CN115770604A - Fe-N@C catalyst prepared from blue algae in Taihu lake and preparation method and application thereof - Google Patents
Fe-N@C catalyst prepared from blue algae in Taihu lake and preparation method and application thereof Download PDFInfo
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- GSDSWSVVBLHKDQ-UHFFFAOYSA-N 9-fluoro-3-methyl-10-(4-methylpiperazin-1-yl)-7-oxo-2,3-dihydro-7H-[1,4]oxazino[2,3,4-ij]quinoline-6-carboxylic acid Chemical compound FC1=CC(C(C(C(O)=O)=C2)=O)=C3N2C(C)COC3=C1N1CCN(C)CC1 GSDSWSVVBLHKDQ-UHFFFAOYSA-N 0.000 claims description 21
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- NQXWGWZJXJUMQB-UHFFFAOYSA-K iron trichloride hexahydrate Chemical compound O.O.O.O.O.O.[Cl-].Cl[Fe+]Cl NQXWGWZJXJUMQB-UHFFFAOYSA-K 0.000 claims description 6
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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 method for removing PPCPs in a water body by using a Fe-N@C biochar catalyst activated persulfate prepared from blue algae in Taihu lake to remove PPCPs, wherein a Fe-N@C biochar material prepared from the blue algae in Taihu lake is used as a catalyst for activating PMS to remove the PPCPs, and a Fe-N@C biochar material is prepared by calcining at the temperature of more than 500 ℃. The invention takes the biochar material with the advantages of large specific surface area, high catalytic performance, many active sites, low leaching rate of transition metal ions and the like as the catalyst, and can efficiently activate PMS so as to convert PMS into free radicals and non-free radicals with strong oxidizing property, thereby effectively attacking macromolecular substances and converting the macromolecular substances into micromolecules and realizing high removal rate of PPCPs. The method has the characteristics of simple process, easily obtained raw materials, low cost, simple and convenient operation, environmental protection, high removal efficiency and the like, and has high use value and application prospect.
Description
Technical Field
The invention belongs to the field of recycling of lake Tai blue algae and advanced oxidation treatment of PPCPs, and particularly relates to a Fe-N@C biochar catalyst prepared from lake Tai blue algae and a method for removing PPCPs in a water body by activating persulfate by using the biochar catalyst.
Background
With the continuous development of society, the increasing of human living indexes leads to the discharge of various new pollutants into the water body environment, especially PPCPs organic pollutants, although the half-life period of PPCPs organic pollutants is not long, the PPCPs organic pollutants are frequently and largely used in the personal and livestock industry, so that the problem of water body and soil environment pollution is increasingly serious, and the PPCPs organic pollutants are the focus of attention of researchers and society in various fields.
At present, the traditional drinking water and wastewater treatment plants do not have a treatment process specially aiming at the PPCPs, and the existing treatment process technology can not completely remove the PPCPs. At present, common treatment methods for PPCPs organic pollutants include an adsorption method, a common oxidation method, a chemical method, a membrane separation method, a biological method and the like, and the traditional treatment technologies all have the defects of complex and tedious operation, high equipment requirement, high cost, easy secondary pollution to the environment, low treatment efficiency and the like, and a large amount of chemical agents are added in the chemical method as a removal means. In view of the above, there is a need for a technology that can process PPCPs with high efficiency, green color, and low cost.
Based on the above problems, the advanced oxidation method was first proposed in 1987. Advanced oxidation technologies (AOPs) are defined as generating a large amount of strong oxidizing radicals, attacking macromolecular organic matters and reacting with the macromolecular organic matters by using the high-activity radicals, further destroying the macromolecular structures to form small molecules so as to achieve the purpose of removing organic pollutants by oxidation, and realizing efficient oxidation treatment. Among them, hydrogen peroxide, peroxodisulfate (PDS), peroxomonosulfate (PMS) are commonly used oxidizing agents in the field of advanced oxidation at present. The hydrogen peroxide generates hydroxyl radicals to attack organic macromolecules, but the reaction of the hydroxyl radicals under acidic conditions is limited. In recent years, persulfate is widely applied to advanced oxidation technology, and has high stability and solvent property; the activation mode is various, the application range is wide, and the like, and the generated sulfate radical has longer service life, thereby being beneficial to fully contacting with pollutants and improving the effect of degrading the pollutants to a great extent. Persulfate salts, however, have a limited ability to oxidize organic pollutants by themselves and therefore require activation by other external means to generate highly reactive and non-free radicals.
The traditional persulfate activation method has the characteristics of heat, UV, transition metal ions and the like, but has the characteristics of high cost, high energy consumption and the like, and has the defects of poor reutilization property, secondary environmental pollution caused by metal dissolution and the like when organic matters are degraded by using the transition metal as an activation means. Biochar is a non-metallic material converted from biomass, has the advantages of biocompatibility, environmental friendliness, low cost, wide source and the like, and is widely applied to the fields related to environmental adsorption, environmental catalysis and the like, but the catalytic activity of pure biochar is limited. Therefore, a persulfate biochar catalyst with high catalytic activity is needed, and has great significance for improving the capacity of activating persulfate so as to remove PPCPs.
Disclosure of Invention
The invention provides a preparation method of Fe-N@C biochar material prepared by using blue algae in Taihu lake and a method for removing PPCPs by activating persulfate.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
a method for preparing Fe-N@C catalyst by using blue algae in Taihu lake is characterized in that the fished blue algae is naturally dried and then is pyrolyzed and activated by acid and alkali to prepare a biochar catalytic material Fe-N@C, and the method specifically comprises the following steps:
s1, airing and collecting the salvaged blue algae in the Taihu lake under natural conditions, mixing the collected blue algae with an iron source, grinding the mixture into powder and sieving the powder;
s2, putting the mixed powder into a tube furnace, and adding N 2 Carbonizing under protection to obtain charcoal;
s3, mixing the biochar with potassium hydroxide, putting the mixture into a tubular furnace, and reacting the mixture in a reactor N 2 Activating under protection to obtain alkali-activated charcoal;
and S4, carrying out acid washing on the alkali-activated biochar, washing with water until the pH value is neutral, drying the sample, grinding the sample into powder, and sieving the powder to obtain the Fe-N@C biochar material.
Further defined, the iron source in S1 is ferric chloride hexahydrate.
Further limiting, the S1 is sieved by a 100-mesh sieve.
Further limiting, the adding amount of the iron source in S1 is 1-5mg/g.
Further limiting, the carbonization temperature in S2 is 400-500 ℃, and the time is 2-3h.
Further limiting, the mass ratio of the biochar to the potassium hydroxide in the S3 is (1-2): 1.
further limiting the activation temperature in S3 to 600-900 ℃ and the activation time to 2.5-3.5h.
Further limiting, 1-2mol/L sulfuric acid solution is used for acid washing in S4, the temperature is 60-90 ℃, and the time is 8-16h, so as to remove other iron substances and ash on the surface of the carbon material.
Further limiting, in S4, the powder is sieved by a 100-mesh sieve.
Further limiting, the drying temperature in S4 is 85-105 ℃.
Another object of the present invention is to provide a Fe-N@C type biochar material obtained by the preparation method as described above.
The invention also aims to use the Fe-N@C type biochar material obtained by the preparation method as a catalyst to activate peroxymonosulfate to remove PPCPs in water, and the method comprises the steps of adding the Fe-N@C biochar material and persulfate into organic wastewater, mixing and stirring at room temperature, and removing PPCPs organic pollutants in the wastewater.
Further defined, the PPCPs organic contaminant is ofloxacin, a fluoroquinolone antibiotic in PPCPs.
Further limit, the adding amount of the Fe-N@C biochar material is 0.05-0.3g/L.
Further limiting, the adding amount of the persulfate is 0.3-2mmol/L, and the mixing and stirring time is 30-80min.
Further limited, the persulfate is PMS monopersulfate.
Further limiting, the pH value of the organic wastewater is 3-11, and the initial concentration of the ofloxacin is 5-20mg/L.
Further, the pH value of the organic wastewater is adjusted by using a sulfuric acid solution or a sodium hydroxide solution.
Compared with the prior art, the invention has the following characteristics and advantages:
(1) The preparation method of the invention is to utilize the blue algae in Taihu lake to prepare the Fe-N@C biochar material, is a simple preparation method with low cost and low consumption, has the advantages of environmental protection, and can realize the resource utilization of the blue algae in Taihu lake to a certain extent.
(2) The method is simple and convenient to operate, low in cost and beneficial to industrial production.
(3) The biochar is prepared by a method of firstly pyrolyzing and then activating, can be used for preliminarily removing some unstable substances on the surface of blue-green algae by pyrolysis and carbonization, opening a certain pore diameter, and then activating the biochar after the process, so that the pore diameter can be further fully opened, the specific surface area and the number of active sites are increased, and the adsorption catalytic capability is further improved.
(4) The iron-doped cyanobacteria charcoal prepared by the method can further improve the adsorption and catalysis capability of the cyanobacteria charcoal. In a system for activating peroxymonosulfate, the doping of iron can enable the system to generate sulfate radicals, singlet oxygen, high-valence iron species and other oxidizing species, thereby realizing the removal of organic pollutants. Therefore, the Fe-N@C biochar material prepared by the invention has excellent capability of removing pollutants in an activated peroxymonosulfate system, and also has good removal effect on other antibiotics.
Drawings
FIG. 1 is a graph showing the effect of Fe-N@C-8 obtained in example 5 on ofloxacin removal without PMS, but with varying amounts of biochar material added;
FIG. 2 is a graph showing the effect of Fe-N@C-8 obtained in example 6 on ofloxacin removal with PMS added and with other conditions unchanged, but with the amount of biochar material added varied;
FIG. 3 is a graph showing the effect of Fe-N@C-8 on ofloxacin removal obtained in example 7 of the present invention when PMS is added and the amount of PMS added is changed without changing other conditions;
Detailed Description
The present invention is further described in detail below with reference to specific examples, but the scope of the present invention is not limited thereto.
Unless otherwise stated, the experimental conditions for the removal of ofloxacin from PMS using Fe-N@C in the following examples were: the concentration of the ofloxacin is 10mg/L, 100mL of ofloxacin solution is prepared, 0.1g of Fe-N@C biochar material is added, and 0.1mol/L of H is added 2 SO 4 And NaOH solution the pH of the ofloxacin solution was adjusted =7.0 and the removal time was 60min. What is more.
Example 1:
naturally airing, grinding and crushing the salvaged blue algae, and mixing the smashed blue algae with ferric chloride hexahydrate according to the ratio of iron to blue algae being 3 mg/g. Grinding the obtained iron-containing blue algae into powder, sieving with a 100-mesh sieve, placing into a tube furnace, and performing N 2 Carbonizing at the flow rate of 300mL/min and the temperature of 500 ℃ for 2h to obtain the biochar. Mixing the obtained biochar with potassium hydroxide according to the carbon-alkali ratio of 2, putting the mixture into a tubular furnace, and reacting in N 2 Activating for 3h at the flow rate of 300mL/min and the temperature of 600 ℃ to obtain the biochar after alkali activation, then stirring for 12h at 70 ℃ by using 1mol/L sulfuric acid solution, repeatedly washing with deionized water to be neutral, and naming the biochar as Fe-N@C-6.
The efficiency of removing ofloxacin by catalyzing PMS by Fe-N@C-6 obtained in the embodiment reaches 72.16%.
Example 2:
the difference between this example and example 1 is: the activation temperature was 700 ℃. The specific mode is as follows:
naturally airing, grinding and crushing the salvaged blue algae, and mixing the smashed blue algae with ferric chloride hexahydrate according to the ratio of iron to blue algae being 3 mg/g. Grinding the obtained iron-containing blue algae into powder, sieving with a 100-mesh sieve, placing into a tube furnace, and performing N 2 Carbonizing for 2h at the flow rate of 300mL/min and the temperature of 500 ℃ to obtain the biochar. Mixing the obtained biochar with potassium hydroxide according to the carbon-alkali ratio of 2, putting the mixture into a tubular furnace, and reacting in N 2 Activating for 3h at the flow rate of 300mL/min and the temperature of 700 ℃ to obtain alkali-activated biochar, stirring for 12h at 70 ℃ by using 1mol/L sulfuric acid solution, repeatedly washing with deionized water to be neutral, and naming the biochar as Fe-N@C-7.
The efficiency of removing ofloxacin by catalyzing PMS by Fe-N@C-7 obtained in the embodiment reaches 90.14%.
Example 3:
the difference between this example and example 1 is: the activation temperature was 800 ℃. The specific mode is as follows:
naturally airing, grinding and crushing the salvaged blue algae, and mixing the smashed blue algae with ferric chloride hexahydrate according to the ratio of iron to blue algae being 3 mg/g. Grinding the obtained iron-containing blue algae into powder, sieving with a 100-mesh sieve, placing into a tube furnace, and performing N 2 Carbonizing for 2h at the flow rate of 300mL/min and the temperature of 500 ℃ to obtain the biochar. Mixing the obtained biochar with potassium hydroxide according to the carbon-alkali ratio of 2, putting the mixture into a tubular furnace, and reacting in N 2 Activating for 3h at the flow rate of 300mL/min and the temperature of 800 ℃ to obtain the biochar after alkali activation, stirring for 12h at 70 ℃ by using 1mol/L sulfuric acid solution, repeatedly washing with deionized water to be neutral, and naming the biochar as Fe-N@C-8.
The efficiency of the Fe-N@C-8 obtained in the embodiment for catalyzing PMS to remove ofloxacin reaches 94.98%.
Example 4:
the difference between this example and example 1 is: the activation temperature was 900 ℃. The specific mode is as follows:
naturally airing, grinding and crushing the salvaged blue algae, and mixing the smashed blue algae with ferric chloride hexahydrate according to the ratio of iron to blue algae being 3 mg/g. Grinding the obtained iron-containing blue algae into powder, sieving with a 100-mesh sieve, placing into a tube furnace, and performing N 2 Carbonizing for 2h at the flow rate of 300mL/min and the temperature of 500 ℃ to obtain the biochar. Mixing the obtained biochar with potassium hydroxide according to the carbon-alkali ratio of 2, putting the mixture into a tubular furnace, and reacting in N 2 Activating at flow rate of 300mL/min and temperature of 900 deg.C for 3h to obtain alkali-activated charcoal, stirring with 1mol/L sulfuric acid solution at 70 deg.C for 12h, repeatedly washing with deionized water to neutrality, and naming as Fe-N@C-9
The efficiency of the Fe-N@C-9 obtained in the embodiment for catalyzing PMS to remove ofloxacin reaches 95.01%.
Example 5:
by adopting the Fe-N@C-8 catalyst obtained in example 3, under the condition of not adding PMS, other conditions are controlled to be unchanged, the adding amount of the Fe-N@C-8 biochar material is changed to be 0.05, 0.1, 0.15 and 0.2g/L respectively, and the removal efficiency of Fe-N@C-8 to ofloxacin is shown in figure 1.
As can be seen from FIG. 1, the adsorption removal rate of the Fe-N@C-8 alone for ofloxacin is increased with the increase of the dosage, and the adsorption removal rate of the Fe-N@C-8 alone reaches 86.24% when the dosage is increased to 0.2 g/L.
Example 6:
the Fe-N@C-8 catalyst obtained in example 3 was used, other conditions were controlled to be unchanged, and the addition amounts of the biochar material were changed to 0.05, 0.1, 0.15 and 0.2g/L, to obtain Fe-N@C-8 with ofloxacin removal efficiency as shown in FIG. 2.
As can be seen from FIG. 2, under the condition of fixed peroxymonosulfate concentration, the capability of activating peroxymonosulfate to remove ofloxacin is improved along with the increase of the dosage of Fe-N@C-8, and the removal rate of activated peroxymonosulfate reaches 100% when the dosage of Fe-N@C-8 is up to 0.15 g/L.
Example 7:
the Fe-N@C-8 catalyst obtained in example 3 was used, other conditions were controlled to be unchanged, and the amounts of PMS added were changed to 0.3, 0.5, 0.1 and 0.2mmol/L, to obtain Fe-N@C-8 with ofloxacin removal efficiency as shown in FIG. 3.
As shown in FIG. 3, it can be seen that the removal efficiency of ofloxacin was improved with the increase of the concentration of the peroxymonosulfate by changing the amount of the peroxymonosulfate added to the fixed amount of Fe-N@C-8, but the removal rate of ofloxacin reached 100% when the concentration of the sulfate was increased to 0.15 mmol/L.
It should be noted that the above-mentioned embodiments are only for illustrating the technical solutions of the present invention and not for limiting, and although the present invention has been described in detail with reference to the preferred embodiments, it should be understood by those skilled in the art that modifications or equivalent substitutions may be made on the technical solutions of the present invention without departing from the spirit and scope of the technical solutions of the present invention, which should be covered by the claims of the present invention.
Claims (10)
1. A method for preparing Fe-N@C catalyst by using blue algae in Taihu lake is characterized by comprising the following steps:
s1, airing and collecting the salvaged blue algae in the Taihu lake under natural conditions, mixing the collected blue algae with an iron source, grinding the mixture into powder and sieving the powder;
s2, putting the mixed powder into a tube furnace, and adding N 2 Carbonizing under protection to obtain charcoal;
s3, mixing the biochar with potassium hydroxide, putting the mixture into a tube furnace, and reacting the mixture in a reactor under N 2 Activating under protection to obtain alkali-activated charcoal;
and S4, carrying out acid washing on the alkali-activated biochar, washing with water until the pH value is neutral, drying the sample, grinding the sample into powder, and sieving the powder to obtain the Fe-N@C biochar material.
2. The method for preparing the Fe-N@C catalyst by using blue algae in Taihu lake as claimed in claim 1, wherein the iron source in S1 is ferric chloride hexahydrate.
3. The method for preparing the Fe-N@C catalyst by using blue algae in Taihu lake as claimed in claim 1, wherein the amount of the iron source added in S1 is 1-5mg/g.
4. The method for preparing the Fe-N@C catalyst by using the blue algae in the Taihu lake as the catalyst in claim 1, wherein the carbonization temperature in S2 is 400-500 ℃ and the carbonization time is 2-3h.
5. The method for preparing the Fe-N@C catalyst by using the blue algae in the Taihu lake according to claim 1, wherein the mass ratio of the biochar to the potassium hydroxide in S3 is (1-2): 1; the activation temperature is 600-900 ℃, and the activation time is 2.5-3.5h.
6. The method for preparing the Fe-N@C catalyst by using blue algae in Taihu lake as claimed in claim 1, wherein 1-2mol/L sulfuric acid solution is used for acid washing in S4, the temperature is 60-90 ℃, and the time is 8-16h.
7. The Fe-N@C type biochar material obtained by the preparation method of claim 1.
8. A method for removing PPCPs in a water body by using Fe-N@C catalyst activation peroxymonosulfate prepared from blue algae in Taihu lake to activate the peroxymonosulfate is characterized in that Fe-N@C biochar material prepared by the method in claim 1 is used as a catalyst, fe-N@C biochar material and persulfate are added into organic wastewater, and are mixed and stirred at room temperature to remove the organic pollutants in the PPCPs in the wastewater.
9. The method for removing PPCPs in water by using Fe-N@C catalyst activation peroxymonosulfate prepared from blue algae in Taihu lake of claim 8, wherein the adding amount of Fe-N@C biochar material is 0.05-0.3g/L, the adding amount of persulfate is 0.3-2mmol/L, and the mixing and stirring time is 30-80min.
10. The method for removing PPCPs in water body by using Fe-N@C catalyst activated peroxymonosulfate prepared from blue algae in Taihu lake as claimed in claim 8, wherein the pH value of the organic wastewater is 3-11, and the initial concentration of ofloxacin is 5-20mg/L.
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Citations (10)
| Publication number | Priority date | Publication date | Assignee | Title |
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