CN110540321B - Fenton-like reagent and preparation method and application thereof - Google Patents
Fenton-like reagent and preparation method and application thereof Download PDFInfo
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- CN110540321B CN110540321B CN201910827967.XA CN201910827967A CN110540321B CN 110540321 B CN110540321 B CN 110540321B CN 201910827967 A CN201910827967 A CN 201910827967A CN 110540321 B CN110540321 B CN 110540321B
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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
- C02F1/66—Treatment of water, waste water, or sewage by neutralisation; pH adjustment
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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
- C02F1/72—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
- 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
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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
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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- Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W10/00—Technologies for wastewater treatment
- Y02W10/30—Wastewater or sewage treatment systems using renewable energies
- Y02W10/37—Wastewater or sewage treatment systems using renewable energies using solar energy
Abstract
The invention discloses a Fenton-like reagent and a preparation method and application thereof, the reagent adopts molybdenum oxide quantum dots and hydrogen peroxide as raw materials, the molybdenum oxide quantum dots replace metal salts such as iron salt and the like in the traditional Fenton reagent, the hydrogen peroxide is catalyzed to generate free radical, the free radical is oxidized and the organic pollutants are degraded, the problem that the subsequent treatment cost is high and difficult to be high due to the fact that metal salts such as iron salt, manganese salt and the like are easy to generate metal mud precipitate is solved by utilizing the reagent to degrade the organic pollutants, and the reaction efficiency and the utilization efficiency of the hydrogen peroxide are greatly improved. Meanwhile, the Fenton reagent has higher reactivity in a wider pH range, does not need an extreme acid environment, reduces the cost and prolongs the service life of equipment, so that the efficiency of degrading organic pollutants by the Fenton technology is improved, the treatment cost is reduced, the application range of the technology is expanded, and the Fenton reagent has a good application prospect.
Description
Technical Field
The invention relates to the technical field of material preparation, in particular to a Fenton-like reagent and a preparation method and application thereof.
Background
The Fenton technology is a technology which utilizes the strong oxidation capability of the reaction of ferrous ions and hydrogen peroxide and degrades organic matters without selective oxidation. As a typical representative of advanced oxidation technologies, fenton technology is widely used in oxidation treatment of organic wastewater in industries such as printing and dyeing.
Although the traditional Fenton technology has strong oxidation treatment capacity, the following defects still exist: 1) the decomposition efficiency level of the hydrogen peroxide is low, and a large amount of hydrogen peroxide or hydrogen peroxide is required to be added repeatedly, so that the reaction cost is high, equipment is seriously corroded due to excessive hydrogen peroxide, and the service life is influenced; 2) according to the condition of the to-be-degraded product, the concentration of ferrous ions is generally 18-410 mmol/L, the treatment cost is increased due to the addition of a large amount of ferric salt, and the generated iron mud generated by dissolving out a large amount of ferric ions is time-consuming and labor-consuming in the subsequent treatment process, so that secondary pollution is easily caused; 3) the traditional Fenton technology requires to be carried out under lower acidity, the pH value of the reaction is generally controlled to be 2-4, and in practical application, if the acidity of the wastewater does not reach the range, an acid reagent needs to be additionally added, so that the treatment cost is increased, and the equipment has certain corrosivity.
Therefore, the problem to be solved by the skilled in the art is how to provide a fenton-like reagent material with low cost, high activity, wide pH application range and good treatment effect.
Disclosure of Invention
In view of the above, the present invention provides a molybdenum oxide quantum dot-based fenton reagent without metal salt, a preparation method thereof, and a method for degrading organic pollutants using the same. The degradation cost of organic pollutants can be effectively reduced in a wide pH range, and the problem of secondary pollution caused by easy precipitation of metal salts such as iron salt, manganese salt and the like is solved.
In order to achieve the purpose, the invention adopts the following technical scheme:
the Fenton-like reagent is characterized by consisting of molybdenum oxide quantum dots and 30 wt% of hydrogen peroxide, wherein the mass-volume ratio of the molybdenum oxide quantum dots to the hydrogen peroxide is 0.33-40 mg/mL.
Preferably, the molybdenum oxide quantum dots are prepared by adopting the following process: a50 mL Erlenmeyer flask was charged with 10.0mg of molybdenum oxide powder, 6.0mL of H2And O and 4.0mL of 30% hydrogen peroxide, standing at room temperature for 30min, adjusting the pH value to 7.0 by using NaOH, and finally centrifuging at 8000rpm/min for 10min to remove precipitates, wherein the supernatant is the molybdenum oxide quantum dots.
The Fenton-like reagent provided by the invention is applied to organic wastewater treatment.
Preferably, the organic wastewater is azo organic polluted wastewater.
Preferably, the application of the fenton-like reagent comprises the following steps:
(1) adjusting the pH value of the organic wastewater, then adding molybdenum oxide quantum dots into the organic wastewater, and stirring and mixing uniformly;
(2) and (2) adding 30 wt% of hydrogen peroxide solution into the mixed solution obtained in the step (1) in proportion, and stirring while adding until the mixture is uniformly mixed.
Preferably, the pH value of the organic wastewater is adjusted to 4-12 in the step (1).
The beneficial effects of the preferred technical scheme are as follows: the Fenton-like reagent of the molybdenum oxide quantum dot component has a high catalytic effect in the pH range, so that the application range is effectively expanded, and the treatment cost is reduced.
Preferably, the amount of the molybdenum oxide quantum dots added in the step (1) is 10-100mg/L of the organic wastewater.
Further, the amount of the molybdenum oxide quantum dots added in the step (1) is 80mg/L of organic wastewater.
Preferably, the amount of the 30 wt% hydrogen peroxide added in the step (2) is 2.5-30mL/L of the organic wastewater.
Further, in the step (2), 30 wt% of hydrogen peroxide is added in an amount of 20mL/L of organic wastewater.
Through the scheme, compared with the prior art, the invention has the following beneficial effects:
compared with the traditional Fenton technology, the Fenton-like reagent does not need metal salts such as iron salt and the like, no iron mud is generated in the reaction process, and the subsequent treatment cost is greatly reduced; compared with the traditional Fenton technology, the dosage of hydrogen peroxide is reduced, and the corrosion to equipment is reduced to a certain extent while the reaction cost is reduced; the method widens the pH range of azo organic matter treatment to 4-12, and compared with the traditional Fenton reaction, the method has the advantages that the pH of pollutants must be adjusted to 2-4, so that the acid adjusting step is simplified, the cost is saved, and the corrosion of equipment is further reduced; the invention can realize high-efficiency degradation of azo organic pollution without the assistance of an ultraviolet light source, widens the application range of the azo organic pollution and has higher practical application significance.
Drawings
In order to more clearly illustrate the embodiments of the present invention or the technical solutions in the prior art, the drawings used in the description of the embodiments or the prior art will be briefly described below, it is obvious that the drawings in the following description are only embodiments of the present invention, and for those skilled in the art, other drawings can be obtained according to the provided drawings without creative efforts.
FIG. 1 is a graph showing the degradation spectrum of methyl orange by Fenton-like reagent according to the present invention;
FIG. 2 is a graph showing the effect of the concentration of molybdenum oxide quantum dots in the Fenton-like reagent on the removal rate of methyl orange.
Detailed Description
The technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the embodiments of the present invention, and it is obvious that the described embodiments are only a part of the embodiments of the present invention, and not all of the embodiments. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Preparing molybdenum oxide quantum dots:
the preparation method specifically comprises the following steps: a50 mL Erlenmeyer flask was charged with 10.0mg of molybdenum oxide powder, 6.0mL of H2And O and 4.0mL of 30% hydrogen peroxide, standing at room temperature for 30min, adjusting the pH value to 7.0 by using NaOH, and finally centrifuging at 8000rpm/min for 10min to remove precipitates, wherein the supernatant is the molybdenum oxide quantum dots.
Example 2
Adopting the molybdenum oxide quantum dots prepared in the example 1 and 30 wt% of hydrogen peroxide sold in the market as raw materials;
the following experiments are set up to prove that the Fenton-like reagent obtained by matching the molybdenum oxide quantum dots with the hydrogen peroxide has organic matter degradation performance:
a: 0.2mL of the 0.4g/L methyl orange dye solution to be treated was taken, 0.3mL of distilled water was added, and the pH was adjusted to neutral.
B, 0.2mL of 0.4g/L methyl orange dye solution to be treated, adjusting the pH value to be neutral, and then adding 1 muL of 30% hydrogen peroxide.
C, 0.2mL of 0.4g/L methyl orange dye solution to be treated, adjusting the pH value to be neutral, and then adding 40 mu L of 1mg/mL molybdenum oxide quantum dots.
And D, 0.2mL of 0.4g/L methyl orange dye solution to be treated, adjusting the pH value to be neutral, and then adding 40 mu L of 1mg/mL molybdenum oxide quantum dots and 1 mu L of 30% hydrogen peroxide.
The experimental result is shown in figure 1, when the hydrogen peroxide or the molybdenum oxide quantum dots are added into the methyl orange dye solution independently, the methyl orange dye can not be degraded basically. However, when both are added to the methyl orange dye solution, the methyl orange is degraded, as shown by the substantial disappearance of the characteristic absorption peak intensity of methyl orange near 465 nm. Meanwhile, the color of the solution can also be seen, when the hydrogen peroxide or the molybdenum oxide quantum dots and the methyl orange dye coexist, the color of the solution is consistent with that of the methyl orange, and the solution is orange; however, when both were present with methyl orange, the color of the solution faded and the solution was colorless.
Example 3
Determining the optimal addition amount of the molybdenum oxide quantum dots:
the following sets of control tests were performed, the contaminants were degraded after adding the reagents according to the following conditions, and the concentration was determined using an ultraviolet-visible spectrophotometer.
E: 0.2mL of methyl orange dye solution of 0.4g/L to be treated, adjusting the pH value to be neutral, and then adding 1 uL of 30% hydrogen peroxide.
F, 0.2mL of 0.4g/L methyl orange dye solution to be treated, adjusting the pH value to be neutral, and then adding 5 muL of 1mg/mL molybdenum oxide quantum dots and 1 muL of 30% hydrogen peroxide.
G, 0.2mL of 0.4G/L methyl orange dye solution to be treated, adjusting the pH value to be neutral, and then adding 10 muL of 1mg/mL molybdenum oxide quantum dots and 1 muL of 30% hydrogen peroxide.
H, 0.2mL of 0.4g/L methyl orange dye solution to be treated, adjusting the pH value to be neutral, and then adding 20 muL of 1mg/mL molybdenum oxide quantum dots and 1 muL of 30% hydrogen peroxide.
I, 0.2mL of 0.4g/L methyl orange dye solution to be treated, adjusting the pH value to be neutral, and then adding 30 muL of 1mg/mL molybdenum oxide quantum dots and 1 muL of 30% hydrogen peroxide.
J, 0.2mL of 0.4g/L methyl orange dye solution to be treated, adjusting the pH value to be neutral, and then adding 40 muL of 1mg/mL molybdenum oxide quantum dots and 1 muL of 30% hydrogen peroxide.
K, 0.2mL of 0.4g/L methyl orange dye solution to be treated, adjusting the pH value to be neutral, and then adding 60 muL of 1mg/mL molybdenum oxide quantum dots and 1 muL of 30% hydrogen peroxide.
L: 0.2mL of methyl orange dye solution of 0.4g/L to be treated, adjusting the pH value to be neutral, and then adding 80 muL of molybdenum oxide quantum dots of 1mg/mL and 1 muL of 30% hydrogen peroxide.
As shown in the attached figure 2, the removal rate of methyl orange is increased along with the increase of the dosage of the molybdenum oxide quantum dots, but when the concentration of the molybdenum oxide quantum dots is more than 80mg/L, the removal rate tends to be flat, so that the concentration of the molybdenum oxide quantum dots is limited to 10-100mg/L, the waste of raw materials is avoided, and the optimal treatment efficiency is ensured.
Example 4
Determining the optimal addition amount of hydrogen peroxide:
the following sets of control tests were performed, the contaminants were degraded after adding the reagents according to the following conditions, and the concentration was determined using an ultraviolet-visible spectrophotometer.
M: 0.2mL of 0.4g/L methyl orange dye solution to be treated, the pH was adjusted to neutral, and then 40. mu.L of 1mg/mL molybdenum oxide quantum dots were added.
L, 2mL of 0.4g/L methyl orange dye solution to be treated, adjusting the pH value to be neutral, and then adding 400 muL of 1mg/mL molybdenum oxide quantum dots and 5 muL of 30% hydrogen peroxide.
And N is 2mL of 0.4g/L methyl orange dye solution to be treated, the pH is adjusted to be neutral, and then 400 muL of 1mg/mL molybdenum oxide quantum dots and 10 muL of 30% hydrogen peroxide are added.
O, 2mL of 0.4g/L methyl orange dye solution to be treated, adjusting the pH value to be neutral, and then adding 400 mu L of 1mg/mL molybdenum oxide quantum dots and 15 mu L of 30% hydrogen peroxide.
P, 2mL of 1g/L methyl orange dye solution to be treated, adjusting the pH to be neutral, and then adding 400 uL of 1mg/mL molybdenum oxide quantum dots.
And Q, 2mL of 1g/L methyl orange dye solution to be treated, adjusting the pH value to be neutral, and then adding 400 muL of 1mg/mL molybdenum oxide quantum dots and 10 muL of 30% hydrogen peroxide.
And R, 2mL of 1g/L methyl orange dye solution to be treated, adjusting the pH value to be neutral, and then adding 400 muL of 1mg/mL molybdenum oxide quantum dots and 20 muL of 30% hydrogen peroxide.
S: 2mL of 1g/L methyl orange dye solution to be treated, adjusting the pH value to be neutral, and then adding 400 uL of 1mg/mL molybdenum oxide quantum dots and 40 uL of 30% hydrogen peroxide.
T: 2mL of 1g/L methyl orange dye solution to be treated, adjusting the pH value to be neutral, and then adding 400 mu L of 1mg/mL molybdenum oxide quantum dots and 60 mu L of 30% hydrogen peroxide.
The results of the experiment are shown in table 1 below:
TABLE 1 Effect of Hydrogen peroxide concentration on removal Rate
As can be seen from Table 1, when the concentration of methyl orange is small, the removal rate of methyl orange increases with the amount of hydrogen peroxide, and when the concentration of hydrogen peroxide reaches 5ml/L, the removal rate tends to be flat. However, when the methyl orange concentration is high and the hydrogen peroxide concentration is 5ml/L, the removal rate is low, and the amount of hydrogen peroxide to be used is further increased. When the amount of hydrogen peroxide was 20ml/L, the removal rate tended to be flat. Therefore, the amount of hydrogen peroxide added is closely related to the concentration of the organic contaminants, and in order to ensure the removal efficiency of the organic contaminants and avoid the waste of raw materials, the concentration of hydrogen peroxide is limited to 2.5 to 30ml/L in the present invention.
The embodiments in the present description are described in a progressive manner, each embodiment focuses on differences from other embodiments, and the same and similar parts among the embodiments are referred to each other. The device disclosed by the embodiment corresponds to the method disclosed by the embodiment, so that the description is simple, and the relevant points can be referred to the method part for description.
The previous description of the disclosed embodiments is provided to enable any person skilled in the art to make or use the present invention. Various modifications to these embodiments will be readily apparent to those skilled in the art, and the generic principles defined herein may be applied to other embodiments without departing from the spirit or scope of the invention. Thus, the present invention is not intended to be limited to the embodiments shown herein but is to be accorded the widest scope consistent with the principles and novel features disclosed herein.
Claims (9)
1. The application of the Fenton-like reagent in organic wastewater treatment is characterized in that the Fenton-like reagent is composed of molybdenum oxide quantum dots and 30 wt% of hydrogen peroxide, and the mass-volume ratio of the molybdenum oxide quantum dots to the hydrogen peroxide is 0.33-40 mg/mL.
2. The use of a fenton-like reagent according to claim 1 in organic wastewater treatment, wherein the molybdenum oxide quantum dots are prepared by the following process: in a 50mL Erlenmeyer flask was added 10.0mg of molybdenum oxide powder, 6.0mL of H2And O and 4.0mL of 30 wt% hydrogen peroxide, standing at room temperature for 30min, adjusting the pH value to 7.0 by using NaOH, and finally centrifuging at 8000rpm/min for 10min to remove precipitates, wherein the supernatant is the molybdenum oxide quantum dots.
3. Use of a fenton-like reagent according to claim 1, wherein the organic waste water is azo-based organic contaminated waste water.
4. Use of a fenton-like reagent according to any of claims 1-3, characterised in that it comprises the following steps:
(1) adjusting the pH value of the organic wastewater, then adding molybdenum oxide quantum dots into the organic wastewater, and stirring and mixing uniformly;
(2) and (2) adding 30 wt% of hydrogen peroxide solution into the mixed solution obtained in the step (1) in proportion, and stirring while adding until the mixture is uniformly mixed.
5. Use of a fenton's reagent according to claim 4, wherein the pH of the organic waste water is adjusted to 4-12 in step (1).
6. The use of a Fenton's reagent according to claim 4, wherein the amount of the molybdenum oxide quantum dots added in step (1) is 10-100mg/L of the organic wastewater.
7. The use of a Fenton's reagent according to claim 6, wherein the amount of molybdenum oxide quantum dots added in step (1) is 80mg/L of organic wastewater.
8. Use of a fenton's-like reagent according to claim 4, wherein the amount of 30 wt% hydrogen peroxide added in step (2) is 2.5-30mL/L of organic waste water.
9. Use of a fenton's reagent according to claim 8, wherein 30 wt% of the hydrogen peroxide is added in step (2) in an amount of 20mL/L of the organic waste water.
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