CN113087117A - MXene enhanced Fenton-like oxidative degradation heavy metal complex and method for recovering heavy metal - Google Patents
MXene enhanced Fenton-like oxidative degradation heavy metal complex and method for recovering heavy metal Download PDFInfo
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- CN113087117A CN113087117A CN202110476968.1A CN202110476968A CN113087117A CN 113087117 A CN113087117 A CN 113087117A CN 202110476968 A CN202110476968 A CN 202110476968A CN 113087117 A CN113087117 A CN 113087117A
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- C—CHEMISTRY; METALLURGY
- C02—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F—TREATMENT OF WATER, WASTE WATER, SEWAGE, OR SLUDGE
- C02F1/00—Treatment of water, waste water, or sewage
- C02F1/72—Treatment of water, waste water, or sewage by oxidation
- C02F1/722—Oxidation by peroxides
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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
- C02F1/70—Treatment of water, waste water, or sewage by reduction
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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
- C02F2101/20—Heavy metals or heavy metal 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
- C02F2305/00—Use of specific compounds during water treatment
- C02F2305/02—Specific form of oxidant
- C02F2305/026—Fenton's reagent
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Abstract
The invention relates to a method for MXene reinforced Fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal, and belongs to the field of environmental protection. The method comprises the following steps: MXene with the concentration of 0.1-100 mg/L and persulfate or hydrogen peroxide with the concentration of 0.1-100 mM are added into the wastewater containing the heavy metal complex, and the mixture is stirred and reacted for 10-90 min. The method has wide pH application range, does not need to additionally add low-valence transition metal ions and repeatedly adjust the pH value, and can realize high-efficiency degradation of the heavy metal complex and synchronous recovery of the heavy metal.
Description
Technical Field
The invention relates to the technical field of environmental protection, in particular to a method for MXene enhanced Fenton-like oxidative degradation of a heavy metal complex and recovery of heavy metals.
Background
The heavy metal complex has strong stability in a wide pH range, and is difficult to effectively remove by traditional free heavy metal ion treatment methods such as adsorption, alkali precipitation, ion exchange and the like. The development of a novel high-efficiency heavy metal complex treatment technology is of great significance.
In recent years, advanced oxidation techniques have been studied in the field of removal of heavy metal complexes. The heavy metal complex can be oxidized and broken by active species with strong oxidizing property generated by modes of electrocatalysis, photocatalysis, heterogeneous catalyst catalysis and the like, free heavy metal is released, and heavy metal ions are precipitated and removed by treatment methods such as alkali precipitation and the like. However, the method still cannot realize the synchronous removal and recovery of heavy metals with high added values, and a large amount of acid-base reagents are consumed.
Therefore, it is very important to develop a method which has a wide pH application range, does not need to additionally add low-valence transition metal ions, does not need to repeatedly adjust the pH value, and can realize the high-efficiency degradation of the heavy metal complex and the synchronous recovery of the heavy metal.
Disclosure of Invention
Aiming at the defects of the prior art, the invention provides a method for MXene enhanced Fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal, the method has wide pH application range, does not need to additionally add low-valence transition metal ions, does not need to repeatedly adjust the pH value, can realize high-efficiency degradation of the heavy metal complex and synchronous recovery of the heavy metal, simplifies the process flow of heavy metal complex treatment, and reduces the utilization of the low-valence transition metal catalyst.
The technical scheme of the invention is realized as follows:
a method for MXene reinforced Fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal comprises the following specific steps:
(1) 0.1-100 mg/L MXene and 0.1-100 mM oxidant are added into the wastewater containing the heavy metal complex, and the mixture is stirred and reacts for 10-90 minutes at the temperature of 10-30 ℃;
(2) standing the solution obtained in the step (1) or filtering the solution to separate solid from liquid, washing precipitates or filter residues by using a pickling solution, and recovering heavy metals;
(3) the washed MXene was recycled after freeze-drying.
Preferably, the heavy metal complex is formed by heavy metal and complexing agent, the heavy metal is Cu, Ni, Pb, Cd, Fe, Zn, Cr, Ag, Hg, Co, As or Tl, and the complexing agent is ethylenediamine tetraacetic acid, citric acid, tartaric acid, ammonium aminotriacetate or diethanolamine.
Preferably, MXene refers to a multi-or few-layer two-dimensional transition metal carbide or nitride.
Preferably, MXene is of the formula Mn+1XnN is 1, 2 or 3, M is Sc, Ti, V, Cr, Zr, Nb, Mo, Hf or Ta, and X is C or N.
Preferably, MXene is Ti3C2MXene or NbC MXene.
Preferably, the oxidizing agent is a persulfate or hydrogen peroxide.
Preferably, the persulfate is a peroxydisulfate and a monopersulfate.
Preferably, the disulfate salt is sodium persulfate or potassium persulfate; the monopersulfate is potassium peroxymonosulfate.
Preferably, the acid washing solution is dilute hydrochloric acid, dilute sulfuric acid or dilute nitric acid.
Preferably, in the step (1), 10-60 mg/L MXene and 2-20 mM oxidant are added into the wastewater containing 50 MuM heavy metal complex, and the mixture is stirred and reacts for 20-60 minutes at 25 ℃.
Preferably, MXene cleaned in the step (3) is repeatedly used after being frozen and dried for 23-25 h at-40 to-10 ℃.
The invention has the following beneficial effects:
(1) the MXene material is adopted, because the large specific surface area and the surface electronegativity of the MXene material are beneficial to adsorption of free heavy metals, and meanwhile, the MXene material also has reducibility, and can reduce high-valence heavy metals to generate low-valence metals to further promote activation of an oxidant and enhance removal of complex heavy metals.
(2) The MXene enhanced Fenton-like oxidative degradation heavy metal complex and the method for recovering heavy metal can realize high-efficiency degradation of the heavy metal complex and synchronous recovery of the heavy metal by one step without additionally adding a low-valence transition metal catalyst, and compared with the existing two-step heavy metal complex treatment methods such as high-grade oxidation-alkali precipitation and the like, the method simplifies the process treatment flow and reduces the use of the low-valence transition metal and an acid-base reagent.
Drawings
FIG. 1 is a graph showing the effect of example 1 on the removal of copper, a heavy metal in a complex state, by using the method of the present invention.
FIG. 2 shows example 1 using the technique of the present invention with different Ti3C2The effect of the dosage on removing the complex heavy metal copper is shown.
Detailed Description
For a more clear understanding of the technical features, objects and advantages of the present invention, reference is now made to the following detailed description of the embodiments of the present invention taken in conjunction with the accompanying drawings, which are included to illustrate and not to limit the scope of the present invention.
Example 1
A method for MXene reinforced Fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal comprises the following specific steps:
(1) selecting Ti3C2MXene, the target pollutant is selected from ethylenediaminetetraacetic acid copper complex (EDTA-Cu), and the oxidant is selected from potassium hydrogen Peroxymonosulfate (PMS). To the beaker were added 50. mu.M EDTA-Cu solution, 60mg/LTi in order3C2And 1mM potassium monopersulfate. The reaction solution was rapidly stirred using a magnetic stirrer at a stirring speed of 500rpm, and after 20 minutes of reaction, the concentration of Cu element in the reaction solution was measured using an inductively coupled plasma mass spectrometer (ICP-MS), and the Cu ion removal rate was 85%.
(2) And (2) standing the solution obtained after the reaction in the step (1) or filtering the solution to separate solid from liquid, washing the precipitate or filter residue by using an acid washing solution, and recovering the heavy metal.
(3) The washed MXene is repeatedly used after being frozen and dried for 24h at the temperature of-10 ℃.
Example 2
A method for MXene reinforced Fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal comprises the following specific steps:
(1) selecting Ti3C2MXene, the target pollutant is selected from a citric acid copper complex, and the oxidant is selected from sodium persulfate. To the beaker were added 50. mu.M of a copper citrate complex solution and 100mg/L of Ti in this order3C2And 2mM sodium persulfate. The reaction solution was rapidly stirred with a magnetic stirrer at a stirring speed of 700rpm, and after 90 minutes of reaction, the concentration of Cu element in the reaction solution was measured with an inductively coupled plasma mass spectrometer (ICP-MS), and the Cu ion removal rate was 97%.
(2) And (2) standing the solution obtained after the reaction in the step (1) or filtering the solution to separate solid from liquid, washing the precipitate or filter residue by using an acid washing solution, and recovering the heavy metal.
(3) The washed MXene is repeatedly used after being frozen and dried for 23h at the temperature below-20 ℃.
Example 3
A method for MXene reinforced Fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal comprises the following specific steps:
(1) selecting Nb2C MXene, the target pollutant is selected from an ethylene diamine tetraacetic acid iron complex (EDTA-Fe), and the oxidant is selected from hydrogen peroxide. To the beaker were added 50. mu.M EDTA-Fe solution, 10mg/LNb in order2C and 20mM hydrogen peroxide. Rapidly stirring by using a magnetic stirrer at the stirring speed of 500rpm, and measuring the concentration of Fe element in the reaction solution by using an inductively coupled plasma mass spectrometer (ICP-MS) after reacting for 30 minutes, wherein the removal rate of Fe ions is 92%.
(2) And (2) standing the solution obtained after the reaction in the step (1) or filtering the solution to separate solid from liquid, washing the precipitate or filter residue by using an acid washing solution, and recovering the heavy metal.
(3) The washed MXene is repeatedly used after being frozen and dried for 24h at the temperature below-30 ℃.
Example 4
A method for MXene reinforced Fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal comprises the following specific steps:
(1) selecting Nb2C MXene, the target pollutant is selected from ethylene diamine tetraacetic acid lead complex (EDTA-Pb), and the oxidant is selected from potassium hydrogen peroxymonosulfate. To the beaker were added 50. mu.M EDTA-Pb solution, 10mg/LNb in that order2C and 20mM potassium hydrogen peroxymonosulfate. The reaction solution was rapidly stirred with a magnetic stirrer at a stirring speed of 800rpm, and after 60 minutes of reaction, the concentration of Pb element in the reaction solution was measured with an inductively coupled plasma mass spectrometer (ICP-MS), and the Pb ion removal rate was 87%.
(2) And (2) standing the solution obtained after the reaction in the step (1) or filtering the solution to separate solid from liquid, washing the precipitate or filter residue by using an acid washing solution, and recovering the heavy metal.
(3) The washed MXene is repeatedly used after being frozen and dried for 25h at the temperature below-40 ℃.
The above embodiments are merely provided to help understand the method and core principle of the present invention, and the main steps and embodiments of the present invention are described in detail by using specific examples. To those skilled in the art, the various conditions and parameters may be varied as desired in a particular implementation in accordance with the principles of the invention, and in view of the foregoing, the description is not to be taken as limiting the invention.
Claims (10)
1. A method for MXene reinforced Fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal is characterized by comprising the following steps: the method comprises the following specific steps:
(1) 0.1-100 mg/L MXene and 0.1-100 mM oxidant are added into the wastewater containing the heavy metal complex, and the mixture is stirred and reacts for 10-90 minutes at the temperature of 10-30 ℃;
(2) standing the solution obtained in the step (1) or filtering the solution to separate solid from liquid, washing precipitates or filter residues by using a pickling solution, and recovering heavy metals;
(3) the washed MXene was recycled after freeze-drying.
2. The method for MXene enhanced Fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal according to claim 1, wherein: the heavy metal complex is formed by heavy metal and a complexing agent, the heavy metal is Cu, Ni, Pb, Cd, Fe, Zn, Cr, Ag, Hg, Co, As or Tl, and the complexing agent is ethylenediamine tetraacetic acid, citric acid, tartaric acid, ammonium aminotriacetate or diethanolamine.
3. The method for MXene enhanced Fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal according to claim 1, wherein: the MXene is two-dimensional transition metal carbide or nitride.
4. The method for MXene enhanced Fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal according to claim 1, wherein: MXene is the structural formula Mn+1XnN is 1, 2 or 3, M is Sc, Ti, V, Cr, Zr, Nb, Mo, Hf or Ta, and X is C or N.
5. The method for MXene enhanced Fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal according to claim 1, wherein: the oxidant is persulfate or hydrogen peroxide.
6. The method for MXene enhanced Fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal according to claim 5, wherein: the persulfate is peroxydisulfate and monopersulfate.
7. The method for MXene enhanced Fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal according to claim 6, wherein: the dithionate is sodium persulfate or potassium persulfate; the monopersulfate is potassium peroxymonosulfate.
8. The method for MXene enhanced Fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal according to claim 1, wherein: the pickling solution is dilute hydrochloric acid, dilute sulfuric acid or dilute nitric acid.
9. The method for MXene enhanced Fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal according to claim 1, wherein: in the step (1), MXene and 2-20 mM oxidant are added into the wastewater containing 50 mu M heavy metal complex, and the mixture is stirred and reacted for 20-60 minutes at 25 ℃.
10. The method for MXene enhanced Fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal according to claim 1, wherein: and (4) repeatedly utilizing the MXene cleaned in the step (3) after freeze drying for 23-25 h at-40 to-10 ℃.
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| CN202110476968.1A CN113087117B (en) | 2021-04-29 | 2021-04-29 | MXene enhanced Fenton-like oxidative degradation heavy metal complex and method for recovering heavy metal |
| PCT/CN2021/135161 WO2022227571A1 (en) | 2021-04-29 | 2021-12-02 | Method for mxene-enhanced fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal |
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| CN113559872A (en) * | 2021-07-30 | 2021-10-29 | 四川大学 | Catalyst for activating persulfate, preparation method and application |
| CN113697930A (en) * | 2021-09-04 | 2021-11-26 | 河海大学 | Method for removing pollutants in water |
| WO2022227571A1 (en) * | 2021-04-29 | 2022-11-03 | 东莞理工学院 | Method for mxene-enhanced fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal |
| CN115676892A (en) * | 2022-11-03 | 2023-02-03 | 东莞理工学院 | Preparation method of trivalent manganese |
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| CN116212882B (en) * | 2023-03-31 | 2024-04-26 | 中国科学院生态环境研究中心 | Layered copper-based solid Fenton catalyst and preparation method and application thereof |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| WO2022227571A1 (en) * | 2021-04-29 | 2022-11-03 | 东莞理工学院 | Method for mxene-enhanced fenton-like oxidative degradation of heavy metal complex and recovery of heavy metal |
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| CN113697930A (en) * | 2021-09-04 | 2021-11-26 | 河海大学 | Method for removing pollutants in water |
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