CN107540062B - Method for removing diclofenac in water by ferrite magnetic nanoparticles - Google Patents
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Abstract
The invention relates to a method for removing diclofenac in water by ferrite magnetic nanoparticles, which is characterized by comprising the following steps: (1) adjusting the pH value of the water body to be treated, and adding ferrite magnetic nanoparticles; (2) stirring and fully mixing to perform adsorption reaction; (3) after the adsorption balance is achieved, solid-liquid separation is carried out by adopting a method of an external magnetic field, and the diclofenac in the water body to be treated is removed. Compared with the prior art, the method utilizes the characteristic that the ferrite magnetic nanoparticles have large specific surface area to adsorb diclofenac, has high removal efficiency, can be quickly separated and recycled from water through an external magnetic field due to the magnetic property of the ferrite magnetic nanoparticles, has no secondary pollution, has wide application prospect in the aspect of removing trace diclofenac pollutants in drinking water or sewage, and provides an effective method for the reinforced removal technology of the trace diclofenac pollutants in environmental water.
Description
Technical Field
The invention belongs to the technical field of environmental protection and water treatment, and relates to a method for removing diclofenac in water by ferrite magnetic nanoparticles.
Background
In recent years, drugs and personal care products (PPCPs) are receiving more and more attention as environmental ecological risks caused by a novel class of pollutants, wherein Diclofenac (Diclofenac, DFC) is widely used as a non-steroidal anti-inflammatory drug for relieving pain, resisting arthritis, treating rheumatism and the like.
There have been many reports on the removal of trace amount of drugs in water by using membrane filtration, advanced oxidation and adsorptive separation. However, the technologies such as membrane filtration and advanced oxidation not only increase the cost of sewage treatment, but also are easily inhibited by interfering substances in the water environment, so that the removal rate of diclofenac is reduced, and meanwhile, the advanced oxidation technology easily generates intermediate products with stronger toxicity, thereby causing secondary pollution. The adsorption method is widely applied to removing trace organic pollutants in various water bodies such as sewage, surface water, underground water, drinking water and the like at present. For example, researchers have used adsorbents such as carbon-based materials, synthetic resins, and molecularly imprinted polymers to remove drug compounds from water. However, due to their high cost, difficulty in separation and regeneration, the wide use of these adsorbents is limited. Therefore, how to remove the trace amount of diclofenac in the water body with high efficiency is a technical problem to be solved seriously.
In this regard, the use of magnetic nanomaterials would be an economical and efficient alternative due to the simple synthesis and operation. Most of the magnetic nano materials applied in the current environmental field are ferrites (shown in a general formula MFe)2O4Expressed, where M is generally a divalent metal ion), although ferrites are mainly used in the fields of inductors, transformers, gas sensors, photocatalysts, etc., they are considered as potential adsorbents for removing trace amounts of drugs in water bodies due to their high adsorption performance to various pollutants due to their large specific surface area, abundant surface functional groups and high saturation magnetization. For example, magnetite (Fe)3O4) The nanoparticles are used for adsorbing tetracycline, sulfonamide compounds and the like in water. In addition, the ferrite magnetic nanoparticles have higher stability in an acidic medium, which allows the adsorption reaction to be carried out in a wider pH range; and the ferrite magnetic nanoparticles adsorbed with the drug compound can be separated by an external magnetic fieldAnd the regeneration (solvent elution or high-temperature heating) is carried out under certain conditions, so that the repeated utilization of the adsorption material is realized.
Chinese patent CN102125848A discloses a method for degrading organic pollutants by using a magnetic heterogeneous photo-fenton catalyst, which comprises the following steps: placing an organic contaminant solution in a reaction vessel; adding a proper amount of oxalic acid into a reaction container; adding a proper amount of magnetic heterogeneous photo-Fenton catalyst into a reaction container; carrying out photocatalytic reaction under the irradiation of visible ultraviolet light. The patent mainly utilizes the photocatalysis performance of nickel ferrite as a magnetic heterogeneous photo-Fenton catalyst to degrade organic pollutants in water, and an additional ultraviolet light source is needed in the degradation process to increase energy consumption and cost, and secondary pollutants are easily generated.
Disclosure of Invention
The invention aims to overcome the defects of the prior art and provide a method for removing diclofenac in water by using ferrite magnetic nanoparticles.
The purpose of the invention can be realized by the following technical scheme:
a method for removing diclofenac in water by ferrite magnetic nanoparticles comprises the following steps:
(1) adjusting the pH value of the water body to be treated, and then putting the ferrite magnetic nanoparticles into the water body to be treated;
(2) stirring and fully mixing the ferrite magnetic nanoparticles and the water body to be treated, and carrying out adsorption reaction;
(3) after the adsorption balance is achieved, solid-liquid separation is carried out by adopting a method of an external magnetic field, and the diclofenac in the water body to be treated is removed.
Preferably, the ferrite magnetic nanoparticles are nickel ferrite magnetic nanoparticles or manganese ferrite magnetic nanoparticles.
Through studying the adsorption of diclofenac in water by various ferrites, other ferrites (such as ZnFe) are discovered2O4、CoFe2O4、CuFe2O4) The adsorption of diclofenac is greatly influenced by the pH value of water, the removal rate is basically 100% when the pH value is 2, and once the pH value is increased, the removal rate is reducedThe pH value is in the range of 4-10, and the diclofenac removal rate is only 10% -45%. The nickel ferrite magnetic nanoparticles and the manganese ferrite magnetic nanoparticles selected by the application have higher adsorption effect within a wider pH value range. The adsorption reaction is fast, the exothermic reaction is adopted, the adsorption principle is physical adsorption, the adsorption process is slightly influenced by pH, so that the diclofenac is adsorbed on the surface of the ferrite mainly under the action of hydrogen bond or van der Waals force instead of electrostatic force, and the strong adsorption effect mainly depends on the large specific surface area of the ferrite. Preferably, the particle size of the ferrite magnetic nanoparticles is 30-50 nm.
Preferably, the pH value of the water body to be treated is adjusted to 2-10 by sodium hydroxide or hydrochloric acid in the step (1).
Further preferably, the pH value of the water body to be treated is adjusted to 2-4 by sodium hydroxide or hydrochloric acid in the step (1).
pKa of diclofenac is 4.2, pH of diclofenac<4 is in molecular form. Correspondingly, the smaller the pH value of the water body to be treated is, the less the H adsorbed on the surface of the ferrite magnetic nano-particles+The more ions, the more hydrogen bonds are formed between the ferrite magnetic nanoparticles and the diclofenac molecules, the more diclofenac molecules are adsorbed by the ferrite magnetic nanoparticles, and the better the adsorption effect is. Therefore, it is further preferable that the pH value of the water body to be treated in step (1) is adjusted to 2 to 4 with sodium hydroxide or hydrochloric acid.
Preferably, the concentration of diclofenac in the water body to be treated is 1-10 mg/L.
When the addition amount of the ferrite magnetic nanoparticles is 0.5 mg/L, the removal rate of the diclofenac reaches more than 90% when the concentration of the diclofenac in a water sample is 10 mg/L, but when the addition amount is more than 0.5 g/L0, the addition amount of the ferrite magnet is increased, the removal rate of the diclofenac is not obviously increased, and when the addition amount is more than 0.5 g/L, the addition amount of the ferrite magnet is continuously increased, the removal rate of the diclofenac is not obviously increased, and similarly, when the concentration of the diclofenac in the water sample to be treated is 1 mg/L, the addition amount is less than 0.1 g/L, when the addition amount of the ferrite magnet is increased, the removal rate of the diclofenac is increased, when the addition amount is 0.1 g/4934, the addition amount of the ferrite magnetic nanoparticles is more than 90%, but the addition amount of the ferrite magnetic nanoparticles is less than 0.1 g/8297, the addition amount of the ferrite magnetic nanoparticles is more than 0.1 g/L, the removal rate of the ferrite magnetic nanoparticles is more than 90%, but the addition amount of the ferrite magnetic magnet is less than 0.1 mg/1, the addition amount of the ferrite magnetic magnet to be treated, so that the ferrite magnetic nanoparticles is not increased, and the addition amount of the ferrite magnetic nanoparticles is more than 0.5 g/355-10, the ferrite magnetic concentration of the ferrite magnetic magnet is more favorable, and the ferrite magnetic concentration of the ferrite magnetic nanoparticles is not increased, so that the ferrite magnetic nanoparticles is more favorable for the ferrite magnetic concentration of the ferrite magnetic nanoparticles is increased, and the ferrite magnetic concentration of the ferrite.
Preferably, the adsorption reaction in the step (2) is carried out at 25-35 ℃, the stirring speed is 30-100rmp, and the reaction time is 1-2 h.
The reaction time of the process parameters is short, strong stirring strength is not needed, a good removing effect can be achieved at normal temperature, energy consumption is saved, and the economic applicability of the method is further embodied. Preferably, the water to be treated comprises sewage, effluent of a sewage treatment plant, surface water or drinking water.
Compared with the prior art, the invention has the following beneficial effects:
(1) wide application range and simple and easy reaction condition. The method adds ferrite magnetic nanoparticles into a water sample to be treated containing diclofenac, has unlimited reaction temperature, and can achieve good removal effect at normal temperature and normal pressure.
(2) The reaction rate is high, the adopted ferrite magnetic nano particles are 30-50nm, and have huge specific surface area and high activity, so the reaction rate is high, the water sample containing 1-10 mg/L of diclofenac can be well removed within 5 minutes, and the removal rate reaches more than 95%.
(3) When the technology is used for removing diclofenac in a water sample, the influence of the pH value of the water sample and natural organic matters (humic acid concentration is 0-20 mg/L) is small.
(4) The ferrite magnetic nanoparticles used in the technology have strong saturation magnetization, and after pollutants are adsorbed, the materials are easily separated from a water body in a short time through an external magnetic field and then recycled.
(5) Low treatment cost and environmental protection. Compared with other adsorbents, the ferrite magnetic nanoparticles used in the invention are cheap and easily available, the treatment process is simple and easy, an additional ultraviolet source and the like are not needed, and secondary pollution to the environment is avoided.
(6) The application range of the target is wide. The invention is suitable for diclofenac-containing sewage, and is also suitable for environmental water bodies such as surface water, underground water, drinking water and the like.
Drawings
FIG. 1 is a graph showing the adsorption kinetics of manganese ferrite and nickel ferrite on diclofenac acid;
FIG. 2 is the effect of pH on the adsorption of diclofenac by manganese ferrite and nickel ferrite;
FIG. 3 is the effect of humic acid on the adsorption of diclofenac by manganese ferrite and nickel ferrite;
FIG. 4 shows the result of reusing diclofenac removed from ferrite of manganese and nickel.
Detailed Description
The invention is described in detail below with reference to the figures and specific embodiments.
Example 1
Nickel ferrite (NiFe)2O4) Magnetic nano-particle diclofenac removing method in sewage
Adding a diclofenac wastewater sample containing 10 mg/L into a centrifugal tube, adjusting the pH value of the water sample to 4 +/-0.2 by using sodium hydroxide or hydrochloric acid, then adding nickel ferrite magnetic nanoparticles with the addition of 0.5 g/L, carrying out oscillation reaction at the speed of 30rpm for 2 hours at room temperature, separating the nickel ferrite magnetic nanoparticles by using a magnet after adsorption balance, and analyzing the concentration of diclofenac in the treated water sample by using a high performance liquid chromatograph, wherein the removal rate reaches 98.8%.
Example 2
Manganese ferrite (MnFe)2O4) Magnetic nano-particle diclofenac removing from surface water
The method of example 1 is used, except that the treated water sample is surface water, the adsorbent is manganese ferrite magnetic nanoparticles, the pH value of the water sample is adjusted to 6 +/-0.2 by sodium hydroxide or hydrochloric acid, and the diclofenac concentration in the treated water sample is analyzed by a high performance liquid chromatograph, so that the removal rate is 93.9%.
Example 3
Diclofenac removal from drinking water by nickel ferrite magnetic nanoparticles
The method of example 1 is used, except that the treated water sample is drinking water and standard water sample, the concentration of diclofenac is 1.5 mg/L, the adding amount of the nickel ferrite magnetic nanoparticles is 0.1 g/L, the pH value of the water sample is adjusted to 7 +/-0.2 by sodium hydroxide or hydrochloric acid, and the diclofenac concentration in the treated water sample is analyzed by a high performance liquid chromatograph, so that the removal rate is more than 99.6%.
Experiments and analysis tests show that when the nickel ferrite and the manganese ferrite remove diclofenac acid in a water sample, the reaction rate is high, the influence of the pH value of the water sample and natural organic matters (the concentration of humic acid is 0-20 mg/L) is small, and the sodium ferrite and the manganese ferrite can be repeatedly utilized, and the specific experimental conditions are as follows:
(1) adsorption kinetics of ferrite magnetic nanoparticles for removing diclofenac in water
Taking a nickel ferrite as an example, a series of water samples containing 10 mg/L of diclofenac acid are respectively taken and put into a centrifuge tube, the pH value of the water samples is adjusted to 6 +/-0.2 by sodium hydroxide or hydrochloric acid, 0.5 g/L of the nickel ferrite is respectively added, the reaction time is respectively 2min, 5min, 10min, 20min, 30min, 60min, 90min and 120min under the room temperature condition and the rotating speed of 30rpm/min, the mixed solution is separated by an external magnetic field, and the concentration of the diclofenac acid in the supernatant is measured by a high performance liquid chromatograph.
(2) Diclofenac in water removed by ferrite magnetic nanoparticles under different pH values
Taking a nickel ferrite as an example, a series of water samples containing diclofenac 10 mg/L are respectively taken and loaded into a centrifugal tube, the pH value of the water samples is respectively adjusted to 2, 4, 5, 6, 7, 8 and 10 by using sodium hydroxide or hydrochloric acid, 0.5 g/L of the nickel ferrite is simultaneously and respectively added, the adsorption time is 2h under the condition of room temperature and 30rpm, after the mixed solution is separated by an external magnetic field, the concentration of the diclofenac in supernatant is measured by using a high performance liquid chromatograph, the operation steps of the manganese ferrite are the same as above, the result is shown in figure 2, the removal rate of the nickel ferrite on the diclofenac is maintained at 96-100% within the range of pH value of 2-8, the removal rate of the manganese ferrite on the diclofenac is maintained at 88-100%, when the pH value is 10, although the removal rate of the nickel ferrite on the diclofenac is reduced, the removal rate can still reach 82.4%, and within the range of the whole pH value of 2-10, the dissolution of the iron ferrite is basically not achieved, the spinel structures of the two kinds of ferrite in the range of pH value 2-10, the water samples are further, the stable, and the pH value of the water samples can be still achieved by a wide and the method, even if the pH value of the water samples are stable reaction process, the pH value of the water samples, the method is still, the method can be used.
(3) Diclofenac in water removed by ferrite magnetic nanoparticles in the presence of natural organic matters (humic acid)
Taking a nickel ferrite as an example, a series of water samples containing 10 mg/L of diclofenac acid are respectively taken and put into a centrifuge tube, sodium hydroxide or hydrochloric acid is used for adjusting the pH value of the water samples to 6 +/-0.2, 2 mg/L, 5 mg/L, 8 mg/L, 10 mg/L, 15 mg/L and 20 mg/L of humic acid and 0.5 g/L of nickel ferrite are respectively added, the adsorption time is 2 hours at the room temperature and the rotating speed of 30rpm/min, a high performance liquid chromatograph is used for measuring the concentration of the diclofenac acid in a supernatant after the mixed liquid is separated by an external magnetic field, the operation steps of the manganese ferrite are the same as the above, the influence of the humic acid (the concentration range: 0-20 mg/L) on the adsorption of the diclofenac acid on the nickel ferrite and the manganese ferrite is found to be small (fig. 3), which shows that the natural organic matters in the water sample of the environment are less influenced when the nickel ferrite and the manganese ferrite are used.
From the above, the method for removing the trace amount of diclofenac in the natural water body by adopting the magnetic nanoparticles of the nickel ferrite and the manganese ferrite has the advantages of simple operation, no secondary pollution, energy conservation and environmental protection, high reaction rate, adsorption balance within 5 minutes, removal rate of more than 90, no influence of the pH value of a water sample and natural organic matters (humic acid concentration of 0-20 mg/L), high removal rate of more than 90 percent when the diclofenac with concentration range of 1-10 mg/L is treated, and strong practicability, and huge economic and social benefits.
(4) Influence of repeated use times of nickel ferrite and manganese ferrite on removal rate of tellurium-containing wastewater
Taking a nickel ferrite as an example, taking a water sample to be treated with the diclofenac concentration of 10 mg/L, 10m L, adding 0.5 g/L of the nickel ferrite, adjusting the pH value of the wastewater to be 6 +/-0.2 by using sodium hydroxide or hydrochloric acid, adsorbing for 2 hours at the rotating speed of 30rpm, separating the mixed solution by using an external magnetic field, and then measuring the concentration of the diclofenac in the supernatant by using a high performance liquid chromatograph.
Example 4
This example is substantially the same as example 1 except that diclofenac removal from wastewater was carried out at a temperature of 35 ℃.
Example 5
This example is substantially the same as example 1 except that diclofenac removal from wastewater was carried out at a temperature of 30 ℃.
Example 6
This example is substantially the same as example 1 except that the stirring speed in this example was 100rpm and the reaction time was 1 hour.
Example 7
This example is essentially the same as example 1, except that the stirring speed in this example was 50rpm and the reaction time was 1.5 h.
Example 8
The present embodiment is substantially the same as embodiment 1, except that the water sample in the present embodiment is effluent from a sewage treatment plant.
The above-mentioned nickel ferrite and manganese ferrite magnetic nanoparticles may be commercially available or self-made ferrite magnetic nanoparticles, and the particle size is preferably 30 to 50 nm.
The embodiments described above are described to facilitate an understanding and use of the invention by those skilled in the art. It will be readily apparent to those skilled in the art that various modifications to these embodiments may be made, and the generic principles described herein may be applied to other embodiments without the use of the inventive faculty. Therefore, the present invention is not limited to the above embodiments, and those skilled in the art should make improvements and modifications within the scope of the present invention based on the disclosure of the present invention.
Claims (7)
1. A method for removing diclofenac in water by ferrite magnetic nanoparticles is characterized by comprising the following steps:
(1) adjusting the pH value of the water body to be treated, and then putting the ferrite magnetic nanoparticles into the water body to be treated;
(2) stirring and fully mixing the ferrite magnetic nanoparticles and the water body to be treated, and carrying out adsorption reaction;
(3) after the adsorption balance is achieved, solid-liquid separation is carried out by adopting a method of an external magnetic field, and the diclofenac in the water body to be treated is removed;
the ferrite magnetic nanoparticles are nickel ferrite magnetic nanoparticles or manganese ferrite magnetic nanoparticles.
2. The method for removing diclofenac acid in water by using ferrite magnetic nanoparticles as claimed in claim 1, wherein the particle size of the ferrite magnetic nanoparticles is 30-50 nm.
3. The method for removing diclofenac acid from water by using ferrite magnetic nanoparticles as claimed in claim 1, wherein in step (1), the pH value of the water body to be treated is adjusted to 2-10 by using sodium hydroxide or hydrochloric acid.
4. The method for removing diclofenac acid in water by using ferrite magnetic nanoparticles as claimed in claim 1, wherein the concentration of diclofenac acid in the water body to be treated is 1-10 mg/L.
5. The method for removing diclofenac acid from water by using ferrite magnetic nanoparticles as claimed in claim 1 or 4, wherein the dosage of the ferrite magnetic nanoparticles in the step (1) is 0.1-0.5 g/L.
6. The method for removing diclofenac acid from water by using ferrite magnetic nanoparticles as claimed in claim 1, wherein the adsorption reaction in step (2) is carried out at 25-35 ℃, the stirring speed is 30-100rmp, and the reaction time is 1-2 h.
7. The method for removing diclofenac from water by using ferrite magnetic nanoparticles as claimed in claim 1, wherein the water body to be treated comprises sewage, effluent from sewage treatment plants, surface water or drinking water.
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| CN112121798B (en) * | 2020-09-16 | 2023-10-20 | 中国科学院城市环境研究所 | Method for degrading chloramphenicol in water under catalysis of MIL-101 (Fe/Co) derived magnetic cobalt ferrite and application thereof |
| CN115180678B (en) * | 2022-06-24 | 2023-12-12 | 浙江工业大学 | Method for enhancing performance of degrading typical PPCPs by using magnetic zinc ferrite nanorods and using UV-LED/chlorine system |
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| CN103193352A (en) * | 2013-04-24 | 2013-07-10 | 中国科学院生态环境研究中心 | Deep processing method of wastewater during production of diclofenac |
| CN106040194A (en) * | 2016-06-23 | 2016-10-26 | 南京师范大学 | Chitosan magnetic composite spherule adsorbent with core-brush structure as well as preparation method and application thereof |
| CN106365141A (en) * | 2008-09-29 | 2017-02-01 | 索尼公司 | Porous carbon material composites and their production process, adsorbents, cosmetics, purification agents, and composite photocatalyst materials |
| FR3009789B1 (en) * | 2013-08-23 | 2017-07-28 | Saur | METHOD OF MONITORING AND MONITORING THE ABATEMENT OF ORGANIC MICROPOLLUTANTS IN WASTEWATER |
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| CN106365141A (en) * | 2008-09-29 | 2017-02-01 | 索尼公司 | Porous carbon material composites and their production process, adsorbents, cosmetics, purification agents, and composite photocatalyst materials |
| CN103193352A (en) * | 2013-04-24 | 2013-07-10 | 中国科学院生态环境研究中心 | Deep processing method of wastewater during production of diclofenac |
| FR3009789B1 (en) * | 2013-08-23 | 2017-07-28 | Saur | METHOD OF MONITORING AND MONITORING THE ABATEMENT OF ORGANIC MICROPOLLUTANTS IN WASTEWATER |
| CN106040194A (en) * | 2016-06-23 | 2016-10-26 | 南京师范大学 | Chitosan magnetic composite spherule adsorbent with core-brush structure as well as preparation method and application thereof |
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