CN113231082A - High-activity iron-based-sulfide heterogeneous Fenton composite material and method for removing organic pollutants by using same - Google Patents
High-activity iron-based-sulfide heterogeneous Fenton composite material and method for removing organic pollutants by using same Download PDFInfo
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Abstract
The invention discloses a high-activity iron-based sulfide heterogeneous Fenton composite material and a method for removing organic pollutants by using the same, relates to the field of chemistry, and particularly relates to pollutant treatment. The method is characterized in that a high-activity iron-sulfide heterogeneous Fenton composite material is synthesized by a simple method, the removal benefit of the high-activity iron-sulfide heterogeneous Fenton composite material on pollutants is shown in that phenol is removed to 90-100% within 25 min under the condition that the pH = 3-9, and the corresponding phenol removal rate is more than 70% in a buffer solution with the pH = 6.86. The invention provides a method for constructing a high-activity iron-based-sulfide heterogeneous Fenton composite material for removing organic pollutants, which has higher degradation activity on the degradation of the organic pollutants under acidic and neutral conditions and provides possibility for treating wastewater under the neutral conditions.
Description
Technical Field
The present invention relates to the field of chemistry.
In particular to a high-activity iron-based sulfide heterogeneous Fenton composite material and a method for removing organic pollutants by using the same.
Background
With the rapid development of economy, the acceleration of industrialization pace, and the overuse of natural resources, the problem of water pollution has become a worldwide problem of widespread concern. In the refractory organic matter wastewater, phenol wastewater is taken as typical coal chemical wastewater, and if the wastewater is not treated, the wastewater is directly discharged into the environment, so that the wastewater can generate toxic action on all individuals in biospheres, and therefore, the treatment of the phenol wastewater has important significance for human survival and sustainable development of society. The Fenton technology has the characteristics of environmental friendliness, high efficiency, cleanness, economy, practicability and the like, so that the Fenton technology is more and more widely researched on environmental improvement. The heterogeneous Fenton technology is considered to degrade organic matters under a neutral condition, so that the development of a high-activity iron-based sulfide composite material for the heterogeneous Fenton reaction is particularly important. The pH limit is hopefully overcome by a heterogeneous Fenton reaction system, and the method has important scientific significance in the field of environmental pollution control.
Disclosure of Invention
The invention aims to overcome the defects of the traditional technology and provide a high-activity iron-based-sulfide heterogeneous Fenton composite material and a method for removing organic pollutants by using the same, which are used for treating the organic pollutants in the wastewater under a neutral condition so as to solve the problem of pollution in the wastewater.
The aim of the invention is achieved by the following technical measures:
the high-activity iron-sulfide heterogeneous Fenton composite material is characterized in that the construction method comprises the following steps:
step one, preparing a uniform sulfide solution;
step two, adding 1-1000 mg of iron-based heterogeneous Fenton material into the sulfide homogeneous solution obtained in the step one, and mechanically stirring for 1-600 minutes to obtain an iron-based heterogeneous Fenton material-sulfide mixed solution;
reacting the iron-based heterogeneous Fenton material-sulfide mixed solution at the temperature of 80-250 ℃ for 2-1000 hours;
and step four, after the reaction is finished and the reaction product is cooled, washing the reaction product for 1-100 times by using ultrapure water and ethanol, and drying the reaction product to obtain the high-activity iron-based sulfide heterogeneous Fenton composite material.
The high-activity iron-based-sulfide heterogeneous Fenton composite material is prepared by utilizing the chemical combination between the iron-based heterogeneous Fenton material and sulfide, and is used for removing organic pollutants under a neutral condition; the chemical combination between the iron-based heterogeneous Fenton material and the sulfide can construct an acidic microenvironment on the surface of the iron-based heterogeneous Fenton material, so that stable circulation of iron ions in a local microenvironment is guaranteed, and the pH limitation of Fenton reaction is overcome.
A specific optimization scheme is that the preparation method of the sulfide homogeneous solution comprises the following steps:
adding a molybdenum source and/or a tungsten source and/or a cadmium source and/or a cobalt source and/or a zinc source with the total amount of 1-1000 mg and a sulfur source with the total amount of 1-2000 mg into a beaker containing 10-100 mL of aqueous solution, carrying out ultrasonic treatment for 1-100 min, and stirring to obtain a uniform solution.
According to a specific optimization scheme, a molybdenum source is ammonium molybdate, sodium molybdate, molybdenum trioxide, molybdenum dioxide or molybdenum powder, a tungsten source is sodium tungstate, tungsten trioxide or tungsten chloride, a cadmium source is cadmium acetate, cadmium hydroxide or cadmium carbonate, a cobalt source is cobalt chloride, cobalt nitrate or cobalt acetate, a zinc source is zinc oxide, zinc sulfate, zinc acetate, zinc chloride or zinc nitrate, and a sulfur source is thioacetamide, thiourea, sulfur powder or sodium sulfide.
A specific optimization scheme is that the preparation method of the iron-based heterogeneous Fenton material-sulfide mixed solution comprises the following steps:
and (3) adding 1-1000 mg of the iron-based heterogeneous Fenton material into the sulfide uniform solution obtained in the step one, and mechanically stirring for 1-600 minutes to obtain the iron-based heterogeneous Fenton material-sulfide mixed solution.
According to a specific optimization scheme, the iron-based heterogeneous Fenton material is an iron-supported, iron sulfide, iron oxide, iron-based metal-organic framework or iron-based bimetallic magnetic spinel material.
A specific optimization scheme is characterized in that the iron-supported type is that an iron-based material is supported on an Al2O3 carrier, iron sulfide is ferric sulfide or ferrous sulfide, iron oxide is ferric oxide or ferroferric oxide, and the iron-based bimetal magnetic spinel material is cobalt ferrite, copper ferrite, manganese ferrite, zinc ferrite, sodium ferrite, calcium ferrite, lithium ferrite, nickel ferrite or bismuth ferrite.
A specific optimization scheme is characterized in that in the third step, the iron-based heterogeneous Fenton material-sulfide mixed solution is firstly transferred into a polytetrafluoroethylene lining of a high-pressure reaction kettle, then placed into the reaction kettle, and reacted for 2-1000 hours at the temperature of 80-250 ℃.
The method for removing the organic pollutants by using the high-activity iron-based sulfide heterogeneous Fenton composite material is characterized by comprising the following steps of:
a: selecting a phenol pollutant solution with the concentration of 1-2000 mg/L;
b: the high-activity iron-sulfide heterogeneous Fenton composite material is put into 100 mL of prepared wastewater, so that organic pollutants such as phenol and the like are removed.
According to a specific optimization scheme, 1-10000 mu L of hydrogen peroxide solution by weight percent is added in the step B to initiate reaction.
A specific optimization scheme is that the step B is stirred for reaction under the dark condition.
The adsorption-desorption balance of the pollutant on the surface of the catalyst can be achieved under the dark condition.
Due to the adoption of the technical scheme, compared with the prior art, the invention has the advantages that:
1. compared with a traditional wastewater treatment system, the method has the advantages that the environment-friendly, efficient and clean heterogeneous catalyst is added, so that the excellent effect of removing pollutants in wastewater under a neutral condition can be achieved;
2. through a chemical compounding mode, the iron-based heterogeneous Fenton material is chemically combined with the sulfide, and an acidic microenvironment can be constructed on the surface of the iron-based heterogeneous Fenton material, so that stable circulation of iron ions in a local microenvironment is ensured, the pH limit of Fenton reaction is overcome, and the effective removal of organic pollutant phenol in wastewater under a neutral condition is realized;
3. the catalyst added in the system is less in amount, the catalyst is magnetic, the recovery is convenient and simple, and the secondary pollution to the environment can be avoided.
The invention is further described with reference to the following figures and detailed description.
Drawings
FIG. 1 is a process route of the high activity Fe-based sulfide heterogeneous Fenton composite material constructed by the present invention;
fig. 2 is a graph showing the degradation of phenol according to the present invention under the conditions of initial pH =3, pH =4, pH =7, and pH = 9;
fig. 3 is a graph showing the degradation rate of phenol in a buffer at pH =6.86 for the catalyst prepared according to the present invention;
figure 4 is a bar graph of the degradation rate of the present invention for different simulated contaminants in a buffer system at pH = 6.86.
Detailed Description
Example 1: the construction method of the high-activity iron-sulfide heterogeneous Fenton composite material comprises the following steps:
step one, preparing a uniform sulfide solution;
step two, adding 1-1000 mg of iron-based heterogeneous Fenton material into the sulfide homogeneous solution obtained in the step one, and mechanically stirring for 1-600 minutes to obtain an iron-based heterogeneous Fenton material-sulfide mixed solution;
reacting the iron-based heterogeneous Fenton material-sulfide mixed solution at the temperature of 80-250 ℃ for 2-1000 hours;
and step four, after the reaction is finished and the reaction product is naturally cooled, washing the reaction product for 1-100 times by using ultrapure water and ethanol, and drying the reaction product to obtain the high-activity iron-sulfide heterogeneous Fenton composite material.
The high-activity iron-based-sulfide heterogeneous Fenton composite material is prepared by utilizing the chemical combination between the iron-based heterogeneous Fenton material and sulfide, and is used for removing organic pollutants under a neutral condition; the chemical combination between the iron-based heterogeneous Fenton material and the sulfide can construct an acidic microenvironment on the surface of the iron-based heterogeneous Fenton material, so that stable circulation of iron ions in a local microenvironment is guaranteed, and the pH limitation of Fenton reaction is overcome.
The preparation method of the sulfide homogeneous solution comprises the following steps:
one or more of a molybdenum source, a tungsten source, a cadmium source, a cobalt source and a zinc source, 1-1000 mg of the total amount of the molybdenum source, the tungsten source, the cadmium source, the cobalt source and the zinc source, and 1-2000 mg of the sulfur source are added into a beaker containing 10-100 mL of the aqueous solution, and after ultrasonic treatment for 1-100 min, the mixture is stirred for 1-600 min to obtain a uniform solution.
The molybdenum source is ammonium molybdate, sodium molybdate, molybdenum trioxide, molybdenum dioxide or molybdenum powder, the tungsten source is sodium tungstate, tungsten trioxide or tungsten chloride, the cadmium source is cadmium acetate, cadmium hydroxide or cadmium carbonate, the cobalt source is cobalt chloride, cobalt nitrate or cobalt acetate, the zinc source is zinc oxide, zinc sulfate, zinc acetate, zinc chloride or zinc nitrate, and the sulfur source is thioacetamide, thiourea, sulfur powder or sodium sulfide.
The iron-based heterogeneous Fenton material is an iron-supported type, iron sulfide, iron oxide, iron-based metal-organic framework or iron-based bimetallic magnetic spinel material.
The iron-supported type is that an iron-based material is supported on an Al2O3 carrier, the iron sulfide is iron sulfide or ferrous sulfide, the iron oxide is ferric oxide or ferroferric oxide, and the iron-based bimetal magnetic spinel material is cobalt ferrite, copper ferrite, manganese ferrite, zinc ferrite, sodium ferrite, calcium ferrite, lithium ferrite, nickel ferrite or bismuth ferrite.
And in the third step, the iron-based heterogeneous Fenton material-sulfide mixed solution is firstly transferred into a polytetrafluoroethylene lining of a high-pressure reaction kettle, then placed into the reaction kettle, and reacted for 2-1000 hours at the temperature of 80-250 ℃.
Example 3: the method for removing organic pollutants by using the high-activity iron-based sulfide heterogeneous Fenton composite material comprises the following steps of:
a: selecting a phenol pollutant solution with the concentration of 1-2000 mg/L;
b: the high-activity iron-sulfide heterogeneous Fenton composite material is put into 100 mL of prepared wastewater, so that organic pollutants such as phenol and the like are removed.
And C, adding 1-10000 mu L of hydrogen peroxide of 30 wt% into the step B to initiate reaction.
Step B the reaction was stirred under dark conditions.
Aiming at the effect of the high-activity iron-based-sulfide heterogeneous Fenton composite material on removing organic pollutants, three experiments are respectively as follows:
experiment one: degradation experiments were performed under the following conditions, setting initial pH =3, pH =4, pH =7, pH =9 for the solution.
100 mL of wastewater to be treated, the concentration of phenol is 20 mg/L, and the dosage of the high-activity iron-sulfide heterogeneous Fenton composite catalyst material is 30 mg.
The experimental result is shown in fig. 2, and the experiment shows that the dependence of the prepared high-activity iron-based-sulfide heterogeneous Fenton composite catalyst material on pH is reduced, the limitation of the traditional homogeneous Fenton reaction on pH is overcome, the phenol is efficiently degraded in the range of pH = 3-9, and the removal rate reaches 90-100% within 25 min.
Experiment two: the degradation experiment is carried out according to the following conditions, a standard buffer solution reagent with pH =6.86 is dissolved in a volumetric flask with 250 mL, the volume is determined by deionized water, the solution is shaken and dissolved to obtain a uniform buffer solution with pH =6.86,
the pH =6.86 buffer solution wastewater to be treated is 100 mL, the phenol concentration is 20 mg/L, and the dosage of the high-activity iron-sulfide heterogeneous Fenton composite catalyst material is 30 mg.
The experimental result is shown in fig. 3, and the experiment shows that the prepared high-activity iron-sulfide heterogeneous Fenton composite catalyst material also shows excellent activity in a buffer solution, the high-efficiency degradation of phenol is realized, and the removal rate in 24 h is more than 70%.
Experiment three: the degradation experiment was performed under the following conditions, where the pH =6.86 standard buffer reagent was dissolved in a 250 mL volumetric flask, and the volume was fixed with deionized water, and the solution was shaken to obtain a uniform pH =6.86 buffer solution, and the results were as follows:
(1) the pH =6.86 buffer solution wastewater to be treated has the enrofloxacin concentration of 20 mg/L and the dosage of the high-activity iron-based sulfide heterogeneous Fenton composite catalyst material of 30 mg;
(2) the pH =6.86 buffer solution wastewater to be treated has the tetracycline concentration of 20 mg/L and the dosage of the high-activity iron-based sulfide heterogeneous Fenton composite catalyst material of 30 mg;
(3) the concentration of norfloxacin in buffer solution wastewater to be treated is 20 mg/L, and the dosage of the high-activity iron-sulfide heterogeneous Fenton composite catalyst material is 30 mg;
(4) the pH =6.86 buffer solution wastewater to be treated has the concentration of 4-chlorophenol of 10 mg/L and the dosage of the high-activity iron-based-sulfide heterogeneous Fenton composite catalyst material of 30 mg;
(5) the pH =6.86 buffer solution wastewater to be treated has the bisphenol A concentration of 10 mg/L and the dosage of the high-activity iron-based sulfide heterogeneous Fenton composite catalyst material of 30 mg;
(6) the pH =6.86 buffer solution wastewater to be treated has the phenol concentration of 20 mg/L and the dosage of the high-activity iron-based sulfide heterogeneous Fenton composite catalyst material of 30 mg;
(7) the pH =6.86 buffer solution wastewater to be treated has the rhodamine B concentration of 20 mg/L and the dosage of the high-activity iron-based-sulfide heterogeneous Fenton composite catalyst material of 30 mg;
(8) the pH =6.86 buffer solution wastewater to be treated has the methylene blue concentration of 20 mg/L and the dosage of the high-activity iron-based sulfide heterogeneous Fenton composite catalyst material of 30 mg;
(9) the pH =6.86 buffer solution wastewater to be treated has a new carmine concentration of 20 mg/L and a high-activity iron-based sulfide heterogeneous Fenton composite catalyst material dosage of 30 mg;
the experimental result is shown in fig. 4, and the experiment shows that the prepared high-activity iron-based-sulfide heterogeneous Fenton composite catalyst material shows excellent activity on different pollutants such as antibiotics, phenols and dyes in a buffer solution, shows the universality of the prepared composite catalyst material on various pollutants, and shows the feasibility of practical application.
The foregoing shows and describes the general principles and broad features of the present invention and advantages thereof. It will be understood by those skilled in the art that the present invention is not limited to the embodiments described above, which are described in the specification and illustrated only to illustrate the principle of the present invention, but that various changes and modifications may be made therein without departing from the spirit and scope of the present invention, which fall within the scope of the invention as claimed. The scope of the invention is defined by the appended claims and equivalents thereof.
Claims (10)
1. The high-activity iron-sulfide heterogeneous Fenton composite material is characterized in that the construction method comprises the following steps:
step one, preparing a uniform sulfide solution;
step two, adding 1-1000 mg of iron-based heterogeneous Fenton material into the sulfide homogeneous solution obtained in the step one, and mechanically stirring for 1-600 minutes to obtain an iron-based heterogeneous Fenton material-sulfide mixed solution;
reacting the iron-based heterogeneous Fenton material-sulfide mixed solution at the temperature of 80-250 ℃ for 2-1000 hours;
and step four, after the reaction is finished and the reaction product is cooled, washing the reaction product for 1-100 times by using ultrapure water and ethanol, and drying the reaction product to obtain the high-activity iron-based sulfide heterogeneous Fenton composite material.
2. The preparation method of the high-activity iron-sulfide heterogeneous Fenton composite material is characterized by comprising the following steps of:
adding a molybdenum source and/or a tungsten source and/or a cadmium source and/or a cobalt source and/or a zinc source with the total amount of 1-1000 mg and a sulfur source with the total amount of 1-2000 mg into a beaker containing 10-100 mL of aqueous solution, carrying out ultrasonic treatment for 1-100 min, and stirring to obtain a uniform solution.
3. The highly active iron-based sulfide heterogeneous fenton composite according to claim 3, wherein: the molybdenum source is ammonium molybdate, sodium molybdate, molybdenum trioxide, molybdenum dioxide or molybdenum powder, the tungsten source is sodium tungstate, tungsten trioxide or tungsten chloride, the cadmium source is cadmium acetate, cadmium hydroxide or cadmium carbonate, the cobalt source is cobalt chloride, cobalt nitrate or cobalt acetate, the zinc source is zinc oxide, zinc sulfate, zinc acetate, zinc chloride or zinc nitrate, and the sulfur source is thioacetamide, thiourea, sulfur powder or sodium sulfide.
4. The high-activity iron-based-sulfide heterogeneous fenton composite material according to claim 1, wherein the preparation method of the iron-based heterogeneous fenton composite material-sulfide mixed solution comprises the following steps:
and (3) adding 1-1000 mg of the iron-based heterogeneous Fenton material into the sulfide uniform solution obtained in the step one, and mechanically stirring for 1-600 minutes to obtain the iron-based heterogeneous Fenton material-sulfide mixed solution.
5. The highly active iron-based sulfide heterogeneous Fenton's composite material according to claim 4, wherein: the iron-based heterogeneous Fenton material is an iron-supported type, iron sulfide, iron oxide, iron-based metal-organic framework or iron-based bimetallic magnetic spinel material.
6. The highly active iron-based sulfide heterogeneous fenton composite according to claim 5, wherein: the iron-loaded type is that iron-based material is loaded on Al2O3On the carrier, the iron sulfide is ferric sulfide or ferrous sulfide, the iron oxide is ferric oxide or ferroferric oxide, and the iron-based bimetallic magnetic spinel material is cobalt ferrite, copper ferrite, manganese ferrite, zinc ferrite, sodium ferrite, calcium ferrite, lithium ferrite, nickel ferrite or bismuth ferrite.
7. The highly active iron-based sulfide heterogeneous fenton composite according to claim 1, wherein: and in the third step, the iron-based heterogeneous Fenton material-sulfide mixed solution is firstly transferred into a polytetrafluoroethylene lining of a high-pressure reaction kettle, then placed into the reaction kettle, and reacted for 2-1000 hours at the temperature of 80-250 ℃.
8. The method for removing the organic pollutants by using the high-activity iron-based sulfide heterogeneous Fenton composite material is characterized by comprising the following steps of:
a: selecting a phenol pollutant solution with the concentration of 1-2000 mg/L;
b: the high-activity iron-sulfide heterogeneous Fenton composite material is put into 100 mL of prepared wastewater, so that organic pollutants such as phenol and the like are removed.
9. The method for removing organic pollutants with the high activity iron-based sulfide heterogeneous fenton composite material as claimed in claim 8, wherein: and C, adding 1-10000 mu L of hydrogen peroxide of 30 wt% into the step B to initiate reaction.
10. The method for removing organic pollutants with the high activity iron-based sulfide heterogeneous fenton composite material as claimed in claim 8, wherein: step B the reaction was stirred under dark conditions.
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| CN113996316A (en) * | 2021-11-24 | 2022-02-01 | 南京泽佑环保科技有限公司 | Granulation method of heterogeneous Fenton catalyst |
| CN114262068A (en) * | 2022-01-05 | 2022-04-01 | 烟台大学 | Photoelectric biological Fenton reactor, preparation process thereof and ribavirin wastewater treatment process |
| CN114797873A (en) * | 2022-05-11 | 2022-07-29 | 华东理工大学 | High-activity zinc-iron hydrotalcite heterogeneous Fenton material and method for removing organic pollutants by using same |
| CN115350711A (en) * | 2022-09-02 | 2022-11-18 | 济南大学 | Preparation method of ammonium polythiomolybdate/manganese ferrite persulfate catalyst |
| CN115518658A (en) * | 2022-09-20 | 2022-12-27 | 广州大学 | Preparation method and application of cluster spherical multiphase Fenton catalyst |
| CN116850990A (en) * | 2023-04-28 | 2023-10-10 | 重庆工商大学 | Microwave-assisted modified spinel/porous biochar catalyst for efficiently degrading organic pollutants |
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| CN114262068A (en) * | 2022-01-05 | 2022-04-01 | 烟台大学 | Photoelectric biological Fenton reactor, preparation process thereof and ribavirin wastewater treatment process |
| CN114797873A (en) * | 2022-05-11 | 2022-07-29 | 华东理工大学 | High-activity zinc-iron hydrotalcite heterogeneous Fenton material and method for removing organic pollutants by using same |
| CN115350711A (en) * | 2022-09-02 | 2022-11-18 | 济南大学 | Preparation method of ammonium polythiomolybdate/manganese ferrite persulfate catalyst |
| CN115350711B (en) * | 2022-09-02 | 2023-11-14 | 济南大学 | Preparation method of ammonium polythiomolybdate/manganese ferrite persulfate catalyst |
| 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 |
| CN116850990A (en) * | 2023-04-28 | 2023-10-10 | 重庆工商大学 | Microwave-assisted modified spinel/porous biochar catalyst for efficiently degrading organic pollutants |
| CN116850990B (en) * | 2023-04-28 | 2024-06-07 | 重庆工商大学 | Microwave-assisted modified spinel/porous biochar catalyst for efficiently degrading organic pollutants |
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