CN105967314A - Method for restoring organic matter polluted water body using ferrous oxalate-activated persulfate system - Google Patents
Method for restoring organic matter polluted water body using ferrous oxalate-activated persulfate system Download PDFInfo
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- CN105967314A CN105967314A CN201610482121.3A CN201610482121A CN105967314A CN 105967314 A CN105967314 A CN 105967314A CN 201610482121 A CN201610482121 A CN 201610482121A CN 105967314 A CN105967314 A CN 105967314A
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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
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F2101/00—Nature of the contaminant
- C02F2101/30—Organic compounds
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Abstract
The invention relates to a method for restoring an organic matter polluted water body using a ferrous oxalate-activated persulfate system, comprising: adding ferrous oxalate and persulfate matters into the organic matter polluted water body to restore the water body, a molar ratio of the ferrous oxalate to persulfates is 1:10-2:1. The method provides a solution to the problem that an activator in a traditional activated persulfate system is unable to be recycled, restoration efficiency is high, and the method in the application for restoring organic matter polluted water bodies has the advantages such as high efficiency, zero selectivity, environmental friendliness, and zero secondary pollution.
Description
Technical field
The invention belongs to Environmental Chemistry field, be specifically related to control and the restorative procedure of a kind of Organic Pollutants In Water, it is adaptable to
The process of the field organic wastewaters such as printing and dyeing, agricultural.
Background technology
Water is a kind of important natural resources, is the bases depended on for existence and development of the mankind.Along with China's economy, industrial or agricultural fast
Speed development, promotes large amount of sewage, garbage, chemicals etc. to be drained into continuously in natural water, causes water pollution problems
Day by day highlight.Wherein the organic pollution in water body is because of of a great variety, complicated component, and has high toxicity, difficult degradation more, holds
The features such as long property, cause a significant threat human health and social sustainable development.
Classical high-level oxidation technology outstanding feature is to be chief active group with hydroxyl radical free radical (OH).But apply in reality
In, still suffering from following two problem during OH degradable organic pollutant: it is short that (1) OH exists the time, the life-span is less than 1
μ s, it is impossible to be fully contacted with pollutant and cause the utilization rate of OH the highest；(2) some organic pollution can not be had by OH
Effect degraded.Owing to OH has disadvantage mentioned above, there has been proposed utilization in actual applications based on potentiometric titrations senior
Oxidation technology degradable organic pollutant.Persulfate activating technology is one of New Technology about Wastewater Treatment with application prospect.
It is mainly used in the process of organic wastewater, is directed to underground sewage and carries out in-situ immobilization.Relative to classical high-level oxidation technology,
Persulfate activating technology has the advantage that (1) oxidant good stability, the most volatile；(2) sulfate radical produced is freely
Base (SO4·-) there is wider pH range of application；(3) SO produced4·-Life-span (half-life is 4s) is longer than OH.
In addition, the features such as oxidability is strong, response speed fast, non-secondary pollution that it also has, the activity of generation is extremely strong
SO4·-Can be by most persistent organic pollutants mineralising or be oxidized to micro-poison or nontoxic material.Persulfate is stimulated generation
SO4·-Method mainly have thermal activation, photoactivation, alkalescence condition activation, microwave activation and transition metal ions activation etc..
In transition metal ions Fe (II) activate persulfate technology, because of Fe (II) be widely present in the environment, cheap and easy to get, environment friend
The advantage such as good becomes the excitation technique that application is the most universal.But after Fe (II) is oxidized, Fe (III)/Fe (II) circulates difficulty, and
Ferric iron easily generates iron oxide deposits, hinders the carrying out of reaction.The addition of the organic ligands such as oxammonium hydrochloride. (HA) is permissible
Stop ferric iron precipitation, effectively facilitate Fe (III)/Fe (II) circulation, but because HA is noxious substance, participate in reaction and can cause secondary
Pollute.
Summary of the invention
The technical problem to be solved is the deficiency exciting persulfate method for above-mentioned Fe (II), and provides a kind of profit
With Ferrox. (FeC2O4·2H2O) method activating the repairing organic polluted water body of persulfate (PS) system.The inventive method
Solving Fe (II) excites Fe (III) in persulfate system easily to precipitate, Fe (III)/Fe (II) difficult circulation and can not recycling
Problem, and can improve remediation efficiency, the reparation using it for Organic Pollution water body has efficiently, non-selectivity, environment friend
The advantages such as good, non-secondary pollution.
The present invention solves that the technical scheme that problem set forth above is used is:
One utilizes the method for the Ferrox. activation repairing organic polluted water body of persulfate (PS) system, it is characterised in that:
Organic Pollution water body to be repaired adds Ferrox., persulfate material, carries out the reparation of Organic Pollution water body.Described
Ferrox. be the material being insoluble in water, size is not restricted；Described Ferrox. with the mol ratio of persulfate is
1:10～2:1.
By such scheme, it is 3～10 that the pH value of described system controls.
By such scheme, described system in Organic Pollution water body to be repaired after addition persulfate, Ferrox. material
When pH value is less than or exceedes required pH value, add the pH value of inorganic base or mineral acid regulation system for setting pH value.
By such scheme, described mineral acid can be selected for hydrochloric acid, sulphuric acid etc..
By such scheme, described Ferrox. concentration in system is 0.5-2mmol/L；Described persulfate is in system
Concentration is 1-5 mM/l.Comparatively speaking, persulfate concentration is the highest, and response speed is the fastest.
By such scheme, after described addition persulfate, system is stirred, makes solution be sufficiently mixed, then repair.
System is not stirred, it is also possible to obtain better effects.
By such scheme, described Organic substance includes but not limited to G-30027, alachlor, tetracycline, norfloxacin, rhodamine
B。
The know-why of the present invention: there is Fe (III) in the persulfate system of ferrous ion activation at present and easily precipitate,
The difficult circulation of Fe (III)/Fe (II) and can not recycling, and remediation efficiency need the problem that improves, and the method utilizes oxalic acid
Ferrous activation persulfate (PS) anabolic reaction system carries out the reparation of Organic Pollution water body, can adsorb over cure by Ferrox.
Hydrochlorate, causes persulfate to be excited to persulfate transmission electronics, produces strong oxidizing property SO4·-, itself and water or hydroxyl
Effect produces strong oxidizing property OH, SO4·-Can degrade to non-selectivity the high toxicity in water body with OH, persistency organic contaminant
Thing such as G-30027, alachlor, tetracycline, norfloxacin, rhodamine B etc..During degradable organic pollutant, solution
In only detect the Fe (III) of trace, it was demonstrated that the process of activation persulfate is mainly carried out on Ferrox. surface.By synchronizing
Radiation X ray Absorption Fine Structure proves, the Fe (III) that course of reaction mesoxalic acid ferrous iron surface produces can be at Ferrox. mesoxalic acid
It is reduced to Fe (II) under group effect, promotes Ferrox. surface Fe (III)/Fe (II) circulation, improve remediation efficiency, solve general
Utilize the problem that ferrous ion is difficult to when activating circulate.Although persulfate has certain reproducibility, it is possible to be reduced to Fe (II),
But its reaction rate is very slow, and this process can be ignored.Compared with other indissoluble ferrous salt, Ferrox. activation persulfate degraded
Persistence organic pollutant in hgher efficiency.
It is an advantage of the current invention that:
1, the present invention uses Ferrox. as persulfate activator, can not only activate persulfate and produce strong oxidizing property
SO4·-, to organic pollutant degradation non-selectivity, efficiency is high.The Fe (III) that oxidation produces can be by the oxalic acid group in system
It is reduced to Fe (II), thus promotes Fe (III)/Fe (II) circulation.
2, during Ferrox. is widely present in environment, and it is readily synthesized, environmentally friendly, repetition profit can be reclaimed after reaction
With, do not result in secondary pollution.
3, reaction condition is gentle, and normal temperature and pressure gets final product fast reaction, it is not necessary to complex appts, simple to operate, without dangerous, and nothing
Professional need to be engaged to operate.
4, relatively wide by the Ferrox. activation persulfate system pH scope of application, between pH 3-10, there is well activation
Effect.
Accompanying drawing explanation
Fig. 1 is G-30027 design sketch in the inventive method pollution administration water body；
Fig. 2 is tetracycline design sketch in the inventive method pollution administration water body；
Fig. 3 is that the inventive method utilizes variable concentrations Ferrox. activation persulfate degraded tetracycline design sketch.
Fig. 4 is that the inventive method utilizes Ferrox. activation variable concentrations persulfate degraded tetracycline design sketch.
Fig. 5 is norfloxacin design sketch in the inventive method pollution administration water body；
Fig. 6 is rhodamine B design sketch in the inventive method pollution administration water body；
Fig. 7 is the inventive method design sketch of tetracycline in pollution administration water body under the conditions of the initial pH of difference；
Fig. 8 is that the inventive method utilizes the design sketch of tetracycline in recovery Ferrox. activation persulfate pollution administration water body；
Fig. 9 be the inventive method utilize the Ferrox. that reclaims after tetracycline in Ferrox. activation persulfate pollution administration water with
X-ray diffraction (XRD) collection of illustrative plates of Ferrox. before reaction.
Figure 10 is that the inventive method utilizes the Ferrox. reclaimed after tetracycline in Ferrox. activation persulfate pollution administration water
With scanning electron microscope (SEM) collection of illustrative plates of Ferrox. before reaction.
Figure 11 is that the inventive method utilizes synchrotron radiation X-ray near side (ns) Absorption Fine Structure to prove the circulation of Ferrox. Surface Fe.
Figure 12 is that the inventive method utilizes Ferrox. activation persulfate and ferrous sulfate activation persulfate pollution administration water body
The design sketch of middle tetracycline.
Figure 13 is that the inventive method utilizes variety classes slightly soluble ferrous salt activation persulfate degraded tetracycline design sketch.
Detailed description of the invention
Below by being embodied as case to describe the summary of the invention of the present invention in detail, described specific embodiment is only in order to explain
The present invention, is not intended to limit the present invention.
Embodiment 1 administers the sewage containing G-30027
For the reparation at pollution by pesticides water source, the G-30027 aqueous solution with concentration as 20mg/L is as simulated wastewater.Delivery is intended useless
Water 50mL, is added thereto to persulfate, Ferrox. so that it is concentration is respectively 1.0 and 0.5mmol/L, adds over cure
System original ph after hydrochlorate and Ferrox. is 5.2, it is not necessary to additionally regulate pH, makes solution mix by magnetic stirrer
Closing uniformly, rotating speed is 400rpm.Simultaneously to be not added with persulfate or Ferrox. as controlled trial, result is shown in Fig. 1.Fig. 1
Shown in, reacting 10min, atrazine degradation rate has reached 94%；When reaction extends to 30min, atrazine degradation rate
Reach 100%.
Embodiment 2 administers the sewage containing tetracycline
For the reparation of antibiotic polluted source, the tetracycline aqueous solution with concentration as 20mg/L is as simulated wastewater.Delivery is intended useless
Water 50mL, is added thereto to Ferrox., persulfate so that it is concentration is respectively 0.5 and 1.0mmol/L, adds over cure
System original ph after hydrochlorate and Ferrox. is 5.2, it is not necessary to additionally regulate pH, makes solution mix by magnetic stirrer
Closing uniformly, rotating speed is 400rpm.Simultaneously to be not added with persulfate or Ferrox. as controlled trial, result is shown in Fig. 2.Fig. 3
Shown in, reacting 20min, tetracycline degradation rate has reached 94%；When reaction extends to 30min, and tetracycline degradation rate reaches
100%.
In the case of persulfate concentration remains 1.0mmol/L, adjust Ferrox. concentration, repeat above-mentioned test, specifically
Result is shown in Fig. 3.Shown in Fig. 3, in the case of Ferrox. concentration is 0.25mmol/L (Ferrox. and persulfate mole
Ratio is 1:4), react 30min, tetracycline degradation rate reaches 80%.When Ferrox. concentration is for being more than or equal to
In the case of 0.5mmol/L (Ferrox. is more than or equal to 1:2 with the mol ratio of persulfate), reacting 30min, tetracycline drops
Solution rate has all reached 100%.
In the case of Ferrox. concentration remains 0.5mmol/L, adjust persulfate concentration, repeat above-mentioned test, specifically
Result is shown in Fig. 4.Shown in Fig. 4, persulfate concentration is (Ferrox. and the mol ratio of persulfate in the case of 1-5mmol/L
For 1:2-1:10), react 30min, tetracycline effect is all up 100% substantially.
Embodiment 3 administers the sewage containing norfloxacin
For the reparation of antibiotic polluted source, the norfloxacin aqueous solution with concentration as 20mg/L is as simulated wastewater.Delivery is intended
Waste water 50mL, is added thereto to Ferrox., persulfate so that it is concentration is respectively 0.5 and 1.0mmol/L, adds
System original ph after sulfate and Ferrox. is 5.2, it is not necessary to additionally regulates pH, makes solution by magnetic stirrer
Mix homogeneously, rotating speed is 400rpm.Simultaneously to be not added with persulfate or Ferrox. as controlled trial, result is shown in Fig. 5.Fig. 5
Shown in, after reaction 2min, norfloxacin degradation rate has reached 84%；When reaction extends to 10min, norfloxacin degradation rate
Reach 100%.
Embodiment 4 administers the sewage containing rhodamine B
For the reparation of antibiotic polluted source, the rhodamine B aqueous solution with concentration as 20mg/L is as simulated wastewater.Delivery is intended
Waste water 50mL, is added thereto to Ferrox., persulfate so that it is concentration is respectively 0.5 and 1.0mmol/L, adds
System original ph after sulfate and Ferrox. is 5.2, it is not necessary to additionally regulates pH, makes solution by magnetic stirrer
Mix homogeneously, rotating speed is 400rpm.Simultaneously to be not added with persulfate or Ferrox. as controlled trial, result is shown in Fig. 6.Fig. 6
Shown in, after reaction 2min, rhodamine B degradation rate has reached 80%；When reaction extends to 10min, and rhodamine B is degraded
Rate has reached 100%.
Embodiment 5 administers the sewage containing antibiotic tetracycline under different pH condition
Tetracycline aqueous solution with concentration as 20mg/L, as simulated wastewater, takes simulated wastewater 50mL, is added thereto to persulfuric acid
Salt so that it is concentration is respectively 1.0mmol/L, is then respectively 3 with the initial pH of hydrochloric acid or sodium hydrate regulator solution, and 5,7,
9,10, it is separately added into Ferrox. the most again, the concentration making system mesoxalic acid ferrous is 0.5mmol/L, carries out simulated wastewater
Oxidation processes, result is shown in Fig. 7, as it is shown in fig. 7, after processing 15 minutes, the degradation rate of tetracycline in waste water under different pH value
All reach more than 70%.
Embodiment 6 reclaims Ferrox. activation persulfate and administers the pollution containing tetracycline
Tetracycline aqueous solution with concentration as 20mg/L, as simulated wastewater, takes simulated wastewater 50mL, is added thereto to oxalic acid sub-
Ferrum, persulfate so that it is concentration is respectively 0.5 and 1.0mmol/L, add the system after persulfate and Ferrox. initial
PH value is 5.2, it is not necessary to additionally regulate pH, makes solution mix homogeneously by magnetic stirrer, and rotating speed is 400rpm.Oxalic acid
Ferrous iron recycles 5 times altogether, and result is shown in Fig. 8.Shown in Fig. 8, after Ferrox. reclaims 5 times, react 30min, tetracycline
Degradation rate has reached 100%.The oxalic acid can being recycled by X-ray diffraction (XRD) and scanning electron microscope (SEM)
The structure of ferrous Ferrox. front with reaction and pattern, result is shown in Fig. 9 and Figure 10.Shown in Fig. 9, the Ferrox. knot of recovery
Structure is still the Ferrox. that crystallinity is good.Shown in Figure 10, the Ferrox. pattern of recovery maintains the fundamental form before reaction
Looks and size.The Ferrox. variation of valence in reaction, result is recorded by synchrotron radiation X-ray near side (ns) Absorption Fine Structure
See Figure 11.Shown in Figure 11, after adding persulfate, Ferrox. is oxidized, generates high-valence state Fe (III), after having reacted
Fe (III) in Ferrox. is reduced to again lower valency Fe (II).
Embodiment 8 Ferrox. activation persulfate administers, with ferrous sulfate activation persulfate, the contrast polluted containing tetracycline
Tetracycline aqueous solution with concentration as 20mg/L, as simulated wastewater, takes simulated wastewater 50mL, is added thereto to persulfuric acid
Salt, Ferrox. or ferrous sulfate so that it is concentration is respectively 1.0 and 0.5mmol/L, add persulfate and Ferrox. or
System original ph after ferrous sulfate is 5.2, it is not necessary to additionally regulate pH, makes solution mixing all by magnetic stirrer
Even, rotating speed is 400rpm.Result is shown in Figure 12.Shown in Figure 12, in adding the system of persulfate and Ferrox., instead
20min, tetracycline degradation rate is answered to reach 94%；When reaction extends to 30min, and tetracycline degradation rate has reached 100%.
In adding the system of persulfate and ferrous sulfate, reacting 20min, tetracycline degradation rate has reached 70%；When reaction extends
To 30min, tetracycline degradation rate has reached 72%.
Embodiment 9 variety classes slightly soluble ferrous salt activation persulfate degraded tetracycline effect contrast figure
Tetracycline aqueous solution with concentration as 20mg/L, as simulated wastewater, takes simulated wastewater 50mL, is added thereto to persulfuric acid
Salt so that it is concentration is 1.0mmol/L, adds Ferrox. or ferrous carbonate or ferrous phosphate so that it is concentration is 0.5
Mmol/L, regulation system original ph is 5.2, makes solution mix homogeneously by magnetic stirrer, and rotating speed is 400rpm.
Result is shown in Figure 13.Shown in Figure 13, in adding the system of persulfate and Ferrox., reacting 20min, tetracycline is degraded
Rate has reached 94%；When reaction extends to 30min, and tetracycline degradation rate has reached 100%.Adding persulfate and carbonic acid
In ferrous system, reacting 20min, tetracycline degradation rate has reached 24%；When reaction extends to 30min, and tetracycline drops
Solution rate has reached 21%.In adding the system of persulfate and ferrous phosphate, reacting 20min, tetracycline degradation rate reaches
21%；When reaction extends to 30min, and tetracycline degradation rate has reached 27%.
Claims (7)
1. the method utilizing the Ferrox. activation repairing organic polluted water body of persulfate system, it is characterised in that: treating
Repairing organic polluted water body adds Ferrox., persulfate material, carries out the reparation of Organic Pollution water body, described grass
Ferrous and persulfate the mol ratio of acid is 1:10～2:1.
The method utilizing the Ferrox. activation repairing organic polluted water body of persulfate system the most according to claim 1,
It is characterized in that: it is 3～10 that the pH value of described system controls.
The method utilizing the Ferrox. activation repairing organic polluted water body of persulfate system the most according to claim 1,
It is characterized in that: the pH of described system in Organic Pollution water body to be repaired after addition persulfate, Ferrox. material
When value is less than or exceedes required pH value, add the pH value of inorganic base or mineral acid regulation system for setting pH value.
The method utilizing the Ferrox. activation repairing organic polluted water body of persulfate system the most according to claim 1,
It is characterized in that: described mineral acid can be selected for hydrochloric acid, sulphuric acid.
The method utilizing the Ferrox. activation repairing organic polluted water body of persulfate system the most according to claim 1,
It is characterized in that: described Ferrox. concentration in system is 0.5-2mmol/L；Described persulfate concentration in system
For 1-5 mM/l.
The method utilizing the Ferrox. activation repairing organic polluted water body of persulfate system the most according to claim 1,
It is characterized in that: after described addition persulfate, system is stirred, makes solution be sufficiently mixed, then repair.The most right
System is stirred, it is also possible to obtain better effects.
The method utilizing the Ferrox. activation repairing organic polluted water body of persulfate system the most according to claim 1,
It is characterized in that: described Organic substance includes but not limited to G-30027, alachlor, tetracycline, norfloxacin, rhodamine B.
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107140724A (en) * | 2017-05-23 | 2017-09-08 | 湖南工程学院 | A kind of method that the MOFs of Co containing In absorption cooperates with Antibiotics of Low Concentration in water removal with activation persulfate |
| CN107265602A (en) * | 2017-07-25 | 2017-10-20 | 华中师范大学 | It is neutral to alkaline heterophase Fenton method for treating water |
| CN107352633A (en) * | 2017-08-30 | 2017-11-17 | 北京师范大学 | A kind of method of Atrazine in iron aluminium mud activation potassium hydrogen peroxymonosulfate degradation water |
| CN108191036A (en) * | 2017-12-20 | 2018-06-22 | 湖南大学 | A kind of method of Atrazine in activation peroxy-monosulfate degradation water body using potassium ferrate |
| CN110745982A (en) * | 2019-09-12 | 2020-02-04 | 生态环境部华南环境科学研究所 | Method for deep oxidation treatment of organic wastewater based on visible light assisted complexing iron ion activated monoperoxybisulfate |
| CN114560549A (en) * | 2022-02-28 | 2022-05-31 | 中国科学技术大学 | Application of synthetic ferrihydrite in advanced oxidation process water treatment |
| CN116020854A (en) * | 2023-02-03 | 2023-04-28 | 天津大学 | Method for treating waste plastics based on persulfate system |
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| CN102249378A (en) * | 2011-07-19 | 2011-11-23 | 武汉大学 | Method for treating organic waste water by using electrochemistry under assistance of persulfate |
| CN102259993A (en) * | 2011-06-27 | 2011-11-30 | 华南理工大学 | Water treatment method utilizing complex-ferrous-activated persulfate oxidation |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| CN102259993A (en) * | 2011-06-27 | 2011-11-30 | 华南理工大学 | Water treatment method utilizing complex-ferrous-activated persulfate oxidation |
| CN102249378A (en) * | 2011-07-19 | 2011-11-23 | 武汉大学 | Method for treating organic waste water by using electrochemistry under assistance of persulfate |
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| CN107140724A (en) * | 2017-05-23 | 2017-09-08 | 湖南工程学院 | A kind of method that the MOFs of Co containing In absorption cooperates with Antibiotics of Low Concentration in water removal with activation persulfate |
| CN107140724B (en) * | 2017-05-23 | 2020-12-08 | 湖南工程学院 | Method for removing low-concentration antibiotics In water by virtue of adsorption and persulfate activation of MOFs containing In-Co |
| CN107265602A (en) * | 2017-07-25 | 2017-10-20 | 华中师范大学 | It is neutral to alkaline heterophase Fenton method for treating water |
| CN107352633A (en) * | 2017-08-30 | 2017-11-17 | 北京师范大学 | A kind of method of Atrazine in iron aluminium mud activation potassium hydrogen peroxymonosulfate degradation water |
| CN108191036A (en) * | 2017-12-20 | 2018-06-22 | 湖南大学 | A kind of method of Atrazine in activation peroxy-monosulfate degradation water body using potassium ferrate |
| CN110745982A (en) * | 2019-09-12 | 2020-02-04 | 生态环境部华南环境科学研究所 | Method for deep oxidation treatment of organic wastewater based on visible light assisted complexing iron ion activated monoperoxybisulfate |
| CN114560549A (en) * | 2022-02-28 | 2022-05-31 | 中国科学技术大学 | Application of synthetic ferrihydrite in advanced oxidation process water treatment |
| CN116020854A (en) * | 2023-02-03 | 2023-04-28 | 天津大学 | Method for treating waste plastics based on persulfate system |
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