CN111747504A - Remediation agent for water body containing pollutants and application thereof - Google Patents
Remediation agent for water body containing pollutants and application thereof Download PDFInfo
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- CN111747504A CN111747504A CN202010525433.4A CN202010525433A CN111747504A CN 111747504 A CN111747504 A CN 111747504A CN 202010525433 A CN202010525433 A CN 202010525433A CN 111747504 A CN111747504 A CN 111747504A
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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
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/34—Organic compounds containing oxygen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/36—Organic compounds containing halogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
- C02F2101/38—Organic compounds containing nitrogen
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/023—Reactive oxygen species, singlet oxygen, OH radical
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- Hydrology & Water Resources (AREA)
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- Environmental & Geological Engineering (AREA)
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Abstract
The invention provides a repairing agent for a water body containing pollutants and application thereof. In the repairing agent for the water body containing the pollutants, the plant extract can obviously promote the Fe (III)/Fe (II) circulation, so that the content of active species such as OH and the like in the system is increased, the pollutant removal rate and the reaction efficiency of a zero-valent iron Fenton system are effectively improved, the yield of iron sludge is reduced, no toxic substance is separated out, and the secondary pollution is greatly reduced.
Description
Technical Field
The invention belongs to the technical field of water treatment, and particularly relates to a repairing agent for a water body containing pollutants and application thereof.
Background
Antibiotics such as norfloxacin, metronidazole, lincomycin, tetracycline and the like are widely detected in water, and the antibiotics in the water can cause bacteria to generate drug resistance and possibly threaten human health through a food chain, so that the antibiotics are difficult to effectively remove by the traditional water treatment process. Therefore, it is urgently needed to develop an effective treatment method for removing antibiotics in water.
In the field of research on removal of organic pollutants in water, advanced oxidation technology based on zero-valent iron has been proved to be capable of effectively removing the organic pollutants in water. However, the passivation effect of the zero-valent iron weakens the corrosion performance of the zero-valent iron, so that the zero-valent iron is difficult to release divalent iron ions continuously, the removal effect of organic pollutants is influenced, the consumption of the zero-valent iron is increased, and the large-scale application of the repair technology is restricted. Therefore, it is important to overcome the bottleneck problem existing in the application of the zero-valent iron-based advanced oxidation technology.
In recent years, a reducing component is added into a zero-valent iron Fenton system to promote Fe (III)/Fe (II) cycle, so that the iron cycle can be effectively promoted, the Fenton-like efficiency can be improved, and a new idea is provided for further improving the Fenton-like efficiency. However, from the prior reports, the adopted promoter has the disadvantage of high cost, and therefore, how to select an appropriate reducing promoter is important to control the cost.
Disclosure of Invention
The plant extract has the advantages of wide source, easy preparation, environmental protection, low cost and the like, and has been used for replacing toxic and harmful reducing agents to prepare the nano zero-valent iron-based nano material. The invention aims to provide a repairing agent containing a pollutant water body, which has wide sources, easy preparation, environmental friendliness and low cost, and an application thereof.
In a first aspect of the present invention, there is provided:
a repairing agent for water body containing pollutants comprises iron powder, hydrogen peroxide, and plant extractive solution.
Preferably, the mass concentration of the iron powder is (20 to 100) mg/L in terms of a contaminant having a mass concentration of 1 mg/L.
Preferably, the mass concentration of the iron powder is (35 to 65) mg/L in terms of a contaminant having a mass concentration of 1 mg/L.
Preferably, the mass concentration of the hydrogen peroxide is (3 to 15) mg/L based on 1mg/L of the contaminant.
Preferably, the mass concentration of the plant extract is (6-20) mg/L based on 1mg/L of the contaminant.
Preferably, the iron powder is micron-sized iron powder, and the particle size is 10-200 μm.
Preferably, the plant extract is at least one selected from tea extract, water hyacinth extract, eucalyptus leaf extract and grape leaf extract.
Preferably, the plant extract is at least one selected from oolong tea extract, yellow tea extract, black tea extract, green tea extract, black tea extract and white tea extract.
Preferably, the plant extract is deionized water plant extract.
Preferably, the contaminating substance is at least one of norfloxacin, metronidazole, lincomycin and tetracycline.
In a second aspect of the present method, there is provided:
a method for restoring water body containing pollutants comprises adding the restoring agent into polluted water body containing at least one of norfloxacin, metronidazole, lincomycin and tetracycline.
The invention has the beneficial effects that:
1. in the repairing agent for the water body containing the pollutants, the plant extract can obviously promote the Fe (III)/Fe (II) circulation, so that the content of active species such as OH and the like in the system is increased, the pollutant removal rate and the reaction efficiency of a zero-valent iron Fenton system are effectively improved, the yield of iron sludge is reduced, no toxic substance is separated out, and the secondary pollution is greatly reduced.
2. The repairing agent for the water body containing the pollutants has low cost and wide application range, and is suitable for large-scale popularization and application.
3. The method for repairing the water body containing the pollutants is simple and efficient, is simple and convenient to operate, provides a new idea for removing other organic pollutants, and the plant extract effectively promotes zero-valent iron and hydrogen peroxide to generate a large amount of hydroxyl free radicals and singlet oxygen for attacking norfloxacin, metronidazole, lincomycin, tetracycline and the like so as to remove the norfloxacin, the metronidazole, the lincomycin and the tetracycline.
Drawings
FIG. 1 is a graph showing the effect of the remediation agent for water bodies containing pollutants on the remediation of norfloxacin-polluted water bodies in examples 1 to 6.
FIG. 2 is a FRAP method graph showing the antioxidant ability of different plant extracts of examples 1 to 6.
FIG. 3 is a graph showing the effect of different amounts of green tea extract on the remediation of norfloxacin-contaminated water.
FIG. 4 is a graph showing the effect of different iron powder dosages on the remediation effect of norfloxacin-contaminated water.
FIG. 5 is a graph showing the effect of different amounts of added hydrogen peroxide on the remediation of norfloxacin-contaminated water.
FIG. 6 is a diagram of the remediation situation of norfloxacin contaminated water by different systems.
Detailed Description
In order to make the objects, technical solutions and technical effects of the present invention more clear, the present invention will be described in further detail with reference to specific embodiments. It should be understood that the detailed description and specific examples, while indicating the preferred embodiment of the invention, are intended for purposes of illustration only and are not intended to limit the scope of the invention.
For comparison, in the following examples, test examples, experimental examples or comparative examples, the plant extract was prepared by the following method: adding 10g of plant leaves into 1L of deionized water, heating in a water bath to 60-80 ℃, extracting for 1h, cooling to room temperature after extraction is finished, carrying out vacuum filtration on a water bath extracting solution, filling the obtained plant extracting solution into a penicillin bottle, and refrigerating for storage.
Example 1: a repairing agent for water body containing pollutant comprises 0.5g/L micron-sized iron powder, 1mM hydrogen peroxide and 0.1g/L green tea leaf extract (GT).
Example 2: a repairing agent for water body containing pollutant comprises 0.5g/L micron-sized iron powder, 1mM hydrogen peroxide and 0.1g/L black tea leaf extract (BT).
Example 3: a repairing agent for water body containing pollutant comprises 0.5g/L micron-sized iron powder, 1mM hydrogen peroxide and 0.1g/L yellow tea extract (YT).
Example 4: a repairing agent for water body containing pollutant comprises 0.5g/L micron-sized iron powder, 1mM hydrogen peroxide and 0.1g/L black tea extract (DT).
Example 5: a repairing agent for water body containing pollutant comprises 0.5g/L micron-sized iron powder, 1mM hydrogen peroxide and 0.1g/L white tea leaf extract (WT).
Example 6: a repairing agent for water body containing pollutant comprises 0.5g/L micron-sized iron powder, 1mM hydrogen peroxide and 0.1g/L oolong tea extract (OT).
Example 7: a method for remedying a water body containing pollutants comprises the steps of respectively adding the remediation agent for the water body containing the pollutants in the embodiments 1-6 into norfloxacin aqueous solution with the initial concentration of 10mg/L, arranging 2 parallel samples in each group, oscillating the samples in a constant-temperature oscillation box for 2 hours at the temperature of 30 ℃ and the speed of 200rpm, filtering the reaction solution, taking supernate, filtering the supernate with a 0.45-micron filter membrane, analyzing the residual norfloxacin filtrate by using high performance liquid chromatography, and utilizing the norfloxacin filtrate
Calculating the norfloxacin removal rate at different time points (where ω istThe removal rate of norfloxacin at t,%; c. C0And ctInitial norfloxacin concentration in solution and concentration at t) were averaged over 2 replicates and the results are shown in figure 1. From the figure, it is clear that Fe alone0/H2O2Compared with the norfloxacin removal group (the corresponding data are shown in fig. 6), the norfloxacin removal effect can be effectively improved by adding the tea extract. Wherein, the green tea extract (GT) has the best effect of removing norfloxacin from zero-valent iron Fenton, and the removal rate of norfloxacin reaches 98.84% after the reaction is finished. The other tea extract solutions have the increasing effects of removing norfloxacin from zero-valent iron fenton, namely a black tea extract (BT), a yellow tea extract (YT), a black tea extract (DT), a white tea extract (WT) and an oolong tea extract (OT) from large to small, and the removal rates of norfloxacin are respectively 87.92%, 80.11%, 79.16%, 68.03% and 63.94%.
Test example 1: to verify that the plant extract reduces Fe (III) to Fe (II), even Fe0OfThe antioxidant capacity of the plant extracts of examples 1-6 was measured by the total antioxidant capacity assay (FRAP method) to visually verify the reduction capacity of the plant extracts to fe (iii), and the results are shown in fig. 2. As can be seen from FIG. 2, the tea extracts of different types have certain antioxidant capacity, wherein the green tea extract has the strongest antioxidant capacity, and the antioxidant activity of the green tea extract reaches 5802.5mMFe2+The effect is optimal.
Experimental example 1: influence of adding amount of green tea extract on norfloxacin polluted water body remediation effect
Adding 5mL/L, 10mL/L, and 20mL/L green tea extractive solution into Fenton-like reaction system comprising norfloxacin aqueous solution with initial concentration of 10mg/L and reduced iron powder with concentration of 1mM and addition amount of 0.50g/L, arranging 2 parallel samples for each green tea extractive solution group with different concentrations, oscillating at 30 deg.C and 200rpm in a constant temperature oscillation box for 2h, filtering the reaction solution, collecting supernatant, filtering with 0.45 μm filter membrane, analyzing residual norfloxacin filtrate with high performance liquid chromatography, and analyzing with high performance liquid chromatography
Calculating the norfloxacin removal rate at different time points (where ω istThe removal rate of norfloxacin at t,%; c. C0And ctInitial norfloxacin concentration in solution and concentration at t) were averaged over 2 replicates and the results are shown in figure 3. As can be seen from fig. 3, in the aqueous solution containing norfloxacin with an initial concentration of 10mg/L, when the addition amount of the green tea extract is 5mL/L, the removal rate of norfloxacin after the reaction is only 43.25%, and when the addition amount of the green tea extract is 10mL/L, the removal rate of norfloxacin is increased to 99.50%, which shows that as the addition amount of the green tea extract is increased, more green tea extract is present in the system to promote zero-valent iron and hydrogen peroxide to generate more hydroxyl radicals and singlet oxygen, so that more norfloxacin is removed; in addition, when the amount of the green tea leaf extract added was increased to 20mL/L, the norfloxacin removal rate after the completion of the reaction was 98.85%, which indicates that the amount of the green tea leaf extract added reached a certain levelAnd the norfloxacin removal effect in the water body cannot be continuously improved. Therefore, when the adding amount of the green tea extract is 10mL/L, namely the mass concentration is 1mg/L of norfloxacin, the effect of restoring the water body polluted by norfloxacin is the best when the adding amount of the green tea extract is 10 mg/L.
Experimental example 2: influence of iron powder addition on norfloxacin polluted water body remediation effect
Adding 1mL of green tea leaf extract into norfloxacin aqueous solution with initial concentration of 10mg/L and Fenton-like reaction system composed of hydrogen peroxide with concentration of 1mM and reduced iron powder with dosage of 0.10g/L, 0.50g/L and 1.00g/L respectively, setting 2 parallel samples for each reduced iron powder dosage group with different concentrations, oscillating in a constant temperature oscillation box at 30 ℃ and 200rpm for 2h, filtering the reaction solution, collecting supernatant, filtering with 0.45 μm filter membrane, analyzing residual norfloxacin filtrate with high performance liquid chromatography, and analyzing residual norfloxacin filtrate with high performance liquid chromatography
Calculating the norfloxacin removal rate at different time points (where ω istThe removal rate of norfloxacin at t,%; c. C0And ctInitial norfloxacin concentration in solution and concentration at t) were averaged over 2 replicates and the results are shown in figure 4. As can be seen from fig. 4, in the norfloxacin aqueous solution with the initial concentration of 10mg/L, when the addition amount of zero-valent iron is 0.1g/L, the removal rate of norfloxacin after the reaction is finished is 36.89%, and when the addition amount of zero-valent iron is 0.5g/L, the removal rate of norfloxacin is increased to 98.84%, which indicates that more ferrous ions can be generated in the system along with the increase of the content of zero-valent iron for activating hydrogen peroxide, so that the system generates more active species such as hydroxyl radicals for removing norfloxacin; in addition, when the adding amount of the zero-valent iron is increased to 1.0g/L, the removal rate of norfloxacin after the reaction is finished is 99.60%, which shows that the removal effect of norfloxacin can be improved by increasing the amount of the zero-valent iron, but the improvement effect is not more than 1%, so that the norfloxacin pollution is avoided when the adding amount of the zero-valent iron is 0.5g/L, namely the mass concentration of iron powder is 50mg/L based on 1mg/L of norfloxacinThe dye water body has the best repairing effect.
Experimental example 3: influence of hydrogen peroxide dosage on norfloxacin polluted water body remediation effect
Adding 1mL of green tea leaf extract into a Fenton-like reaction system consisting of norfloxacin aqueous solution with an initial concentration of 10mg/L and reduced iron powder with concentrations of 1mM, 10mM and 100mM respectively and an addition amount of 0.50g/L, arranging 2 parallel samples for each hydrogen peroxide addition amount group with different concentrations, oscillating in a constant-temperature oscillation box at 30 ℃ and 200rpm for 2h, filtering the reaction solution, taking supernatant, filtering the supernatant through a 0.45 mu m filter membrane, analyzing residual norfloxacin filtrate by using high performance liquid chromatography, and utilizing the norfloxacin filtrate
Calculating the norfloxacin removal rate at different time points (where ω istThe removal rate of norfloxacin at t,%; c. C0And ctInitial norfloxacin concentration in solution and concentration at t) were averaged over 2 replicates and the results are shown in figure 5. As can be seen from FIG. 5, in the aqueous norfloxacin solution with an initial concentration of 10mg/L, the norfloxacin removal efficiency after the reaction was reduced from 98.84% to 47.66% as the dosage of hydrogen peroxide was increased from 1mM to 10mM, which is probably caused by the consumption of hydroxyl radicals in the system due to excessive hydrogen peroxide; in addition, hydrogen peroxide as an oxidizing agent consumes reducing components in the green tea extract, thereby causing a decrease in the fe (ii)/fe (iii) cycle efficiency, which is another key cause of the decrease in the norfloxacin removal rate. Further, when the amount of hydrogen peroxide added was further increased to 100mM, the removal rate of norfloxacin was 38%, again suggesting that excessive hydrogen peroxide may rather inhibit the removal of norfloxacin. Therefore, when the adding amount of the hydrogen peroxide is 1mM, namely the mass concentration of the hydrogen peroxide is 1mg/L norfloxacin, and the mass concentration of the hydrogen peroxide is 3.4mg/L, the effect of restoring the water body polluted by the norfloxacin is the best.
Comparative example: repairing condition of different systems on norfloxacin polluted water body
Collecting 1mL of green tea leaf extract (GT), 1mM hydrogen peroxide (H)2O2) 0.5g/L reduced iron powder (Fe)0) And green tea leaf extractive solution/Fe comprising 1mL of green tea leaf extractive solution and 0.5g/L of reduced iron powder0System (GT/Fe)0) Fe consisting of 1mM hydrogen peroxide and 0.5g/L reduced iron powder0/H2O2System (Fe)0/H2O2) Green tea leaf extract/Fe consisting of 1mL of green tea leaf extract, 1mM of hydrogen peroxide and 0.5g/L of reduced iron powder0/H2O2System (GT/Fe)0/H2O2) Separately treating norfloxacin aqueous solution with initial concentration of 10mg/L, setting 2 parallel samples in each group, oscillating in a constant temperature oscillation tank at 30 deg.C and 200rpm for 2h, filtering the reaction solution, collecting supernatant, filtering with 0.45 μm filter membrane, analyzing residual norfloxacin filtrate with high performance liquid chromatography, and collecting the supernatant
Calculating the norfloxacin removal rate at different time points (where ω istThe removal rate of norfloxacin at t,%; c. C0And ctInitial norfloxacin concentration in solution and concentration at t) were averaged over 2 replicates and the results are shown in figure 6. As can be seen from FIG. 6, the green tea leaf extract alone, H2O2、Fe0The norfloxacin is difficult to be removed efficiently, and the removal rates of the norfloxacin after the reaction are respectively 5.86%, 5.57% and 33.82%; at the same time, compared with Fe0Adding green tea leaf extract to Fe0In a system, the removal rate of norfloxacin is improved by 14.63 percent; however, when Fe0And H2O2When a Fenton-like system is combined and constructed, the removal rate of norfloxacin reaches 56.69%. This shows that compared to other systems, the zero-valent iron-based fenton-like system is more favorable for norfloxacin removal; furthermore, in comparison with Fe0/H2O2When in Fe0/H2O2After the green tea extract is added into the system, the removal rate of norfloxacin is obviously improved, and the removal rate of norfloxacin after the reaction is finished is improved by 42.15 percent; moreover, the introduction of the green tea leaf extract is also effectiveIncreased reaction rate, green tea leaf extract/Fe0/H2O2The reaction rate of the system for removing the norfloxacin is 0.037min-1Is about Fe0/H2O25.3 times of the system, which can show that the green tea extract can effectively promote the conversion of Fe (III) to Fe (II) in the system.
The above embodiments are preferred embodiments of the present invention, but the present invention is not limited to the above embodiments, and any other changes, modifications, substitutions, combinations, and simplifications which do not depart from the spirit and principle of the present invention should be construed as equivalents thereof, and all such changes, modifications, substitutions, combinations, and simplifications are intended to be included in the scope of the present invention.
Claims (10)
1. A restoration agent for a water body containing pollutants is characterized in that: comprises iron powder, hydrogen peroxide and plant extract.
2. The remediation agent for a contaminated water body according to claim 1, wherein: the mass concentration of the iron powder is (20-100) mg/L calculated by the pollutant with the mass concentration of 1 mg/L.
3. The remediation agent for a contaminated water body according to claim 1, wherein: the mass concentration of the hydrogen peroxide is (3-15) mg/L calculated by the pollutant with the mass concentration of 1 mg/L.
4. The remediation agent for a contaminated water body according to claim 1, wherein: the mass concentration of the plant extracting solution is (6-20) mg/L calculated by a pollutant with the mass concentration of 1 mg/L.
5. The remediation agent for a contaminated water body according to claim 1 or 2, wherein: the iron powder is micron-sized iron powder, and the particle size of the micron-sized iron powder is 10-200 mu m.
6. The remediation agent for a contaminated water body according to claim 1 or 4, wherein: the plant extract is at least one of tea extract, water hyacinth extract, eucalyptus leaf extract and grape leaf extract.
7. The remediation agent for a contaminated water body according to claim 6, wherein: the plant extractive solution is at least one selected from oolong tea extractive solution, yellow tea extractive solution, black tea extractive solution, green tea extractive solution, black tea extractive solution, and white tea extractive solution.
8. The remediation agent for a contaminated water body according to claim 6, wherein: the plant extract is deionized water plant extract.
9. The remediation agent for a contaminated water body according to any one of claims 1 to 4 or 7 to 8, wherein: the pollutant is at least one of norfloxacin, metronidazole, lincomycin and tetracycline.
10. A method for restoring a water body containing pollutants is characterized by comprising the following steps: the remediation agent for a contaminated water body containing pollutants, which is described in any one of claims 1 to 9, is added to a contaminated water body containing at least one of norfloxacin, metronidazole, lincomycin and tetracycline.
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