 hour without addition of the scavenger, while IPA (isopropyl alcohol, test. OH), TEA (triethanolamine, test. O) are added2 −），N2(Nitrogen, detection h)+) And L-histidine (L-histidine, assay1O2) The photo-fenton effect decreases. The addition of L-histidine resulted in the least photo-Fenton effect, indicating that singlet oxygen: (1O2) Is the main active component in the photo-Fenton system. This is also the reason why this type of catalyst consumes a smaller amount of hydrogen peroxide.
Example 2:
evaluation conditions were as follows: in 40mg/L organic wastewater containing methylene blue, the adding mass of a catalyst is 1.2g/L calculated by the volume of the organic wastewater, the mass fraction of magnesium element in the catalyst is 0.1%, the concentration of hydrogen peroxide in the wastewater is 50mM, the pH value of the wastewater is 10, the wastewater is stirred and reacted at room temperature under the irradiation of a light source with the wavelength of 420-600 nm, the reaction time of the photo-Fenton catalytic oxidation is 1 hour, and the catalyst is filtered and removed, so that the water body after the methylene blue is degraded and removed is obtained.
The results show that: in the embodiment, the degradation rate of the magnesium-doped graphite-phase nitrogen carbide on methylene blue is 99.4%.
Example 3:
evaluation conditions were as follows: in 40mg/L organic wastewater containing methylene blue, the adding mass of a catalyst is 0.8g/L in terms of the volume of the organic wastewater, the mass fraction of magnesium element in the catalyst is 2.0%, the concentration of hydrogen peroxide in the wastewater is 30mM, the pH value of the wastewater is 3, the wastewater is stirred and reacts at room temperature under the irradiation of a light source with the wavelength of 500-800 nm, the reaction time of the photo-Fenton catalytic oxidation is 0.2 h, and the catalyst is removed by filtration, so that the water body after the methylene blue is removed by degradation is obtained.
Regeneration conditions are as follows: after the completion of the photo-Fenton catalytic oxidation reaction, the catalyst precipitate was washed with deionized water and ethanol in sequence several times, and the obtained precipitate was dried at 80 ℃ for 4 hours.
The results show that: the magnesium-doped graphite-phase nitrogen carbide of the embodiment has very good catalytic performance after being recycled for four times. The test results are as follows: the catalyst is used for the first time, the degradation rate of methylene blue is 99.5%, the catalyst is recycled for the first time, the degradation rate of the methylene blue is 99.3%, the catalyst is recycled for the second time, the degradation rate of the methylene blue is 99.1%, the catalyst is recycled for the third time, the degradation rate of the methylene blue is 99.0%, and the degradation rate of the methylene blue is 98.8% after the catalyst is recycled for the fourth time.
As shown in the attached FIG. 2, the O element of the catalyst before the operation has two peaks at 531.6eV and 532.8eV, which are respectively the H adsorbed by the catalyst2O and hydroxyl groups. In addition, no peak was observed at 529.7eV, indicating the absence of magnesium oxide in the catalyst.
As can be seen from FIG. 3, the Mg element of the catalyst before the operation has a peak at 1303.9eV, which indicates the presence of the N-Mg bond. From a review of fig. 2 and 3, it can be determined that Mg is doped in the graphite phase nitrogen carbide backbone, rather than a composite of magnesium oxide and graphite phase nitrogen carbide.
As can be seen from FIG. 4, the Mg element of the catalyst had a peak at 1303.9eV after four times of recycling, and the magnesium component remained in the catalyst structure after four times of recycling.
FIG. 5 is an XRD pattern of the catalyst before non-operation and after four repetitions in this example, from which it can be seen that the catalyst still maintains a good structure after four repetitions.
Example 4:
evaluation conditions were as follows: in 40mg/L of tetracycline hydrochloride-containing organic wastewater, the adding mass of the catalyst is 1.0g/L calculated by the volume of the organic wastewater, the mass fraction of magnesium element in the catalyst is 0.8%, the concentration of hydrogen peroxide in the wastewater is 40mM, the pH value of the wastewater is 7, the wastewater is stirred and reacted at room temperature under the irradiation of a light source with the wavelength of 420-800nm, the reaction time of the photo-Fenton catalytic oxidation is 0.5 h, and the catalyst is removed by filtration to obtain the water body after the tetracycline hydrochloride is degraded and removed.
The results show that: in the embodiment, the degradation rate of magnesium-doped graphite-phase nitrogen carbide on tetracycline hydrochloride is 98.2%.
Example 5:
evaluation conditions were as follows: in 20mg/L tetracycline hydrochloride-containing and 20mg/L methylene blue-containing organic wastewater, the adding mass of the catalyst is 1.0g/L calculated by the volume of the organic wastewater, the mass fraction of magnesium element in the catalyst is 0.8%, the concentration of hydrogen peroxide in the wastewater is 40mM, the pH value of the wastewater is 7, the reaction is stirred at room temperature under the irradiation of a light source with the wavelength of 420-800nm, the reaction time is 0.5 hour, and the catalyst is removed by filtration, so that the water body from which the tetracycline hydrochloride and the methylene blue are degraded is obtained.
The results show that: in the embodiment, the degradation rate of magnesium-doped graphite-phase nitrogen carbide on tetracycline hydrochloride is 98.7%, and the degradation rate on methylene blue is 99.7%.
The above description is only for the purpose of illustrating the preferred embodiments of the present invention and is not to be construed as limiting the invention, and any modifications, equivalents, improvements and the like that are within the spirit and principle of the present invention are intended to be included in the scope of the present invention.
Claims (9)
1. The photo-Fenton catalyst for degrading organic matters in wastewater is characterized in that: the photo-Fenton catalyst is metal magnesium doped graphite phase nitrogen carbide, and the appearance of the photo-Fenton catalyst is a two-dimensional nanosheet.
2. The photo-Fenton catalyst for degrading organic substances in wastewater according to claim 1, wherein: in the photo-Fenton catalyst, the mass fraction of magnesium element is 0.1-2.0%, and the balance is graphite phase nitrogen carbide.
3. The use of the photo-Fenton catalyst according to claim 1 for degrading methylene blue and tetracycline hydrochloride in wastewater.
4. Use according to claim 3, characterized in that: adding the photo-Fenton catalyst and hydrogen peroxide into wastewater containing methylene blue and/or tetracycline hydrochloride, stirring and reacting for 0.2-2h under the irradiation of a light source with the wavelength of 420-800nm, and filtering the catalyst.
5. The use of claim 4, wherein: in the wastewater, the dye content is 5-100mg/L, the addition amount of the catalyst meets 0.5-1.5g of the catalyst per 1L of the wastewater, and the concentration of hydrogen peroxide in the wastewater is 10-70 mM.
6. The use of claim 4, wherein: the pH value of the wastewater is 2-12.
7. The use of claim 4, wherein: the stirring reaction is carried out at room temperature, and the reaction time is 0.2-1 h.
8. The use of claim 5, wherein: the addition amount of the catalyst meets 0.8-1.2g of catalyst per 1L of wastewater, and the concentration of hydrogen peroxide in the wastewater is 30-50 mM.
9. The use of claim 6, wherein: the pH value of the wastewater is 3-10.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114768808A (en) * | 2022-05-27 | 2022-07-22 | 重庆理工大学 | Preparation method and application of carbon quantum dot doped iron-based oxide photo-Fenton catalyst |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106492870A (en) * | 2016-10-17 | 2017-03-15 | 阜阳师范学院 | A kind of photochemical catalyst of doped metallic oxide and preparation method thereof |
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- 2021-11-23 CN CN202111394662.8A patent/CN114146720A/en active Pending
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106492870A (en) * | 2016-10-17 | 2017-03-15 | 阜阳师范学院 | A kind of photochemical catalyst of doped metallic oxide and preparation method thereof |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN114768808A (en) * | 2022-05-27 | 2022-07-22 | 重庆理工大学 | Preparation method and application of carbon quantum dot doped iron-based oxide photo-Fenton catalyst |
| CN114768808B (en) * | 2022-05-27 | 2023-12-08 | 重庆理工大学 | Preparation method and application of carbon quantum dot doped iron-based oxide photo-Fenton catalyst |
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