CN116020413A - Adsorption material for removing perfluorinated compounds in water, and preparation method and application thereof - Google Patents
Adsorption material for removing perfluorinated compounds in water, and preparation method and application thereof Download PDFInfo
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- CN116020413A CN116020413A CN202211675105.8A CN202211675105A CN116020413A CN 116020413 A CN116020413 A CN 116020413A CN 202211675105 A CN202211675105 A CN 202211675105A CN 116020413 A CN116020413 A CN 116020413A
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- 238000001179 sorption measurement Methods 0.000 title claims abstract description 48
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- 238000002360 preparation method Methods 0.000 title abstract description 9
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- 238000000034 method Methods 0.000 claims abstract description 8
- OBOSXEWFRARQPU-UHFFFAOYSA-N 2-n,2-n-dimethylpyridine-2,5-diamine Chemical compound CN(C)C1=CC=C(N)C=N1 OBOSXEWFRARQPU-UHFFFAOYSA-N 0.000 claims abstract description 6
- 239000000203 mixture Substances 0.000 claims description 16
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- BWOAAAYNOWWMHL-UHFFFAOYSA-K trichloroyttrium;hydrate Chemical compound O.[Cl-].[Cl-].[Cl-].[Y+3] BWOAAAYNOWWMHL-UHFFFAOYSA-K 0.000 claims description 7
- 229910021642 ultra pure water Inorganic materials 0.000 claims description 6
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- 125000005010 perfluoroalkyl group Chemical group 0.000 claims description 5
- 239000002351 wastewater Substances 0.000 claims description 3
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- 239000003463 adsorbent Substances 0.000 abstract description 11
- SNGREZUHAYWORS-UHFFFAOYSA-N perfluorooctanoic acid Chemical compound OC(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F SNGREZUHAYWORS-UHFFFAOYSA-N 0.000 abstract description 10
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- 230000000694 effects Effects 0.000 abstract description 4
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- 238000010438 heat treatment Methods 0.000 abstract description 2
- 238000005342 ion exchange Methods 0.000 abstract description 2
- 101001136034 Homo sapiens Phosphoribosylformylglycinamidine synthase Proteins 0.000 description 21
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- 102100036473 Phosphoribosylformylglycinamidine synthase Human genes 0.000 description 21
- QUILVBWWBRWZPL-UHFFFAOYSA-L O[Y]Cl Chemical compound O[Y]Cl QUILVBWWBRWZPL-UHFFFAOYSA-L 0.000 description 11
- 230000007613 environmental effect Effects 0.000 description 5
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 description 3
- YFSUTJLHUFNCNZ-UHFFFAOYSA-N perfluorooctane-1-sulfonic acid Chemical compound OS(=O)(=O)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)C(F)(F)F YFSUTJLHUFNCNZ-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 229910052727 yttrium Inorganic materials 0.000 description 3
- VWQVUPCCIRVNHF-UHFFFAOYSA-N yttrium atom Chemical compound [Y] VWQVUPCCIRVNHF-UHFFFAOYSA-N 0.000 description 3
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Abstract
The invention discloses an adsorption material for removing perfluorinated compounds in water, and a preparation method and application thereof. The method selects the hydrated yttrium chloride as a precursor, takes an activated carbon material as a carrier, and adopts an in-situ vacuum heat treatment method to obtain the adsorption material for removing the perfluoro compound pollutants in water in one step. The basic yttrium chloride/activated carbon adsorbent prepared by the invention has multiple adsorption effects such as ion exchange, electrostatic adsorption, coordination and the like, shows excellent adsorption performance on perfluoro compound pollutants in treated water, has an adsorption capacity of up to 957.1mg/g for typical perfluoro compounds (perfluorooctanoic acid, PFOA), has a fast adsorption rate, and has a wide application prospect in the aspect of deep removal of perfluoro compounds.
Description
Technical Field
The invention relates to the technical field of environmental functional materials, in particular to an adsorption material for removing perfluorinated compounds in water, and a preparation method and application thereof.
Background
Perfluoroalkyl compounds (perfluoroalkyl substances, PFAS) are a class of synthetic compounds that are widely used in industrial and personal consumer products for their excellent hydrophobic oleophobic and chemical stability. Meanwhile, the end group of the PFAS generally contains hydrophilic groups such as carboxylate groups, sulfonate groups or hydroxyl groups, so the PFAS has good water solubility, and high-energy C-F bonds exist in the molecular structure of the PFAS, so the PFAS is shown as environmental persistence in water and is often regarded as a permanent chemical. With the application of PFAS in industrial production and life, PFAS has become a pollutant of widespread concern in global scale, and the presence of PFAS has been detected in various environmental media (surface water, groundwater, soil, sediments, etc.) in various countries and regions worldwide in recent years, which poses a potential threat to ecological environment and human health.
Recent studies have shown that PFAS is bioaccumulative in organisms and that prolonged exposure to PFAS contamination can cause a range of diseases, such as thyroid disease, high cholesterol, liver injury, reduced immune response, ulcerative colitis, and even cancer, even at very low concentrations. In view of the environmental persistence, bioaccumulation and potential biotoxicity of PFAS, many countries have set out relevant regulations restricting the use of PFAS production. In 2016, the U.S. Environmental Protection Agency (EPA) set the standard limit for the sum of perfluorooctanoic acid (PFOA) and perfluorooctyl sulfonic acid (PFOS) in drinking water to 70ng/L. Month 5 of 2022, EPA further enhanced the management of these two classes of compounds, with PFOA and PFOS limits set to 0.004ng/L and 0.02ng/L, respectively.
Therefore, developing a technology for effectively removing PFAS pollutants in water has important research and practical significance.
Disclosure of Invention
Aiming at the technical problems, the invention provides an adsorbing material for removing perfluorinated compounds in water and a preparation method thereof. In-situ structure on active carbon surface by vacuum heat treatment methodBuilding basic yttrium chloride (Y) 2 (OH) 4.86 Cl 1.44 ·1.07H 2 And O) the material is used as an adsorbent to realize the deep purification of the perfluorinated compound polluted water body.
In order to achieve the above purpose, the technical scheme adopted by the invention is as follows:
the first aspect of the present invention provides a method for producing an adsorbent material for removing perfluoro compounds from water, the method comprising: (1) Yttrium chloride hydrate (YCl) 3 ·6H 2 O) dissolving in water to obtain a precursor solution; (2) Dropwise adding the precursor solution onto an activated carbon material to obtain a precursor mixture; (3) Filling the precursor mixture into a single-end packaged quartz tube, placing the quartz tube into a tube furnace for calcination, and continuously pumping air in the tube furnace by using a vacuum pump to keep the system in a vacuum state to obtain a calcined sample; (4) And washing and drying the calcined sample for multiple times to obtain the adsorbing material for removing the perfluorinated compounds in the water.
Further, in the step (1), the concentration of the precursor solution is in the range of 1mol/L to 3mol/L.
Further, in the step (2), the mass ratio of the hydrated yttrium chloride to the activated carbon material in the precursor mixture is 1: (15-30). The activated carbon material is specifically one of granular activated carbon and powdery activated carbon, and is preferably granular activated carbon.
Further, in the step (3), the calcination temperature in the tube furnace is 400-700 ℃. The calcination temperature is preferably 500 ℃.
Further, in the step (3), the calcination time in the tube furnace is 20 min-50 min. The calcination time is preferably 30 minutes.
Further, in the step (4), the washing solvent is selected to be ultrapure water, and the washing times are 3 to 7 times; the drying temperature is 40-80 ℃.
The second aspect of the invention provides the adsorbing material for removing the perfluorinated compounds in water, which is prepared by the preparation method of the adsorbing material for removing the perfluorinated compounds in water.
In a third aspect, the present invention provides the use of an adsorbent for removing perfluoro compounds from water as described above in the field of adsorption treatment of wastewater containing perfluoroalkyl compounds.
The invention has the following beneficial effects:
(1) The preparation process is simple, has low requirements on experimental equipment, can realize large-scale macro preparation, and is easy for industrialized expansion production;
(2) The yttrium chloride hydroxide/activated carbon adsorption material prepared by the invention has large adsorption capacity (up to 957.1 mg/g) for typical perfluorinated compounds (perfluorooctanoic acid, PFOA), has high adsorption rate and good stability, and can be repeatedly used for many times, and the good adsorption performance is still maintained.
(3) The yttrium chloride hydroxide/activated carbon adsorption material prepared by the invention has multiple adsorption effects, can realize the adsorption of various perfluorinated compounds, and has wide application prospects for other anions such as fluoride ions, phosphate and the like.
Drawings
One or more embodiments are illustrated by way of example and not limitation in the figures of the accompanying drawings, which are not to be construed as limiting the embodiments unless specifically indicated otherwise.
FIG. 1 is an adsorption isotherm of typical perfluoro compounds (PFOA) of the yttrium chloride basic adsorbent material obtained in example 1 of the present invention;
FIG. 2 is a schematic diagram of an apparatus for PFAS adsorption in example 1 of the present invention;
FIG. 3 shows the adsorption performance of yttrium chloride hydroxide/activated carbon adsorbent materials for various PFAS in example 1 of the present invention.
Detailed Description
The inventors have found that the techniques currently used to remove perfluorinated compounds from water are adsorption, ion exchange resins, reverse osmosis and the like. Among them, the activated carbon-based adsorption technology is the most commonly used solution, but has problems of slow adsorption, limited adsorption capacity, difficulty in long-period operation, and the like. In addition, since PFAS molecules mostly show electronegativity or neutrality in water, if an adsorbent with positive charge property can be constructed on the surface of activated carbon in situ, adsorption kinetics and adsorption performance of the activated carbon material can be improved.
Layered rare earth hydroxides (LRHs) are an emerging class of two-dimensional layered structure materials with laminates consisting of rare earth oxides or hydroxides, with interlayer SO supplementation 4 2- 、Cl - And NO 3 - Plasma anions, which are positively charged in water, are a very promising class of materials for PFAS adsorption. By modifying a layer of LRHs on the surface of the activated carbon, the adsorption performance of the traditional activated carbon material is expected to be remarkably improved.
The first aspect of the present invention provides a method for producing an adsorbent material for removing perfluoro compounds from water, the method comprising: (1) Yttrium chloride hydrate (YCl) 3 ·6H 2 O) dissolving in water to obtain a precursor solution; (2) Dropwise adding the precursor solution onto an activated carbon material to obtain a precursor mixture; (3) Filling the precursor mixture into a single-end packaged quartz tube, placing the quartz tube into a tube furnace for calcination, and continuously pumping air in the tube furnace by using a vacuum pump to keep the system in a vacuum state to obtain a calcined sample; (4) And washing and drying the calcined sample for multiple times to obtain the adsorbing material for removing the perfluorinated compounds in the water. The adsorption material comprises the following components: an yttrium chloride hydroxide material (hereinafter referred to simply as yttrium chloride hydroxide/activated carbon adsorption material) is constructed in situ on the surface of the activated carbon.
The second aspect of the invention provides the adsorbing material for removing the perfluorinated compounds in water, which is prepared by the preparation method of the adsorbing material for removing the perfluorinated compounds in water.
In a third aspect, the present invention provides the use of an adsorbent for removing perfluoro compounds from water as described above in the field of adsorption treatment of wastewater containing perfluoroalkyl compounds.
In the present invention, all the equipment, raw materials and the like are commercially available or commonly used in the industry unless otherwise specified.
The methods in the following examples are conventional in the art unless otherwise specified.
Example 1:
the first step: 3g of yttrium chloride hydrate is weighed and dissolved in 6mL of water to prepare a precursor solution;
and a second step of: dropwise adding the precursor solution onto 60g of granular activated carbon to obtain a precursor mixture;
and a third step of: filling the precursor mixture into a single-end packaged quartz tube, placing the quartz tube in a tube furnace, calcining for 30min at 500 ℃, and continuously pumping air in the tube furnace by using a vacuum pump to keep the system in a vacuum state;
fourth step: and (3) washing the calcined sample with ultrapure water for multiple times, and drying in a 60 ℃ oven to obtain the yttrium chloride hydroxide/activated carbon adsorption material.
To verify the adsorption performance of yttrium basic chloride on perfluoro compounds, the adsorption performance of typical perfluoro compounds (PFOA) is tested on yttrium basic chloride materials without activated carbon in the invention, and the corresponding adsorption isotherm of the example is shown in FIG. 1. As can be seen from FIG. 1, yttrium basic chloride has an ultra-high adsorption capacity of 957.1mg/g on PFOA.
FIG. 2 is a schematic diagram of the apparatus for PFAS adsorption according to the present embodiment; FIG. 3 shows the adsorption performance of the yttrium chloride hydroxide/activated carbon adsorbent material of this example on various PFAS (initial concentration of each PFAS was set at 500. Mu.g/L). The yttrium chloride hydroxide/activated carbon adsorbent prepared by the invention has multiple adsorption effects such as ion exchange, electrostatic adsorption and coordination, has excellent adsorption performance in treating perfluoro compound pollutants in water, has good adsorption effect on various low-concentration PFAS, has high adsorption rate, and has wide application prospect in the aspect of deep removal of perfluoro compounds.
Example 2:
the first step: 3g of yttrium chloride hydrate is weighed and dissolved in 6mL of water to prepare a precursor solution;
and a second step of: dropwise adding the precursor solution onto 60g of granular activated carbon to obtain a precursor mixture;
and a third step of: filling the precursor mixture into a single-end packaged quartz tube, placing the quartz tube in a tube furnace, calcining for 30min at 400 ℃, and continuously pumping air in the tube furnace by using a vacuum pump to keep the system in a vacuum state;
fourth step: and (3) washing the calcined sample with ultrapure water for multiple times, and drying in a 60 ℃ oven to obtain the yttrium chloride hydroxide/activated carbon adsorption material.
Example 3:
the first step: 3g of yttrium chloride hydrate is weighed and dissolved in 6mL of water to prepare a precursor solution;
and a second step of: dropwise adding the precursor solution onto 60g of granular activated carbon to obtain a precursor mixture;
and a third step of: filling the precursor mixture into a single-end packaged quartz tube, placing the quartz tube in a tube furnace, calcining for 30min at 600 ℃, and continuously pumping air in the tube furnace by using a vacuum pump to keep the system in a vacuum state;
fourth step: and (3) washing the calcined sample with ultrapure water for multiple times, and drying in a 60 ℃ oven to obtain the yttrium chloride hydroxide/activated carbon adsorption material.
Example 4:
the first step: 3g of yttrium chloride hydrate is weighed and dissolved in 6mL of water to prepare a precursor solution;
and a second step of: dropwise adding the precursor solution onto 60g of granular activated carbon to obtain a precursor mixture;
and a third step of: filling the precursor mixture into a single-end packaged quartz tube, placing the quartz tube in a tube furnace, calcining at 700 ℃ for 30min, and continuously pumping air in the tube furnace by using a vacuum pump to keep the system in a vacuum state;
fourth step: and (3) washing the calcined sample with ultrapure water for multiple times, and drying in a 60 ℃ oven to obtain the yttrium chloride hydroxide/activated carbon adsorption material.
The foregoing is only a preferred embodiment of the invention, it being noted that: it will be apparent to those skilled in the art that various modifications and adaptations can be made without departing from the principles of the present invention, and such modifications and adaptations are intended to be comprehended within the scope of the invention.
Claims (8)
1. A method for preparing an adsorbing material for removing perfluoro compounds in water, comprising the steps of:
(1) Dissolving yttrium chloride hydrate in water to obtain a precursor solution;
(2) Dropwise adding the precursor solution onto an activated carbon material to obtain a precursor mixture;
(3) Filling the precursor mixture into a single-end packaged quartz tube, placing the quartz tube into a tube furnace for calcination, and continuously pumping air in the tube furnace by using a vacuum pump to keep the system in a vacuum state to obtain a calcined sample;
(4) And washing and drying the calcined sample for multiple times to obtain the adsorbing material for removing the perfluorinated compounds in the water.
2. The method for producing an adsorbing material for removing perfluoro compounds from water according to claim 1, wherein in said step (1), the concentration of said precursor solution is in the range of 1mol/L to 3mol/L.
3. The method of claim 1, wherein in the step (2), the mass ratio of the hydrated yttrium chloride to the activated carbon material in the precursor mixture is 1: (15-30).
4. The method for producing an adsorbing material for removing perfluoro compounds from water according to claim 1, wherein in said step (3), the calcination temperature in a tube furnace is 400 to 700 ℃.
5. The method for producing an adsorbing material for removing perfluoro compounds from water according to claim 1, wherein in said step (3), said calcining is carried out in a tube furnace for 20 to 50 minutes.
6. The method for producing an adsorbing material for removing a perfluoro compound from water according to claim 1, wherein in said step (4), said washed solvent is selected to be ultrapure water, and the number of washing is 3 to 7; the drying temperature is 40-80 ℃.
7. The adsorbing material for removing perfluoro compounds in water, which is produced by the method for producing adsorbing material for removing perfluoro compounds in water according to any one of claims 1 to 6.
8. The use of the adsorbing material for removing perfluoro compounds from water according to claim 7 in the field of adsorption treatment of wastewater containing perfluoroalkyl compounds.
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| CN101780952A (en) * | 2010-03-26 | 2010-07-21 | 上海交通大学 | Method for preparing loading functional oxide porous carbon |
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