CN109589995B - Catalyst for rapidly degrading organic pollutants in wastewater and use method thereof - Google Patents
Catalyst for rapidly degrading organic pollutants in wastewater and use method thereof Download PDFInfo
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- CN109589995B CN109589995B CN201910060048.4A CN201910060048A CN109589995B CN 109589995 B CN109589995 B CN 109589995B CN 201910060048 A CN201910060048 A CN 201910060048A CN 109589995 B CN109589995 B CN 109589995B
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- 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
- B01J27/053—Sulfates
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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
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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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Abstract
The invention relates to the technical field of organic wastewater treatment, and particularly discloses a catalyst for rapidly degrading organic pollutants in wastewater and a use method thereof. The catalyst comprises Fe2+、H2O2And a pH adjuster, said Fe2+And H2O2The molar ratio is 0.25-0.83: 1, the pH regulator is used for regulating the pH of a wastewater system to 5-9. The catalyst for fast degrading organic pollutant, Fe2+And H2O2Simultaneously generating a plurality of homogeneous phase and heterogeneous phase Fenton catalytic reaction active centers in situ in a reaction system, efficiently generating a large amount of hydroxyl free radicals under near-neutral pH, and carrying out oxidative degradation on organic pollutants in a short time. The defects that the traditional homogeneous Fenton system needs acidic pH condition and is easy to generate a large amount of iron-containing sludge are overcome; the method gets rid of the limitation of reaction implementation conditions, and can achieve ideal degradation effect under the conditions of dark state, natural light or other light source illumination.
Description
Technical Field
The invention relates to the technical field of organic wastewater treatment, in particular to a catalyst for rapidly degrading organic pollutants in wastewater and a using method thereof.
Background
In recent years, rapid development of chemical industry has led to continuous increase in discharge of industrial wastewater, of which pesticides and printing and dyeing wastewater are one of the major harmful industrial wastewater. The wastewater has the characteristics of complex components, high Chemical Oxygen Demand (COD) and large discharge. From the current research, the Fe2+And H2O2The constructed homogeneous Fenton system can rapidly generate hydroxyl free radicals (OH) with strong oxidizing property in the system, can be used for degrading various persistent organic matters, particularly aromatic compounds and some heterocyclic compounds of which common reagents are difficult to degrade, and has wide application prospect in wastewater treatment. The homogeneous Fenton system has the characteristics of high reaction rate, low cost and capability of meeting the treatment requirement in a short time, and has practical application value, but the system also has two defects to limit the practical application of the system, firstly, the reaction needs to be carried out under acidic pH (2-4), and the generation efficiency of hydroxyl radicals is greatly reduced along with the increase of the pH; secondly, iron ion loss is caused, and after the reactionIron-containing sludge is generated, and secondary pollution is easily caused.
Based on the above problems, various iron oxides such as alpha-FeOOH, gamma-FeOOH, alpha-Fe are derived2O3、γ-Fe2O3And Fe3O4Etc. and H2O2The constructed out-of-phase Fenton system can be used for degrading organic pollutants because the iron oxide can catalyze and decompose hydrogen peroxide to generate hydroxyl radicals. Compared with a homogeneous Fenton system, the heterogeneous Fenton system overcomes the defect that the homogeneous Fenton system generates iron-containing sludge, but most research results show that the heterogeneous Fenton system still needs to show a good effect under an acidic environment, and simultaneously can cause the leaching of iron ions, and the complete degradation time is far longer than that of the homogeneous Fenton system. Therefore, in order to improve the degradation efficiency of organic wastewater, photo-Fenton, electro-Fenton and other transition metal ions and H are developed on the basis of the original Fenton reaction2O2The constructed Fenton system is a novel advanced oxidation technology. However, the implementation of these fenton techniques either requires special equipment, or requires ultrasound, or requires ultraviolet irradiation, and is not suitable for large-scale and large-scale wastewater treatment.
Disclosure of Invention
Aiming at the problems of secondary pollution caused by iron-containing sludge easily generated, long degradation time, harsh implementation conditions and the like in the prior Fenton technology, the invention provides a catalyst for rapidly degrading organic pollutants and a use method thereof.
In order to achieve the purpose of the invention, the embodiment of the invention adopts the following technical scheme:
a catalyst for quickly degradating the organic pollutants in sewage contains Fe2+、H2O2And a pH adjuster, said Fe2+And H2O2The molar ratio is 0.25-0.83: 1, the pH regulator is used for regulating the pH of a wastewater system to 5-9.
Further, said Fe2+Is water soluble ferrous ion salt.
Further, the water-soluble ferrous ion salt is one of ferrous sulfate, ferrous chloride or steel pickling waste liquid.
Further, the pH regulator is one of sodium hydroxide, ammonia water or industrial waste alkali.
Compared with the prior art, the catalyst for rapidly degrading organic pollutants, Fe provided by the invention2+Dripping with pH regulator to maintain pH of the reaction system at 5-9, and adding Fe under near neutral pH condition2+And H2O2A plurality of homogeneous phase and heterogeneous phase Fenton catalytic reaction active centers are simultaneously generated in situ in a reaction system, and a large amount of hydroxyl free radicals are continuously and efficiently generated under the synergistic effect of the plurality of Fenton catalytic reaction active centers, so that organic pollutants are oxidized and degraded in a short time. The defects that the traditional homogeneous Fenton system needs acidic pH condition and is easy to generate a large amount of iron-containing sludge are overcome; the method gets rid of the limitation of reaction implementation conditions, does not need illumination assistance, does not need to use a light source with high price and high power, and can achieve ideal degradation effect under the illumination conditions of dark state, natural light or other light sources.
The invention also provides a using method of the catalyst, and the catalyst H is prepared by reacting2O2Adding into wastewater containing organic pollutants, and simultaneously adding Fe2+And pH regulator, and the pH of the waste water is controlled to be 5-9 in the adding process for degradation treatment.
Specifically, a homogeneous Fenton catalytic reaction active center and a heterogeneous Fenton catalytic reaction active center are formed in the degradation treatment process, and a large amount of hydroxyl radicals are efficiently generated at a near-neutral pH value to degrade organic pollutants. Wherein the active center of the homogeneous Fenton catalytic reaction is Fe2+、FeOH+、Fe3+、Fe(OH)2-Or Fe (OH)2 -With H2O2The reaction system formed; the heterogeneous Fenton catalytic reaction active center is Fe (OH)2Fh (hydrated iron oxide), gamma-FeOOH, alpha-FeOOH, FeII/Fh、FeIIgamma-FeOOH or FeIIH and at least one of/alpha-FeOOH2O2Reaction system formed, FeII/Fh、FeIIgamma-FeOOH and FeIIthe/alpha-FeOOH is combined through adsorption, and has stronger catalytic effect。
Further, after the degradation reaction is finished, the Fe element in the system is converted into alpha-Fe by adopting a liquid phase catalytic phase conversion process2O3alpha-FeOOH or Fe3O4The obtained iron oxide can be used for recycling heterogeneous Fenton-like catalysts, and can be used as a pigment because the chroma value of the iron oxide reaches the national standard of the pigment.
Furthermore, the wastewater after degradation treatment is wastewater containing 0-5000mg/L of single or mixed organic pollutants, and Fe can be properly adjusted according to the concentration of the pollutants2+And H2O2The dosage of the compound has high degradation efficiency on single or mixed pollutants with different concentrations.
Compared with the prior art, the application method of the catalyst for rapidly degrading organic pollutants in wastewater provided by the invention is characterized in that Fe is added2+Adding the pH regulator in a cocurrent manner and maintaining the pH of the reaction system to be nearly neutral by controlling the dropping speed, and adding H in advance2O2The waste water system in situ simultaneously generate multiple homogeneous phases and heterogeneous fenton catalytic reaction active centers, multiple fenton systems have the synergistic effect simultaneously, continuously produce the hydroxyl free radical of strong oxidizing property, and organic pollutant is degraded in quick oxidation, easy operation, the reaction is rapid, green.
Drawings
In order to more clearly illustrate the technical solutions in the embodiments of the present invention, the drawings needed to be used in the embodiments will be briefly described below, and it is obvious that the drawings in the following description are only some embodiments of the present invention, and it is obvious for those skilled in the art that other drawings can be obtained according to these drawings without creative efforts.
Fig. 1 is a comparison graph of the degradation of three pollutant mixtures of acid green 25, malachite green and cationic pink FG at different concentrations in the examples of the invention.
Detailed Description
In order to make the objects, technical solutions and advantages of the present invention more apparent, the present invention is further described in detail with reference to the following embodiments. It should be understood that the specific embodiments described herein are merely illustrative of the invention and are not intended to limit the invention.
Example 1
A catalyst for quickly degradating the organic pollutants in sewage contains Fe2+、H2O2And a pH adjuster, said Fe2+And H2O2The molar ratio is 0.25-0.83: 1, said Fe2+Selecting the concentration of 0.1 mol.L-1The ferrous sulfate solution of (1), the H2O2The concentration is 1 mol.L-1The pH regulator is selected to have a concentration of 1 mol.L-1The NaOH solution of (2) is used for adjusting the pH of the system to 5-9.
The method for rapidly degrading organic pollutants in wastewater by adopting the catalyst comprises the following steps:
(1) according to the raw material components of the above catalyst, the concentrations were respectively prepared to be 0.1 mol. L-1The ferrous sulfate solution has a concentration of 1 mol.L-1H of (A) to (B)2O2And a concentration of 1 mol. L-1NaOH solution of (2) and prepared to a concentration of 100 mg.L-1(about 100ppm) glyphosate solution as a wastewater sample;
(2) 0.5mL of H2O2Adding into 100mL glyphosate solution, adding 2.0mL 0.1mol L-1With 1 mol.L of ferrous sulfate solution-1And (3) dropwise adding the NaOH solution into the glyphosate solution at the same time, controlling the pH of the solution to be 5-9, carrying out degradation treatment until the ferrous sulfate solution is completely consumed, and finishing the reaction.
And filtering the reaction solution, taking supernatant, deriving the glyphosate by using a nitrosation method, and detecting the concentration of the glyphosate in the solution by adopting a pre-column derivation-reversed phase high performance liquid chromatography. The glyphosate degradation rate was calculated to be 94.59%.
By adopting the steps of the method, the concentration (10-5000mg/L) and H of the glyphosate are changed2O2(0.1-8.0mmol) and Fe2 +(0.04-6.0mmol) and degradation rate can reach more than 92% and mineralization rate can reach more than 62% by degradation experiments, and the results are shown in Table 1. Increase Fe properly2+And H2O2After the dosage of the glyphosate, the degradation rates of glyphosate with different concentrations (1000-.
TABLE 1 degradation rates of glyphosate at different concentrations versus Fe2+And H2O2Relation of dosage
TABLE 2 degradation rate and contaminant concentration of high concentration glyphosate, Fe2+And H2O2Relation of dosage
Example 2
A catalyst for quickly degradating the organic pollutants in sewage contains Fe2+、H2O2And a pH adjuster, said Fe2+And H2O2The molar ratio is 0.5: 1, said Fe2+Selecting the concentration of 0.1 mol.L-1The ferrous chloride solution of (1), the H2O2The concentration is 1 mol.L-1The pH regulator is selected to have a concentration of 1 mol.L-1The ammonia water of (2) is used for adjusting the pH value of the system to 5-9.
The method for rapidly degrading organic pollutants in wastewater by adopting the catalyst comprises the following steps:
(1) according to the raw material components of the above catalyst, the concentrations were respectively prepared to be 0.1 mol. L-1The ferrous chloride solution of (1 mol. L)-1H of (A) to (B)2O2And a concentration of 1 mol. L-1Preparing an orange G solution with the concentration of 200ppm as a wastewater sample;
(2) 0.4mL of H2O2Added to 100mL of orange G solution, and 2.0mL of 0.1 mol. L-1With 1 mol.L of ferrous chloride solution-1Adding ammonia water into orange G solution, controlling pH to 5-9, and performing degradation treatment until the solution is chlorinatedThe iron solution was consumed, the reaction was completed, and the degradation rate of orange G was calculated to be 99.59%.
Example 3
The method steps in example 1 were adopted to change the pollutants to acid green 25, mordant yellow 10, brilliant blue, phenol red, rhodamine B, malachite green, cationic pink FG, p-nitrophenol and 2,4, 6-trichlorophenol for degradation experiments, and the results are shown in Table 3, Fe2+And H2O2In a molar ratio of 0.25 to 0.83: 1, the degradation rate of pollutants with different structures exceeds 90 percent. Increase Fe properly2+And H2O2The degradation rate of the added amount of (3) can also be close to 100%.
TABLE 3 degradation rate and contaminant concentration of contaminants of different structures, Fe2+And H2O2Relation of dosage
Example 4
By adopting the method steps in example 1, the degradation experiment was performed by changing the pollutants into a mixture of acid green 25, malachite green and cationic pink FG, and the degradation rate and mineralization rate of the mixed pollutants with a total concentration of 300-1000ppm respectively reach more than 94% and 62%, and the results are shown in Table 4.
Table 4 degradation of three pollutant mixtures of acid green, malachite green and cationic pink FG
In order to directly illustrate the degradation effect of the invention on the mixture of acid green 25, malachite green and cationic pink FG, the appearance colors of the solution before and after degradation are compared, and the results are shown in figure 1, and the solutions with the concentrations of 150ppm, 400ppm, 700ppm and 1000ppm respectively become clear and transparent after degradation treatment, which indicates that the pollutants are effectively degraded.
Example 5
Degradation reactionAfter the reaction system in the embodiment 1-4 is finished, boiling reflux is respectively carried out for 1-2 hours, and the added iron ions are converted into the iron oxides with different crystal phases by using a liquid phase catalytic phase conversion method. Wherein, when Fe2+When the ion addition is less than 0.018mmol, the product is alpha-Fe at pH 5-92O3(ii) a When Fe2+The addition amount of the ions is between 0.02 and 0.025mmol, when the pH value is 5 to 7, the product is alpha-FeOOH, and when the pH value is 7 to 9, the product is alpha-Fe2O3And a mixture of alpha-FeOOH; when Fe2+When the addition amount of the ions is more than 0.05mmol, the products are all Fe within the pH range of 5-93O4。
From the above data, the catalyst, Fe, provided by the examples of the present invention2+And H2O2A plurality of homogeneous phase and heterogeneous phase Fenton catalytic reaction active centers are generated in situ in a reaction system, a large amount of hydroxyl free radicals are efficiently generated under the near-neutral pH, and single or mixed organic pollutants can be rapidly degraded. The ideal degradation effect can be achieved under the conditions of dark state, natural light or other light source illumination without illumination assistance. alpha-Fe obtained by liquid phase catalytic phase conversion method after degradation reaction2O3alpha-FeOOH or Fe3O4The iron oxide can be used for recycling the heterogeneous Fenton-like catalyst, so that resources are saved, and the cost is reduced.
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 or improvements made within the spirit and principle of the present invention should be included in the scope of the present invention.
Claims (6)
1. A use method of a catalyst for rapidly degrading organic pollutants in wastewater is characterized by comprising the following steps: the catalyst comprises Fe2+、H2O2And a pH adjuster, said Fe2+And H2O2The molar ratio is 0.25-0.83: 1, the pH regulator is used for regulating the pH of a wastewater system to 5-9;
the catalyst is used by reacting the H2O2Adding into wastewater containing organic pollutants, and simultaneously adding Fe2+And pH regulator, and the pH of the waste water is controlled to be 5-9 in the adding process for degradation treatment.
2. The method of using the catalyst for rapidly degrading organic pollutants in wastewater according to claim 1, wherein the method comprises the following steps: said Fe2+Is water soluble ferrous ion salt.
3. The method of using the catalyst for rapidly degrading organic pollutants in wastewater according to claim 2, wherein the method comprises the following steps: the water-soluble ferrous ion salt is one of ferrous sulfate, ferrous chloride or steel pickling waste liquid.
4. The method of using the catalyst for rapidly degrading organic pollutants in wastewater according to claim 1, wherein the method comprises the following steps: the pH regulator is one of sodium hydroxide, ammonia water or industrial waste alkali.
5. The method of using the catalyst for rapidly degrading organic pollutants in wastewater according to claim 1, wherein the method comprises the following steps: after the degradation reaction is finished, the Fe element in the system is converted into alpha-Fe by adopting a liquid phase catalytic phase conversion process2O3alpha-FeOOH or Fe3O4。
6. The method of using the catalyst for rapidly degrading organic pollutants in wastewater according to claim 1, wherein the method comprises the following steps: the wastewater after degradation treatment is wastewater containing 0-5000mg/L of single or mixed organic pollutants.
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| CN110302839A (en) * | 2019-07-11 | 2019-10-08 | 南京工业大学 | Photo-Fenton catalyst and preparation method and application thereof |
| CN112791562B (en) * | 2020-12-24 | 2022-09-27 | 广东环境保护工程职业学院 | System for ionic liquid absorbs and handles VOC with out-of-phase light fenton in coordination |
| CN115245834B (en) * | 2021-04-08 | 2024-02-23 | 浙江理工大学 | Efficient neutral heterogeneous Fenton catalyst FeOF and preparation method and application thereof |
| CN114669331A (en) * | 2022-04-02 | 2022-06-28 | 佛山市南海区苏科大环境研究院 | Fenton-like reagent type non-liquid catalyst and preparation method and application thereof |
| CN117865327B (en) * | 2024-03-11 | 2024-06-18 | 中国科学院大学 | Supergravity advanced oxidation wastewater treatment method |
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