CN113044910A - Method for removing perfluoro or polyfluoro compounds in water body by using attapulgite - Google Patents
Method for removing perfluoro or polyfluoro compounds in water body by using attapulgite Download PDFInfo
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- CN113044910A CN113044910A CN202110265673.XA CN202110265673A CN113044910A CN 113044910 A CN113044910 A CN 113044910A CN 202110265673 A CN202110265673 A CN 202110265673A CN 113044910 A CN113044910 A CN 113044910A
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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
- C02F1/28—Treatment of water, waste water, or sewage by sorption
- C02F1/281—Treatment of water, waste water, or sewage by sorption using inorganic sorbents
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B01—PHYSICAL OR CHEMICAL PROCESSES OR APPARATUS IN GENERAL
- B01J—CHEMICAL OR PHYSICAL PROCESSES, e.g. CATALYSIS OR COLLOID CHEMISTRY; THEIR RELEVANT APPARATUS
- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
- B01J20/02—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material
- B01J20/10—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising silica or silicate
- B01J20/12—Naturally occurring clays or bleaching earth
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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
- C02F2101/10—Inorganic compounds
- C02F2101/12—Halogens or halogen-containing compounds
- C02F2101/14—Fluorine or fluorine-containing compounds
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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
- C02F2103/00—Nature of the water, waste water, sewage or sludge to be treated
- C02F2103/06—Contaminated groundwater or leachate
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Abstract
The invention provides a method for removing perfluorinated or polyfluorinated compounds in a water body by using attapulgite, and relates to the technical field of water body purification. The method provided by the invention comprises the following steps: mixing the polluted water body with attapulgite, and adsorbing to remove perfluoro or polyfluoro compounds in the polluted water body. In the invention, the attapulgite has low cost of raw materials, good adsorption effect on perfluoro or polyfluoro compounds, no secondary pollution, and can be further used for repairing water bodies polluted by perfluoro or polyfluoro compounds, such as underground water of a fluorination plant; moreover, the method provided by the invention is simple and easy to operate, and compared with the conventional method for removing the perfluoro or polyfluoro compound, the method is more economic, effective and environment-friendly, and is suitable for large-scale popularization and application.
Description
Technical Field
The invention relates to the technical field of water body purification, in particular to a method for removing perfluoro or polyfluoro compounds in water body by attapulgite.
Background
PFASs (perfluoro or polyfluoro compounds) refer to artificially synthesized organic fluorine compounds in which H atoms on a C-H bond are partially or completely substituted by F atoms, and have excellent properties of heat resistance, acid resistance, water and oil repellency, surface activity and the like. Since the 50-60 years of the last century, PFASs were produced in large scale and widely processed and manufactured by industrial products and living goods, including foam extinguishing agents, non-stick pans, paints, adhesives, waxes, surfactants and the like. However, PFASs have been detected in various environmental media such as water, soil, gas and the like, organic biological tissues and human blood due to the lack of regulation and supervision in the production and use processes, and particularly, the PFASs have been shown to reach the mg/L level in water body (the sum of PFOA and PFOS in drinking water is not more than 70ng/L by the United states environmental protection agency) and have serious pollution. In addition, PFASs have the characteristics of persistent difficult degradability, long-distance migration, biological accumulation, potential toxicity and the like, and can further harm the health of organic organisms, so that the PFASs are very important to treat.
Currently, methods for removing PFASs include physical adsorption, chemical degradation, and microbial degradation. However, as fluorine elements in PFASs molecules have larger electronegativity and smaller atomic radius, the formed C-F bonds are highly polarized and have extremely large bond energy (484kJ/mol), so that the substances have good thermal stability and chemical stability and are difficult to degrade and mineralize. Physical adsorption has proven to be an effective method for the removal of PFASs contamination. Currently, adsorbents for adsorption removal of PFASs include activated carbon, ion exchange resins, carbon nanotubes, etc., but the cost of the adsorption materials in the preparation process is relatively high. Therefore, it is highly desirable to develop a method that is economical and easy to operate.
Disclosure of Invention
The invention aims to provide a method for removing perfluoro or polyfluoro compounds in water by using attapulgite with low economic cost as a raw material to adsorb the perfluoro or polyfluoro compounds, is simple and convenient to operate, can effectively remove the perfluoro or polyfluoro compounds in the water, and is economic, effective, environment-friendly and suitable for large-scale popularization and application.
In order to achieve the above object, the present invention provides the following technical solutions:
the invention provides a method for removing perfluoro or polyfluoro compounds in a water body by using attapulgite, which comprises the following steps:
mixing the polluted water body with attapulgite, and adsorbing to remove perfluoro or polyfluoro compounds in the polluted water body.
Preferably, the perfluoro or polyfluoro compound is an artificially synthesized organic fluorine compound in which all or part of the H atoms in the C-H bond are replaced by F atoms.
Preferably, the perfluoro or polyfluoro compound includes at least one of perfluorooctanoic acid, perfluorooctane sulfonic acid, perfluorobutyric acid, perfluorobutane sulfonic acid, hexafluoropropylene oxide dimer acid, hexafluoropropylene oxide trimer acid, chloropolyfluoroether sulfonic acid, and 6:2 fluorotelomer sulfonic acid.
Preferably, the attapulgite comprises attapulgite in different producing areas, and the producing areas comprise at least one of the provinces of Gansu, Jiangsu, Anhui, and the United states of China.
Preferably, the contaminated water body includes at least one of groundwater, surface water and industrial wastewater
The invention provides a method for removing perfluoro or polyfluoro compounds in a water body by using attapulgite, which comprises the following steps: mixing the polluted water body with attapulgite, and adsorbing to remove perfluoro or polyfluoro compounds in the polluted water body. In the invention, the attapulgite has low cost of raw materials, good adsorption effect on perfluoro or polyfluoro compounds, no secondary pollution to water, and can be further used for repairing underground water and the like of sites polluted by perfluoro or polyfluoro compounds, such as underground water of a fluorination plant; moreover, the method provided by the invention is simple and easy to operate, and compared with the conventional method for removing the perfluoro or polyfluoro compound, the method is more economic, effective and environment-friendly, and is suitable for large-scale popularization and application.
Drawings
FIG. 1 is a graph showing the effect of examples 1 to 4 and comparative example 1 on PFOA and PFOS removal;
fig. 2 is a graph showing the effect of removing PFOA and PFOS in examples 7 to 10 and comparative example 2.
Detailed Description
The invention provides a method for removing perfluoro or polyfluoro compounds in a water body by using attapulgite, which comprises the following steps:
mixing the polluted water body with attapulgite, and adsorbing to remove perfluoro or polyfluoro compounds in the polluted water body.
In the present invention, the perfluoro or polyfluoro compound is preferably an artificially synthesized organofluorine compound in which all or part of the H atoms in the C-H bond are substituted with F atoms. In the present invention, the perfluoro or polyfluoro compound preferably includes at least one of perfluorooctanoic acid, perfluorooctane sulfonic acid, perfluorobutyric acid, perfluorobutane sulfonic acid, hexafluoropropylene oxide dimer acid, hexafluoropropylene oxide trimer acid, chloropolyfluoroether sulfonic acid and 6:2 fluorotelomeric sulfonic acid.
In the invention, the concentration of the perfluoro or polyfluoro compound in the polluted water body is preferably 0.07 to 810mg/L, preferably 0.052 to 81mg/L, and most preferably 0.1 to 0.4 mg/L.
In the present invention, the attapulgite preferably comprises attapulgite of different origins, and the origin preferably comprises at least one of the provinces of Gansu, Jiangsu, Anhui, and the United states of China.
In the invention, the particle size of the attapulgite is preferably 20-100 meshes, and more preferably 50-60 meshes.
In the invention, the concentration of the perfluoro or polyfluoro compound in the polluted water body is preferably 0.07 to 810mg/L, preferably 0.052 to 81mg/L, and most preferably 0.1 to 0.4 mg/L.
In the invention, the dosage ratio of the attapulgite to the polluted water body is preferably 0.05-0.25 g: 10mL, more preferably 0.25 g: 10 mL.
In the invention, the adsorption is preferably carried out under the oscillation condition, and the oscillation rate is preferably 100-250 r/min, more preferably 130-200 r/min, and most preferably 150 r/min; the adsorption time is preferably 8-48 h, more preferably 18-48 h, and more preferably 24-30 h. In the present invention, the adsorption is preferably performed at room temperature, and particularly preferably at 25 ℃. In the present invention, the adsorption is preferably carried out in a constant temperature shaker.
The technical solution of the present invention will be clearly and completely described below with reference to the embodiments of the present invention. It is to be understood that the described embodiments are merely exemplary of the invention, and not restrictive of the full scope of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Putting 0.050g of attapulgite in Jiangsu province into transparent headspace bottles, and respectively adding 10mL of mixed solution of perfluorooctanoic acid (PFOA) and perfluorooctane sulfonic acid (PFOS) into each headspace bottle, wherein the initial concentration of the PFOA in the mixed solution is 200 mu g/L, and the initial concentration of the PFOS is 125 mu g/L; and (3) placing the headspace bottle in a constant-temperature oscillator, and oscillating and adsorbing at the rotating speed of 160r/min and the temperature of 25 ℃ for 24 hours.
And after adsorption, centrifuging at 3000r/min by using a centrifuge, filtering by using a 0.22 mu m filter membrane, detecting the concentrations of the residual PFOA and PFOS in the filtrate by using an LC-MS/MS (liquid chromatography-mass spectrometry) with the model number of 3200, calculating the removal rates of the corresponding PFOA and PFOS, and taking the average value of three detections.
As shown in FIG. 1, when the amount of attapulgite added in Jiangsu province was 0.050g, the PFOS removal rate was 22.56%, and the PFOA adsorption rate was close to 0.
Example 2
The method is basically the same as that of the method in the example 1, except that the adding amount of the attapulgite in Jiangsu province is adjusted from 0.050g to 0.075 g.
As shown in FIG. 1, when the amount of attapulgite added in Jiangsu province was 0.075g, the removal rate of PFOS was 68.21%, and the removal rate of PFOA was 50.59%.
Example 3
The method is basically the same as that of the method in the example 1, except that the adding amount of the attapulgite in Jiangsu province is adjusted from 0.050g to 0.100 g.
As shown in FIG. 1, when the amount of attapulgite added in Jiangsu province was 0.100g, the removal rate of PFOS was 96.24%, and the removal rate of PFOA was 39.23%.
Example 4
The method is basically the same as that of the method in the example 1, except that the adding amount of the attapulgite in Jiangsu province is adjusted from 0.050g to 0.250 g.
As shown in FIG. 1, when the amount of attapulgite added in Jiangsu province was 0.250g, the removal rate of PFOS was 89.17%, and the removal rate of PFOA was 72.66%.
Example 5
The same procedure as in example 1, except that the amount of attapulgite added in Jiangsu province was adjusted from "0.050 g" to "0.250 g", the initial concentration of PFOA in the mixed solution was adjusted to "200. mu.g/L" to "60. mu.g/L", and the initial concentration of PFOS was adjusted to "125. mu.g/L" to "53. mu.g/L".
As a result of the examination, when the amount of attapulgite added in Jiangsu province was 0.250g, the initial concentration of PFOA in the mixed solution was 60. mu.g/L, and the initial concentration of PFOS was 53. mu.g/L, the removal rate of PFOS was 98.78%, and the removal rate of PFOA was 79.45%.
Example 6
The same procedure as in example 1, except that the amount of attapulgite added in Jiangsu province was adjusted from "0.050 g" to "0.250 g", the initial concentration of PFOA in the mixed solution was adjusted to "200. mu.g/L" to "3.8 mg/L", and the initial concentration of PFOS was adjusted to "125. mu.g/L" to "3.2 mg/L".
As a result of the examination, when the amount of attapulgite added in Jiangsu province was 0.250g, the initial concentration of PFOA in the mixed solution was 60. mu.g/L, and the initial concentration of PFOS was 53. mu.g/L, the removal rate of PFOS was 94.77%, and the removal rate of PFOA was 32.01%.
Comparative example 1
The method was substantially the same as that of example 1, except that attapulgite was not added.
As shown in fig. 1, the removal rates of PFOS and PFOA were 0.
Example 7
Placing 0.050g of attapulgite in Gansu province into transparent headspace bottles, and respectively adding 10mL of mixed solution of perfluorooctanoic acid (PFOA) and perfluorooctane sulfonic acid (PFOS) into each headspace bottle, wherein the initial concentration of the PFOA in the mixed solution is 200 mu g/L, and the initial concentration of the PFOS is 125 mu g/L; and (3) placing the headspace bottle in a constant-temperature oscillator, and carrying out oscillation adsorption for 24 hours at the rotation speed of 150r/min and the temperature of 25 ℃.
And after adsorption, centrifuging at 3000r/min by using a centrifuge, filtering by using a 0.22 mu m nylon filter membrane, detecting the concentrations of the residual PFOA and PFOS in the filtrate by using an LC-MS/MS (liquid chromatography-mass spectrometry) with the model number of 3200, calculating the removal rates of the corresponding PFOA and PFOS, and taking the average value of three detections.
As shown in FIG. 2, when the amount of attapulgite added in Gansu province was 0.050g, the adsorption rate of PFOS was close to 0 and the removal rate of PFOA was 10.27%.
Example 8
The method is basically the same as that of example 7, except that the adding amount of attapulgite in Gansu province is adjusted from 0.050g to 0.075 g.
As a result of the examination, as shown in FIG. 2, when the amount of attapulgite added in Gansu province was 0.075g, the removal rate of PFOS was 42.47%, and the removal rate of PFOA was 13.97%.
Example 9
The method is basically the same as that of example 7, except that the adding amount of the attapulgite in Gansu province is adjusted from 0.050g to 0.100 g.
As a result of the examination, as shown in FIG. 2, when the amount of attapulgite added in Gansu province was 0.100g, the removal rate of PFOS was 54.79%, and the removal rate of PFOA was 6.57%.
Example 10
The method is basically the same as that of example 7, except that the adding amount of the attapulgite in Gansu province is adjusted from 0.050g to 0.250 g.
As a result of the examination, as shown in FIG. 2, when the amount of attapulgite added in Gansu province was 0.250g, the removal rate of PFOS was 63.23%, and the removal rate of PFOA was 22.22%.
Comparative example 2
The method was substantially the same as that of example 7, except that attapulgite, Gansu province, was not added.
As a result of the measurement, as shown in fig. 2, the removal rates of PFOS and PFOA were 0.
Example 11
The same procedure as in example 7 was repeated, except that the amount of attapulgite added in Gansu province was adjusted from "0.050 g" to "0.250 g", the initial concentration of PFOA in the mixed solution was adjusted to "200. mu.g/L" to "60. mu.g/L", and the initial concentration of PFOS was adjusted to "125. mu.g/L" to "53. mu.g/L".
As a result of the examination, when the amount of attapulgite added in Gansu province was 0.250g, the initial concentration of PFOA in the mixed solution was 60. mu.g/L, and the initial concentration of PFOS was 53. mu.g/L, the removal rate of PFOS was 95.59%, and the removal rate of PFOA was 50.02%.
Example 12
The same procedure as in example 7 was repeated, except that the amount of attapulgite added in Gansu province was adjusted from "0.050 g" to "0.250 g", the initial concentration of PFOA in the mixed solution was adjusted to "200. mu.g/L" to "3.8 mg/L", and the initial concentration of PFOS was adjusted to "125. mu.g/L" to "3.2 mg/L".
As a result of the examination, when the amount of attapulgite added in Gansu province was 0.250g, the initial concentration of PFOA in the mixed solution was 3.8mg/L, and the initial concentration of PFOS was 3.2mg/L, the removal rate of PFOS was 67.64%, and the removal rate of PFOA was 20.24%.
From the above examples, it can be seen that attapulgite in Gansu province has slightly poorer removal effect on perfluoro or polyfluoro compounds than attapulgite in Jiangsu province, but still has a certain adsorption effect, which indicates that the attapulgite can be used for adsorbing and removing perfluoro or polyfluoro compounds.
The foregoing is only a preferred embodiment of the present invention, and it should be noted that, for those skilled in the art, various modifications and decorations can be made without departing from the principle of the present invention, and these modifications and decorations should also be regarded as the protection scope of the present invention.
Claims (5)
1. A method for removing perfluoro or polyfluoro compounds in a water body by attapulgite is characterized by comprising the following steps:
mixing the polluted water body with attapulgite, and adsorbing to remove perfluoro or polyfluoro compounds in the polluted water body.
2. The method according to claim 1, wherein the perfluoro or polyfluoro compound is an artificially synthesized organofluorine compound in which H atoms in a C-H bond are substituted in whole or in part with F atoms.
3. The method of claim 1 or 2, wherein the perfluoro or polyfluoro compound comprises at least one of perfluorooctanoic acid, perfluorooctanesulfonic acid, perfluorobutyric acid, perfluorobutanesulfonic acid, hexafluoropropylene oxide dimer acid, hexafluoropropylene oxide trimer acid, chloropolyfluoroether-based sulfonic acid, and 6:2 fluorotelomeric sulfonic acid.
4. The method of claim 1, wherein the attapulgite comprises attapulgite from different production places, the production places comprising at least one of Gansu province of China, Jiangsu province of China, Anhui province of China, and the United states of America.
5. The method of claim 1 or 2, wherein the contaminated water body comprises at least one of groundwater, surface water, and industrial wastewater.
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Cited By (1)
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| CN115947339A (en) * | 2022-12-21 | 2023-04-11 | 中国科学院南京土壤研究所 | Layered double hydroxide modified multi-walled carbon nanotube, preparation method and application thereof, and PFASs polluted water body treatment method |
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| CN115947339A (en) * | 2022-12-21 | 2023-04-11 | 中国科学院南京土壤研究所 | Layered double hydroxide modified multi-walled carbon nanotube, preparation method and application thereof, and PFASs polluted water body treatment method |
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