CN114797873A - High-activity zinc-iron hydrotalcite heterogeneous Fenton material and method for removing organic pollutants by using same - Google Patents
High-activity zinc-iron hydrotalcite heterogeneous Fenton material and method for removing organic pollutants by using same Download PDFInfo
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Abstract
The invention discloses a high-activity zinc-iron hydrotalcite heterogeneous Fenton material and a method for removing organic pollutants by using the same, and relates to organic pollutant treatment in the field of chemistry. The method is characterized in that a high-activity zinc-iron hydrotalcite heterogeneous Fenton material is synthesized by a simple method, the removal benefit of the material on pollutants is shown in that phenol is removed to 90-100% within 60min under the condition that the pH is = 3-11, and meanwhile, a reaction system can be quickly adjusted to be neutral. The total organic carbon removal rate in neutral actual wastewater can reach 64.4%, and deep mineralization can be realized. The invention provides a method for constructing a zinc-iron hydrotalcite heterogeneous Fenton material for removing organic pollutants, which has higher degradation activity on the degradation of the organic pollutants under acidic, neutral and alkaline conditions, and the Fenton degradation technology is extensively applied to the neutral and alkaline conditions.
Description
Technical Field
The invention relates to the field of chemistry, in particular to a high-activity zinc-iron hydrotalcite heterogeneous Fenton 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 system is considered to be capable of reacting under a neutral condition, and zinc oxide and zinc hydroxide which are common amphoteric compounds can effectively adjust the pH value, so that the pH limit range of the traditional Fenton technology can be effectively widened. Therefore, the development of the high-activity zinc-iron hydrotalcite material for the heterogeneous Fenton reaction is very important, the pH limit is expected to be really overcome, 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 zinc-iron hydrotalcite heterogeneous Fenton material which can really overcome the pH limitation and is used for widely treating organic pollutants in wastewater under acidic, neutral and alkaline conditions, thereby solving the pollution problem in the wastewater.
The aim of the invention is achieved by the following technical measures:
the high-activity zinc-iron hydrotalcite heterogeneous Fenton material is characterized in that: the zinc-iron hydrotalcite heterogeneous Fenton material is constructed by the following steps:
step one, preparing a zinc-iron ion solution;
slowly adding alkali liquor into the zinc-iron ion solution, and mechanically stirring the mixture until the mixture is uniform to obtain zinc-iron suspension;
step three, heating the zinc-iron suspension to a reaction temperature, and reacting at a constant temperature;
and step four, cooling the zinc-iron suspension after the reaction is finished, alternately washing the zinc-iron suspension by using ultrapure water and ethanol, washing until the supernatant is stable at neutrality, keeping the pH value unchanged after three times of washing, and drying to obtain the zinc-iron hydrotalcite heterogeneous Fenton material.
The constructed high-activity zinc-iron hydrotalcite heterogeneous Fenton material is used for removing organic pollutants through catalysis of a highly dispersed iron-based material; the chemical combination between the highly dispersed iron-based material and the zinc-based material can not only quickly adjust the pH value to be neutral, but also can construct a neutral microenvironment on the surface of the iron-based heterogeneous Fenton material, thereby ensuring the stable circulation of iron ions in a local microenvironment without loss, and further overcoming the pH limitation of the Fenton reaction.
A specific optimization scheme is provided, and the preparation method of the zinc-iron ion solution in the first step comprises the following steps:
adding 1-1000 parts by mass of an iron source and 1-2000 parts by mass of a zinc source into 10000-100000 parts by mass of an aqueous solution, carrying out ultrasonic treatment, uniformly mixing, and stirring until the iron source and the zinc source are completely dissolved to obtain a uniform solution.
According to a specific optimization scheme, the iron source is any one or a mixture of more of ferric chloride, ferrous chloride, ferric sulfate, ferrous sulfate, ferric nitrate, ferrous nitrate, ferric oxalate and ferrous oxalate, and the zinc source is any one or a mixture of more of zinc chloride, zinc sulfate, zinc nitrate and zinc oxalate.
A specific optimization scheme, wherein in the second step, the mass part ratio of the alkali liquor to the zinc-iron ion solution is 0.001-1: 10 to 100.
According to a specific optimization scheme, the alkali liquor is added into the zinc-iron ion solution and then mechanically stirred until the mixed solution is in a complete suspension state.
A specific optimization scheme is that the alkali liquor is one or more of sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium carbonate, sodium bicarbonate and ammonia water, and the concentration of the alkali liquor is 0.05-1 mol/L.
A specific optimization scheme is that in the third step, the zinc-iron suspension is heated to the reaction temperature of 20-100 ℃, and the reaction duration is 2-100 hours.
The method for removing organic pollutants by using the high-activity zinc-iron hydrotalcite heterogeneous Fenton material is characterized by comprising the following steps of: the method comprises the following steps:
step A: selecting an organic pollutant solution;
and B: the high-activity zinc-iron hydrotalcite heterogeneous Fenton material prepared in the claims 1 to 6 is put into an organic pollutant solution, stirred uniformly, and added with potassium hydrogen persulfate to initiate reaction, so as to remove the organic pollutants.
A specific optimization scheme is provided, wherein in the step B, the concentration of the potassium hydrogen persulfate is 42-46%, and the mass part ratio of the added potassium hydrogen persulfate to the organic pollutant solution is 1-1000: 10000.
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.
In a specific optimization scheme, the organic pollutants are any one or more of phenol, nitrobenzene, organic dye or antibiotics.
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 high-activity zinc-iron hydrotalcite heterogeneous Fenton material is an environment-friendly, efficient and clean heterogeneous catalyst, can really overcome the limitation of a pH value, and can achieve an excellent effect of removing pollutants in wastewater under neutral and alkaline conditions;
2. according to the high-activity zinc-iron hydrotalcite heterogeneous Fenton material, an iron-based material and a zinc-based material are chemically combined in a chemical compounding mode, and a neutral microenvironment can be constructed on the surface of the iron-based heterogeneous Fenton material, so that stable circulation and dissolution of iron ions in a local microenvironment are guaranteed, the pH limit of Fenton reaction is overcome, and organic pollutants such as phenol, nitrobenzene, organic dye or antibiotics and the like in waste water under a neutral alkaline condition are effectively removed;
3. the high-activity zinc-iron hydrotalcite heterogeneous Fenton material degradation system constructed by the method can realize effective treatment and deep mineralization of neutral actual wastewater.
The invention is further described with reference to the following figures and detailed description.
Drawings
Fig. 1 is a graph showing the degradation curve of the highly active zinc-iron hydrotalcite heterogeneous fenton material in the present invention on phenol under the conditions of initial pH =3, pH =5, pH =7, pH =9, and pH = 11.
Fig. 2 is a graph showing that the highly active zinc-iron hydrotalcite heterogeneous fenton material in the present invention degrades the pH change of phenol under the conditions of initial pH =3, pH =5, pH =7, pH =9, and pH = 11.
Fig. 3 is a graph comparing the total organic carbon removal rate of the high activity zinc-iron hydrotalcite heterogeneous fenton material of the present invention and other conventional catalysts for neutral actual wastewater.
FIG. 4 is a graph showing the change of chemical oxygen demand of neutral actual wastewater treated by the high-activity zinc-iron hydrotalcite heterogeneous Fenton material.
Fig. 5 is a graph comparing the degradation rate of the high-activity zinc-iron hydrotalcite heterogeneous fenton material in the invention for treating common organic pollutants.
Detailed Description
Example 1: the construction method of the high-activity zinc-iron hydrotalcite heterogeneous Fenton material comprises the following steps:
step one, preparing a zinc-iron ion solution;
slowly adding alkali liquor into the zinc-iron ion solution, and mechanically stirring the mixture until the mixture is uniform to obtain zinc-iron suspension;
step three, heating the zinc-iron suspension to a reaction temperature, and reacting at a constant temperature;
and step four, cooling the zinc-iron suspension after the reaction is finished, alternately washing the zinc-iron suspension by using ultrapure water and ethanol, washing until the supernatant is stable at neutrality, keeping the pH value unchanged after three times of washing, and drying to obtain the zinc-iron hydrotalcite heterogeneous Fenton material.
The constructed high-activity zinc-iron hydrotalcite heterogeneous Fenton material is used for removing organic pollutants through catalysis of a highly dispersed iron-based material; the chemical combination between the highly dispersed iron-based material and the zinc-based material can not only quickly adjust the pH value to be neutral, but also can construct a neutral microenvironment on the surface of the iron-based heterogeneous Fenton material, thereby ensuring the stable circulation of iron ions in a local microenvironment without loss, and further overcoming the pH limitation of the Fenton reaction.
The construction method of the high-activity zinc-iron hydrotalcite heterogeneous Fenton material in a laboratory comprises the following steps:
step one, preparing a zinc-iron ion solution;
the preparation method of the zinc-iron ion solution comprises the following steps:
adding 1-1000 mg of iron source and 1-2000 mg of zinc source into a beaker filled with 10-100 mL of aqueous solution, carrying out ultrasonic treatment for 1-100 min, mixing uniformly, and mechanically stirring by a stirrer until the iron source and the zinc source are completely dissolved without solids to obtain a uniform solution.
The iron source is any one or a mixture of a plurality of ferric chloride, ferrous chloride, ferric sulfate, ferrous sulfate, ferric nitrate, ferrous nitrate, ferric oxalate and ferrous oxalate, the zinc source is any one or a mixture of a plurality of zinc chloride, zinc sulfate, zinc nitrate and zinc oxalate, and the product effect is different under the condition that the iron source and the zinc source are mixed.
Step two, preparing a zinc-iron suspension solution, wherein the method comprises the following steps:
slowly adding 1-1000 mg of alkali liquor into the zinc-iron ion solution obtained in the step one, and mechanically stirring for 1-600 minutes to obtain a zinc-iron suspension solution. The time for mechanical stirring by a stirrer depends on the amount of zinc and iron ions used, and stirring is required to be carried out for at least 2min per mg of zinc and iron ions.
The alkali solution is one or more of sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium carbonate, sodium bicarbonate and ammonia water. The total concentration of the alkali liquor is 0.05-1 mol/L, and the pH value of the alkali liquor is different according to the alkali used.
And step three, transferring the zinc-iron suspension obtained in the step two to a flask, then placing the flask in an electric heating jacket, and reacting for 2-100 hours at the temperature of 20-100 ℃. The optimum temperature and time of different zinc sources and iron sources are different, and most of the optimum temperature and time are required to be between 40 and 80 ℃ and 10 to 40 hours.
And step four, after the reaction in the step three is finished, cooling, alternately washing for 2-100 times by using ultrapure water and ethanol, and drying to obtain the zinc-iron hydrotalcite heterogeneous Fenton material. The washing requirement is that the supernatant is stable at neutral, and the pH value does not change obviously within three times.
Example 2: the method for removing organic pollutants by using the high-activity zinc-iron hydrotalcite heterogeneous Fenton material prepared by the method comprises the following steps:
step A: selecting an organic pollutant solution;
and B: the high-activity zinc-iron hydrotalcite heterogeneous Fenton material is put into an organic pollutant solution, stirred uniformly, added with potassium hydrogen persulfate to initiate reaction, stirred to react under a dark condition, and removed of the organic pollutants.
The concentration of the organic pollutant solution is 1-1000 mg/L, the concentration of potassium hydrogen persulfate is 42-46%, and the mass part ratio of the added high-activity zinc-iron hydrotalcite heterogeneous Fenton material to the organic pollutant solution is 1-1000: 100000, the mass part ratio of the added potassium hydrogen persulfate to the organic pollutant solution is 1-1000: 10000.
aiming at the effect of the high-activity zinc-iron hydrotalcite heterogeneous Fenton material on removing organic pollutants, experiments are carried out according to the operation steps in the embodiment 2, and the operation steps are respectively as follows:
experiment one: the high-activity zinc-iron hydrotalcite heterogeneous Fenton material disclosed by the invention is used for phenol degradation experiments under different pH conditions, and specifically comprises the following steps:
taking 100mL of wastewater to be treated, wherein the concentration of phenol in the wastewater to be treated is 10mg/L, the dosage of the high-activity zinc-iron hydrotalcite heterogeneous Fenton catalyst material is 20mg, and the initial pH =3, the initial pH =5, the initial pH =7, the initial pH =9 and the initial pH =11 of the solution are set. And (3) recording the phenol degradation rate in different time, and monitoring the change of the pH value in the whole process.
The degradation experiment result is shown in fig. 1, and the experiment shows that the prepared high-activity zinc-iron hydrotalcite heterogeneous Fenton catalyst material is low in dependence on pH, the requirement of the traditional homogeneous Fenton reaction on acidity of a reaction system is overcome, the phenol is efficiently degraded within the range of pH = 3-11, and the removal rate reaches 90-100% within 60 min.
The change of the pH value of the solution in the degradation experiment is shown in figure 2, and the experiment shows that the prepared high-activity zinc-iron hydrotalcite heterogeneous Fenton catalyst has the capability of efficiently adjusting the pH value, the reaction pH value can be adjusted to be neutral within 5 minutes for the range of pH = 3-11, and the reaction pH value is kept until the reaction is finished, so that the influence of the pH value is really overcome.
Experiment two: the high-activity zinc-iron hydrotalcite heterogeneous Fenton material and other conventional catalysts are used for carrying out a comparative experiment on the total organic carbon removal rate of neutral actual wastewater. The conventional catalysts used in the comparative experiment were iron oxide, iron powder and ferrous sulfate heptahydrate, and the degradation experiment was performed under the following conditions and the change in total organic carbon was tested.
The dosage of the conventional catalyst of the comparative group is respectively 5.4mg of ferric oxide, 3.8mg of iron powder, 18.8mg of ferrous sulfate heptahydrate, 20mg of high-activity zinc-iron hydrotalcite heterogeneous Fenton catalyst material, and the iron contents of the dosages are the same. The degradation experiments of the four groups are carried out according to the method in the embodiment 2, the experiment time is 24 hours, and the total organic carbon removal rate is measured after the experiment is finished.
The experimental result is shown in fig. 3, and the experiment shows that the high-activity zinc-iron hydrotalcite heterogeneous Fenton catalyst material prepared by the invention has obviously better activity than that of a conventional iron-based catalyst in the actual wastewater treatment, realizes the effective removal of organic pollutants, and has a removal rate of 64.4% within 24 h.
Experiment three: the chemical oxygen demand experiment of the high-activity zinc-iron hydrotalcite heterogeneous Fenton material for treating neutral actual wastewater disclosed by the invention is carried out. Degradation experiments were performed and the change in chemical oxygen demand was tested under the following conditions.
The actual wastewater of nitrobenzene to be treated is 100mL, and the dosage of the high-activity zinc-iron hydrotalcite heterogeneous Fenton catalyst material is 20 mg. The degradation experiments were carried out according to the method of example 2, with the chemical oxygen demand being monitored over time.
Experiment four: the degradation rate comparison experiment of the high-activity zinc-iron hydrotalcite heterogeneous Fenton material for treating common organic pollutants. Common organic pollutants are selected and respectively subjected to degradation experiments, and the degradation rate of the high-activity zinc-iron hydrotalcite heterogeneous Fenton material on different common organic pollutants is detected.
Typical organic pollutants comprise crystal violet, malachite green and rhodamine B as cationic dyes, methyl orange, golden orange II and lemon yellow as anionic dyes, ciprofloxacin, enrofloxacin and norfloxacin as antibiotics, 100mL of wastewater containing the organic pollutants is taken, and the dosage of the high-activity zinc-iron hydrotalcite heterogeneous Fenton catalyst material is 20 mg. Degradation experiments were performed according to the method of example 2, testing the degradation rate for 24 h.
The experimental result is shown in fig. 5, and the experiment shows that the prepared high-activity zinc-iron hydrotalcite heterogeneous Fenton catalyst material achieves the standard of more than 80% degradation rate after being continuously degraded for 24 hours in the process of treating different types of organic pollutants, so that the prepared catalyst material has degradation capability on different types of organic pollutants, and the feasibility of practical application is shown.
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 zinc-iron hydrotalcite heterogeneous Fenton material is characterized in that:
the zinc-iron hydrotalcite heterogeneous Fenton material is constructed by the following steps:
step one, preparing a zinc-iron ion solution;
slowly adding alkali liquor into the zinc-iron ion solution, and mechanically stirring the mixture until the mixture is uniform to obtain zinc-iron suspension;
step three, heating the zinc-iron suspension to a reaction temperature, and reacting at a constant temperature;
and step four, cooling the zinc-iron suspension after the reaction is finished, alternately washing the zinc-iron suspension by using ultrapure water and ethanol, washing until the supernatant is stable at neutrality, keeping the pH value unchanged after three times of washing, and drying to obtain the zinc-iron hydrotalcite heterogeneous Fenton material.
2. The highly active zinc-iron hydrotalcite heterogeneous fenton material according to claim 1, characterized in that:
the preparation method of the zinc-iron ion solution in the first step comprises the following steps:
adding 1-1000 parts by mass of an iron source and 1-2000 parts by mass of a zinc source into 10000-100000 parts by mass of an aqueous solution, carrying out ultrasonic treatment, uniformly mixing, and stirring until the iron source and the zinc source are completely dissolved to obtain a uniform solution.
3. The highly active zinc-iron hydrotalcite heterogeneous fenton material according to claim 1, characterized in that:
the iron source is any one or mixture of more of ferric chloride, ferrous chloride, ferric sulfate, ferrous sulfate, ferric nitrate, ferrous nitrate, ferric oxalate and ferrous oxalate, and the zinc source is any one or mixture of more of zinc chloride, zinc sulfate, zinc nitrate and zinc oxalate.
4. The highly active zinc-iron hydrotalcite heterogeneous fenton material according to claim 1, characterized in that:
in the second step, the mass part ratio of the alkali liquor to the zinc-iron ion solution is 0.001-1: 10 to 100 parts;
and adding the alkali liquor into the zinc-iron ion solution, and mechanically stirring until the mixed solution is in a complete suspension state.
5. The highly active zinc-iron hydrotalcite heterogeneous fenton material according to claim 1, characterized in that:
the alkali liquor is one or more of sodium hydroxide, potassium hydroxide, calcium hydroxide, sodium carbonate, sodium bicarbonate and ammonia water, and the concentration of the alkali liquor is 0.05-1 mol/L.
6. The highly active zinc-iron hydrotalcite heterogeneous fenton material according to claim 1, characterized in that:
in the third step, the zinc-iron suspension is heated to the reaction temperature of 20-100 ℃, and the reaction duration is 2-100 hours.
7. The method for removing organic pollutants by using the high-activity zinc-iron hydrotalcite heterogeneous Fenton material is characterized by comprising the following steps of:
the method comprises the following steps:
step A: selecting an organic pollutant solution;
and B: the high-activity zinc-iron hydrotalcite heterogeneous Fenton material prepared in the claims 1 to 6 is put into an organic pollutant solution, stirred uniformly, and added with potassium hydrogen persulfate to initiate reaction, so as to remove the organic pollutants.
8. The method for removing organic contaminants using a highly active zinc-iron hydrotalcite heterogeneous fenton material according to claim 7, wherein:
in the step B, the concentration of the potassium hydrogen persulfate is 42-46%, and the mass part ratio of the added potassium hydrogen persulfate to the organic pollutant solution is 1-1000: 10000.
9. the method for removing organic contaminants using a highly active zinc-iron hydrotalcite heterogeneous fenton material according to claim 7, wherein:
step B the reaction was stirred under dark conditions.
10. The method for removing organic contaminants using a highly active zinc-iron hydrotalcite heterogeneous fenton material according to claim 7, wherein:
the organic pollutant is any one or mixture of phenol, nitrobenzene, organic dye or antibiotic.
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