CN113244886A - Biochar composite loaded with nano magnesium oxide and preparation method and application thereof - Google Patents
Biochar composite loaded with nano magnesium oxide and preparation method and application thereof Download PDFInfo
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Abstract
The invention belongs to the technical field of adsorption materials, and discloses a nano-magnesia-loaded biochar composite material, and a preparation method and application thereof. The nano magnesium oxide particles of the biochar composite material loaded with nano magnesium oxide prepared by the invention are uniformly distributed, have good adsorption effect on heavy metals such as Pb (II), Cd (II), Cr (VI), Sb (III) and the like, have good potential for repairing heavy metal pollution of water, have simple and feasible preparation process and low preparation cost, fully utilize waste agriculture and forestry biomass, and ammonia water and magnesium chloride in the modification process can not generate secondary pollution to the environment, thereby being beneficial to reducing the environmental pollution and carbon emission of the waste biomass. Can be applied to heavy metal pollution remediation to efficiently remove lead, cadmium, antimony, chromium and the like in the aqueous solution.
Description
Technical Field
The invention belongs to the technical field of adsorption materials, and particularly relates to a biochar composite loaded with nano magnesium oxide, and a preparation method and application thereof.
Background
The biochar is a carbon-rich solid product formed by pyrolyzing waste biomass materials under an anoxic condition, and can adsorb and remove heavy metals in a water body or fix and passivate heavy metals in soil so as to reduce the toxicity of the biochar. The biological carbon has strong anti-decomposition capability in natural environment, and the biological carbon-based material is used for removing heavy metal in polluted water or passivating heavy metal in soil, so that the harm of heavy metal pollution to the environment is effectively reduced, and simultaneously, the biological carbon is beneficial to fixing a large amount of carbon in waste biomass. Therefore, the development of novel efficient and environment-friendly modified biochar has important significance for reducing the harm caused by heavy metal pollution of water and soil.
The biochar composite material loaded with the nano magnesium oxide can improve the specific surface area, adsorption sites and reaction activity of the biochar, and is beneficial to enhancing the adsorption capacity of the biochar on heavy metals. The ultrasonic impregnation method and the nano magnesium hydroxide decomposition method adopted in the prior art are relatively common nano magnesium oxide loading methods, but when the ultrasonic impregnation method is adopted, excessive magnesium chloride crystal particles can generate larger aggregates in the heating reaction process, so that the nano magnesium oxide on the biochar is unevenly distributed, and even the biochar pores are blocked; when the nano magnesium hydroxide decomposition method is adopted, excessive nano magnesium hydroxide is easy to gather and is loaded on the biochar and is subjected to high-temperature treatment, the nano magnesium hydroxide is difficult to be fully decomposed to form nano magnesium oxide, and at the moment, the preparation efficiency and the controllability of the biochar composite material loaded with the nano magnesium oxide are low. The biological carbon composite material loaded with nano magnesium oxide prepared by the methods has low adsorption efficiency on heavy metals, and the improvement on the removal efficiency of the heavy metals is very limited, so that the existing requirements cannot be met.
Disclosure of Invention
The invention provides a biochar composite loaded with nano magnesium oxide, and a preparation method and application thereof, which are used for solving one or more technical problems in the prior art and at least providing a beneficial choice or creation condition.
In order to overcome the technical problems, the technical scheme adopted by the invention is as follows:
a preparation method of a biochar composite loaded with nano magnesium oxide comprises the following steps:
s1, taking the biomass material, and pyrolyzing the biomass material in an inert gas atmosphere to obtain a biochar material;
s2, crushing and sieving the biochar material, adding the biochar material into a steeping liquor containing nano magnesium hydroxide, stirring, filtering, and drying the obtained filter residue;
s3, putting the filter residue obtained in the step S2 into a tubular furnace, and pyrolyzing the filter residue in an inert gas atmosphere to obtain a biochar composite material loaded with nano magnesium oxide;
wherein, the impregnation liquid containing the nano magnesium hydroxide is prepared by adding ammonia water into a magnesium chloride solution and stirring.
As a further improvement of the scheme, the biomass material is selected from one of coconut shells, peanut shells, rice straws, rice hulls, wood chips or barks.
As a further improvement of the above scheme, in step S1, the pyrolysis is: heating to 450-550 ℃ at the heating rate of 20 ℃/min, and preserving the heat for 3.5-4.5 h.
As a further improvement of the above scheme, in step S3, the pyrolysis is: heating to 400-500 ℃ at the heating rate of 15 ℃/min, and keeping the temperature for 2.5-3.5 h.
As a further improvement of the scheme, in the step S2, the particle size of the biochar material during sieving is 0.15-1 mm.
As a further improvement of the above scheme, in step S1 or step S3, the aeration rate of the inert gas is 150 sccm and 250sccm, preferably 200 sccm.
As a further improvement of the above scheme, the mass ratio of the biochar material to Mg in the magnesium chloride solution is about 1: (1-10) to avoid insufficient or excessive magnesium source when preparing the biochar composite material loaded with nano magnesium oxide; preferably 1: 2.43.
as a further improvement of the scheme, the concentration of the magnesium chloride solution is 0.2-2mol/L, preferably 0.5-1.5 mol/L; the concentration of the aqueous ammonia was about 28 wt%.
Further, the volume ratio of the magnesium chloride solution to the ammonia water is 100: (0.42-15), preferably 100: (0.83-3.34), more preferably 100: 1.67, so as to ensure that the nano magnesium hydroxide can be fully decomposed into the nano magnesium oxide when the biochar material loaded with the nano magnesium oxide is prepared, and the nano magnesium oxide particles are uniformly distributed.
The biochar composite material loaded with nano magnesium oxide is prepared by adopting the preparation method of any item of the invention. The nano magnesium oxide particles on the biochar composite material are uniformly distributed, and the adsorption capacity of the biochar composite material on heavy metal ions such as Pb (II), Cd (II), Cr (VI), Sb (III) and the like is improved by more than 10 times compared with that of the control biochar.
The biochar composite material loaded with the nano magnesium oxide is applied to heavy metal pollution remediation.
Preferably, the heavy metals include lead, cadmium, antimony and chromium.
The invention has the beneficial effects that:
the invention provides a biochar composite loaded with nano magnesium oxide and a preparation method and application thereof. The modified biochar material has a large specific surface area, and simultaneously retains the high reactivity of the nano-magnesia, so that the modified biochar material has strong adsorption performance, and has the characteristics of high adsorption rate, large adsorption capacity and the like for heavy metal ions. Therefore, the nano magnesium oxide particles of the biochar composite material loaded with nano magnesium oxide prepared by the invention are uniformly distributed, have good adsorption effect on heavy metals such as Pb (II), Cd (II), Cr (VI), Sb (III) and the like, have good potential for repairing heavy metal pollution of water, have simple and feasible preparation process and low preparation cost, fully utilize waste agriculture and forestry biomass, and ammonia water and magnesium chloride in the modification process can not generate secondary pollution to the environment, thereby being beneficial to reducing the environmental pollution and carbon emission of the waste biomass. The method can be applied to heavy metal pollution remediation, can efficiently remove lead, cadmium, antimony, chromium and the like in the aqueous solution, and has wide application prospect.
Drawings
FIG. 1 is a schematic flow chart of the present invention for preparing a biochar composite loaded with nano-magnesia;
FIG. 2 is TEM and SEM images of the nanocarbon composites with nano-magnesia of examples 1 to 3 and the control biochar of comparative example 1 in the present invention;
FIG. 3 is XPS survey spectra of a nanocarbon composite loaded with nano-magnesia according to example 3 of the present invention and a control biochar of comparative example 1;
fig. 4 is XRD patterns of the nano-magnesia-loaded biochar composites of examples 1-3 of the present invention and the control biochar of comparative example 1;
FIG. 5 is a graph showing the effect of the removal rate of Pb (II), Cd (II), Cr (VI) and Sb (III) of the biochar composite loaded with nano-magnesia according to examples 1-3 and the control biochar of comparative example 1.
Detailed Description
The present invention is specifically described below with reference to examples in order to facilitate understanding of the present invention by those skilled in the art. It should be particularly noted that the examples are given solely for the purpose of illustration and are not to be construed as limitations on the scope of the invention, as non-essential improvements and modifications to the invention may occur to those skilled in the art, which fall within the scope of the invention as defined by the appended claims. Meanwhile, the raw materials mentioned below are not specified in detail and are all commercially available products; the process steps or extraction methods not mentioned in detail are all process steps or extraction methods known to the person skilled in the art.
Example 1
A biochar composite loaded with nano magnesium oxide is prepared by the following steps: crushing and drying the coconut shell of the agricultural and forestry waste biomass to constant weight, placing the coconut shell into a quartz boat, placing the quartz boat into a tube furnace, and heating at 500 ℃ under the environment of 200sccm of argon gas (the temperature rise rate is 15 ℃/min) for heat preservation treatment for 4h to obtain a coconut shell biochar material; uniformly mixing 1.0g of dried coconut shell biochar material with 100mL of mixed solution (nano magnesium hydroxide impregnation solution) of 1mol/L magnesium chloride solution and 0.83mL of ammonia water (28 wt%), fully stirring for 2h, and filtering; and (2) drying the biochar material in an oven at 65 ℃ to constant weight, placing the dried biochar material in a quartz boat, placing the quartz boat in a tube furnace, heating the biochar material at 450 ℃ under an oxygen-deficient environment with the ventilation volume of argon of 200sccm (the heating rate is 15 ℃/min) for 3 hours to ensure that the nano magnesium hydroxide loaded on the coconut shell biochar material is heated and fully decomposed, and cooling the biochar material to room temperature to obtain the biochar composite material loaded with the nano magnesium oxide, which is marked as BC-Mg-0.83.
FIG. 1 is a schematic flow chart of the present invention for preparing a biochar composite loaded with nano-magnesia.
Example 2
A biochar composite loaded with nano magnesium oxide is prepared by the following steps: crushing and drying the coconut shell of the agricultural and forestry waste biomass to constant weight, placing the coconut shell into a quartz boat, placing the quartz boat into a tube furnace, and heating at 500 ℃ under the environment of 200sccm of argon gas (the temperature rise rate is 15 ℃/min) for heat preservation treatment for 4h to obtain a coconut shell biochar material; uniformly mixing 1.0g of dried coconut shell biochar material with 100mL of mixed solution (nano magnesium hydroxide impregnation solution) of 1mol/L magnesium chloride solution and 3.34mL of ammonia water (28 wt%), fully stirring for 2h, and filtering; and (2) drying the biochar material in an oven at 65 ℃ to constant weight, placing the dried biochar material in a quartz boat, placing the quartz boat in a tube furnace, heating the biochar material at 450 ℃ under an oxygen-deficient environment with the ventilation volume of argon of 200sccm (the heating rate is 15 ℃/min) for 3 hours to ensure that the nano magnesium hydroxide loaded on the coconut shell biochar material is heated and fully decomposed, and cooling the biochar material to room temperature to obtain the biochar composite material loaded with the nano magnesium oxide, which is marked as BC-Mg-3.34.
Example 3
A biochar composite loaded with nano magnesium oxide is prepared by the following steps: crushing and drying the coconut shell of the agricultural and forestry waste biomass to constant weight, placing the coconut shell into a quartz boat, placing the quartz boat into a tube furnace, and heating at 500 ℃ under the environment of 200sccm of argon gas (the temperature rise rate is 15 ℃/min) for heat preservation treatment for 4h to obtain a coconut shell biochar material; uniformly mixing 1.0g of dried coconut shell biochar material with 100mL of mixed solution (nano magnesium hydroxide impregnation solution) of 1mol/L magnesium chloride solution and 1.67mL of ammonia water (28 wt%), fully stirring for 2h, and filtering; and (2) drying the biochar material in an oven at 65 ℃ to constant weight, placing the dried biochar material in a quartz boat, placing the quartz boat in a tube furnace, heating the biochar material at 450 ℃ under an oxygen-deficient environment with the ventilation volume of argon of 200sccm (the heating rate is 15 ℃/min) for 3 hours to ensure that the nano magnesium hydroxide loaded on the coconut shell biochar material is heated and fully decomposed, and cooling the biochar material to room temperature to obtain the biochar composite material loaded with the nano magnesium oxide, which is marked as BC-Mg-1.67.
Comparative example 1
Crushing the agricultural and forestry waste biomass coconut shells into blocks (the length and the width are about 2-3cm), and drying in an oven at 65 ℃ to constant weight. Filling a quartz boat with a proper amount of dried coconut shells, putting the quartz boat into a tube furnace, carrying out pyrolysis (with the heating rate of 20 ℃/min) at 500 ℃ in an oxygen-deficient environment with the ventilation volume of 200sccm of nitrogen for 4 hours, and cooling to room temperature (about 25 ℃) to obtain the coconut shell biochar material. Crushing and sieving the coconut shell biochar material, taking the biochar material with the particle size of 0.15mm to 1mm, drying, and storing in a sealed manner for later use, namely, the reference biochar is marked as BC.
Product performance detection 1: physicochemical Properties and characterization of the adsorbent Material
The results of high-power Transmission Electron Microscopy (TEM) and Scanning Electron Microscopy (SEM) on the nanocarbon composite materials loaded with nano-magnesia obtained in examples 1-3 and the control biochar obtained in comparative example 1 are shown in fig. 2, in which a is a TEM image of the control biochar prepared in comparative example 1, b is a TEM image of the nanocarbon composite material loaded with nano-magnesia prepared in example 1, c is a TEM image of the nanocarbon composite material loaded with nano-magnesia prepared in example 2, and d is a TEM image of the nanocarbon composite material loaded with nano-magnesia prepared in example 3; e is an SEM picture of a control biochar prepared in comparative example 1, f is an SEM picture of the nano-magnesia supported biochar composite prepared in example 1, g is an SEM picture of the nano-magnesia supported biochar composite prepared in example 2, and h is an SEM picture of the nano-magnesia supported biochar composite prepared in example 3.
It can be clearly observed from a and e in fig. 2 that the contrast biochar has a flat surface, a relatively balanced material structure and no obvious nanoparticle load; as can be seen from b-d and f-h in FIG. 2, the surface of the biochar composite material loaded with nano magnesium oxide has obvious nano particle loading, and the loaded nano particles are mainly spherical (or square) grains. The size of the nano-particles is increased along with the increase of the using amount of the ammonia water during the preparation, the nano-particles are in uniform scattered-point spherical particles when the using amount of the ammonia water is 0.83mL, the nano-particles are in compact square crystals when the using amount of the ammonia water is 3.34mL, and the nano-particles are in ideal and uniform spherical particles or square crystals when the using amount of the ammonia water is 1.67 mL.
The nanocarbon composite material (BC-Mg-1.67) loaded with nano-magnesia of example 3 and the control Biochar (BC) of comparative example 1 were subjected to X-ray photoelectron spectroscopy (XPS) test, respectively, and the results are shown in fig. 3 and table 1.
Table 1 XPS full spectrum element content analysis of the nanocarbon composite material loaded with nano-magnesia of example 3 and the control biochar of comparative example 1
As can be seen from Table 1, the control biochar contains mainly C, O, N, Si, among other elements, where C is the most and the atomic percentage is 83.77%. A distinct Mg peak was detected in the XPS survey spectrum of the nano magnesia-loaded biochar composite of example 3 compared to the control biochar of comparative example 1, with an atomic percentage of Mg of 7.72% and an atomic percentage of O increased to 28.87% compared to 10.95% for the control biochar. Namely, the biochar composite material loaded with the nano magnesium oxide of example 3 successfully loads a magnesium-containing compound.
Table 2 compares the BET specific surface area, total pore volume and average pore diameter of the nanocarbon composite (BC-Mg-1.67) loaded with nano-magnesia and the control Biochar (BC) of comparative example 1.
Table 2 BET specific surface area, total pore volume, and average pore diameter of the nano-magnesia-loaded biochar composite of example 3 and the control biochar of comparative example 1
As can be seen from table 2, the BET specific surface area, the total pore volume and the average pore diameter of the biochar composite loaded with nano-magnesia in example 3 are significantly improved compared to the control biochar in proportion 1.
Fig. 4 is XRD patterns of the nano-magnesia-loaded biochar composites of examples 1-3 of the present invention and the control biochar of comparative example 1. As can be seen from fig. 4, there is no distinct crystal structure peak in the XRD pattern for the control biochar; the biochar composite materials loaded with the nano magnesium oxide which are successfully prepared all have obvious crystal structure peaks, the strength of the main crystal structure peak is enhanced along with the increase of the using amount of the ammonia water, and the crystal structure of the nano particles is determined to be magnesium oxide through the search and comparison of a Jade 6 software crystal structure peak database, namely the magnesium-containing compound successfully loaded on the composite materials prepared in examples 1-3 is magnesium oxide.
Therefore, the preparation method can controllably prepare the biochar composite loaded with the nano-magnesia, and the nano-particles can be uniformly loaded on the surface of the modified biochar, so that the reaction active surface of the modified biochar material is obviously and effectively increased, but the nano-magnesia particles on the composite prepared in the embodiment 3 with the ammonia water usage amount of 1.67 have better size and uniform distribution.
And (3) product performance detection 2: testing of adsorption capacity of adsorption material on Pb, Cd, Cr and Sb in aqueous solution
0.05g of the adsorbing materials (the nano-magnesia-loaded biocarbon composite of examples 1 to 3 and the control biochar of comparative example 1) were weighed into a polytetrafluoroethylene tube, and 25mL of Pb (NO) was added thereto, respectively3)2、Cd(NO3)2、K2CrO4And K2Sb2(C4H2O6)2Pb (II), Cd (II), Cr (VI) and Sb (III) in a concentration of 500mg/L, 250mg/L, 300mg/L and 500mg/L (containing 0.01M NaNO)3Electrolyte) solution. Adjusting the pH value to 5.0, adjusting the temperature to 25 ℃, oscillating for 24h at a rotating speed of 220rpm in a constant-temperature oscillation box, taking the supernatant of the solution, filtering the supernatant through a 0.45-micron microporous filter membrane, and measuring the concentrations of Pb, Cd, Cr and Sb in the balanced solution by using an atomic absorption spectrometer, wherein the results are shown in Table 3.
The removal rate of the adsorbing material on Pb (II), Cd (II), Cr (VI) and Sb (III) is calculated by the following formula:
removal rate (%). 100 ═ C (C-C)e)/C
Wherein C is the initial concentration of the adsorption solution, CeThe concentration is in mg/L as the equilibrium concentration of the adsorption solution.
TABLE 3 adsorption Effect of the nanocarbon composite materials loaded with nano-magnesia of examples 1-3 and the control biochar of comparative example 1 on Pb (II), Cd (II), Cr (VI) and Sb (III) in aqueous solution
As can be seen from Table 3: when the concentration of Pb (II) is 500mg/L, the removal rate of the control biochar on Pb is only 4.44%, and the removal rates of the biochar composite material loaded with nano magnesium oxide prepared in examples 1-3 on Pb are 88.02%, 94.30% and 92.51% respectively; when the concentration of Cd (II) is 250mg/L, the removal rate of the control biochar to Cd is 7.24%, and the removal rates of the biochar composite material loaded with nano-magnesium oxide prepared in examples 1-3 to Cd reach 96.68%, 99.98% and 99.97% respectively; at an Sb (III) concentration of 500mg/L, the removal rate of Sb by the control biochar was 3.52%, and the removal rates of Sb by the biochar composite material loaded with nano-magnesia prepared in examples 1-3 were 79.20%, 89.16% and 87.97%, respectively; at a concentration of 300mg/L of Cr (VI), the removal rate of Cr from the control biochar was 4.39%, and the removal rates of Cr from the biochar composite loaded with nano-magnesia prepared in examples 1-3 were 72.66%, 84.50% and 83.38%, respectively.
FIG. 5 is a graph showing the effect of the removal rate of Pb (II), Cd (II), Cr (VI) and Sb (III) of the biochar composites loaded with nano-magnesia according to examples 1 to 3 and the control biochar of comparative example 1, and it can be seen from FIG. 5 that the removal rate of Pb (II), Cd (II), Cr (VI) and Sb (III) of the biochar composites loaded with nano-magnesia (BC-Mg-3.34 and BC-Mg-1.67) of examples 2 to 3 is significantly higher than that of the Biochar (BC) of comparative example 1 and the biochar composite loaded with nano-magnesia (BC-Mg-0.83) of example 1; compared with the contrast biochar, the biochar composite loaded with the nano magnesium oxide respectively improves the adsorption efficiency of Pb (II), Cd (II), Cr (VI) and Sb (III) by 19.82-21.24 times, 13.35-13.81 times, 22.50-25.33 times and 16.55-19.25 times. However, the difference between the adsorption efficiencies of the embodiment 2 and the embodiment 3 is not significant, except that the difference between the adsorption efficiencies of the Pb (II) and the Cd (II), the Cr (VI) and the Sb (III) is significant. The biochar composite loaded with nano-magnesia prepared in example 3 can be preferably selected by comprehensively considering the difference between the usage amount of ammonia water and the adsorption efficiency of heavy metals during modification preparation.
Therefore, the nano magnesium oxide particles of the biochar composite material loaded with nano magnesium oxide prepared by the invention are uniformly distributed, have a good adsorption effect on heavy metals such as Pb (II), Cd (II), Cr (VI), Sb (III) and the like, have a good potential for repairing heavy metal pollution of water, have simple and easy preparation process and low preparation cost, fully utilize waste agriculture and forestry biomass, and ammonia water and magnesium chloride in the modification process can not generate secondary pollution to the environment, thereby being beneficial to reducing the environmental pollution and carbon emission of the waste biomass. Can be applied to heavy metal pollution remediation to efficiently remove lead, cadmium, antimony, chromium and the like in the aqueous solution.
It will be obvious to those skilled in the art that many simple derivations or substitutions can be made without inventive effort without departing from the inventive concept. Therefore, simple modifications to the present invention by those skilled in the art according to the present disclosure should be within the scope of the present invention. The above embodiments are preferred embodiments of the present invention, and all similar processes and equivalent variations to those of the present invention should fall within the scope of the present invention.
Claims (10)
1. The preparation method of the biochar composite material is characterized by comprising the following steps of:
s1, taking the biomass material, and pyrolyzing the biomass material in an inert gas atmosphere to obtain a biochar material;
s2, crushing and sieving the biochar material, adding the biochar material into a steeping liquor containing nano magnesium hydroxide, stirring, filtering, and drying the obtained filter residue;
s3, carrying out pyrolysis on the filter residue obtained in the step S2 in an inert gas atmosphere to obtain a biochar composite material loaded with nano magnesium oxide;
wherein, the impregnation liquid containing the nano magnesium hydroxide is prepared by adding ammonia water into a magnesium chloride solution and stirring.
2. The method of claim 1, wherein the biomass material is selected from one of coconut shell, peanut shell, rice straw, rice hull, wood chip, or bark.
3. The method according to claim 1, wherein in step S1, the pyrolysis is: heating to 450-550 ℃ at the heating rate of 20 ℃/min, and preserving the heat for 3.5-4.5 h.
4. The method according to claim 1, wherein in step S3, the pyrolysis is: heating to 400-500 ℃ at the heating rate of 15 ℃/min, and keeping the temperature for 2.5-3.5 h.
5. The method according to claim 1, wherein the biochar material has a particle size of 0.15 to 1mm when sieved in step S2.
6. The method as claimed in claim 1, wherein the inert gas is introduced at a flow rate of 150 sccm, preferably 200sccm in step S1 or step S3.
7. The method of claim 1, wherein the mass ratio of the biochar material to Mg in the magnesium chloride solution is about 1: (1-10), preferably 1: 2.43.
8. the method according to claim 1, wherein the concentration of the magnesium chloride solution is 0.2 to 2mol/L, preferably 0.5 to 1.5 mol/L; the concentration of the ammonia water is about 28 wt%; the volume ratio of the magnesium chloride solution to the ammonia water is 100: (0.42-15), preferably 100: (0.83-3.34).
9. A biochar composite loaded with nano magnesium oxide, which is characterized by being prepared by the preparation method of any claim 1 to 8.
10. The application of the biochar composite loaded with nano magnesium oxide as claimed in claim 9 in heavy metal pollution remediation.
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CN114456809A (en) * | 2022-02-25 | 2022-05-10 | 福建农林大学 | Magnesium modified bamboo dust charcoal and application thereof in soil carbon sequestration and emission reduction |
CN116637590A (en) * | 2023-04-11 | 2023-08-25 | 内蒙古工业大学 | Modified magnetic biochar, preparation method and application thereof in adsorbing heavy metals in compost |
CN117531475A (en) * | 2023-10-27 | 2024-02-09 | 中国热带农业科学院橡胶研究所 | Magnesia doped nano magnesium hydroxide loaded biochar and preparation method and application thereof |
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