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 PDF

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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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mxene
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metal complex
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CN113087117B (en
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李长平
宋浩然
祖道远
李琢
王玉伟
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Dongguan University of Technology
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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
    • 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
    • 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
    • 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

本发明涉及一种MXene强化类芬顿氧化降解重金属络合物和回收重金属的方法，属于环境保护领域。包括以下步骤：在含重金属络合物的废水中投加浓度为0.1～100mg/L的MXene和浓度为0.1～100mM的过硫酸盐或过氧化氢，搅拌反应10～90min。本方法pH应用范围广、无需额外添加低价态过渡金属离子、无需反复调节pH值，能够实现重金属络合物高效降解与重金属同步回收。

Figure 202110476968

The invention relates to a method for MXene-enhanced Fenton-like oxidative degradation of heavy metal complexes and recovery of heavy metals, belonging to the field of environmental protection. The method includes the following steps: adding MXene with a concentration of 0.1-100 mg/L and persulfate or hydrogen peroxide with a concentration of 0.1-100 mM in the wastewater containing heavy metal complexes, and stirring and reacting for 10-90 minutes. The method has a wide pH application range, does not need to add low-valent transition metal ions, and does not need to repeatedly adjust the pH value, and can achieve efficient degradation of heavy metal complexes and simultaneous recovery of heavy metals.

Figure 202110476968

Description

MXene enhanced Fenton-like oxidative degradation heavy metal complex and method for recovering heavy metal
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.
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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)

1.一种MXene强化类芬顿氧化降解重金属络合物和回收重金属的方法，其特征在于：具体步骤如下：1. a method for MXene strengthening class Fenton oxidative degradation heavy metal complex and reclaiming heavy metal, it is characterized in that: concrete steps are as follows: (1)在含重金属络合物的废水中投加0.1～100mg/L MXene和0.1～100mM氧化剂，在10～30℃下搅拌反应10～90分钟；(1) Add 0.1-100 mg/L MXene and 0.1-100 mM oxidant to the wastewater containing heavy metal complexes, and stir and react at 10-30°C for 10-90 minutes; (2)将步骤(1)反应后溶液静置或者过滤使固液分离，使用酸洗液清洗沉淀物或滤渣，回收重金属；(2) the solution after the reaction of step (1) is left standing or filtered to separate the solid and liquid, and the pickling solution is used to clean the sediment or the filter residue to recover the heavy metals; (3)清洗后的MXene在冷冻干燥之后重复利用。(3) The washed MXene is reused after freeze-drying. 2.根据权利要求1所述的一种MXene强化类芬顿氧化降解重金属络合物和回收重金属的方法，其特征在于：所述重金属络合物为重金属与络合剂形成的重金属络合物，所述重金属为Cu、Ni、Pb、Cd、Fe、Zn、Cr、Ag、Hg、Co、As或Tl，所述络合剂为乙二胺四乙酸、柠檬酸、酒石酸、氨三乙酸铵或二乙醇胺。2. the method for a kind of MXene strengthening class Fenton oxidative degradation heavy metal complex and reclaiming heavy metal according to claim 1, is characterized in that: described heavy metal complex is the heavy metal complex 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 EDTA, citric acid, tartaric acid, ammonium triacetate or diethanolamine. 3.根据权利要求1所述一种MXene强化类芬顿氧化降解重金属络合物和回收重金属的方法，其特征在于：所述的MXene为二维过渡金属碳化物或氮化物。3. the method for a kind of MXene-enhanced Fenton-like oxidative degradation of heavy metal complexes and recovery of heavy metals according to claim 1, is characterized in that: described MXene is two-dimensional transition metal carbide or nitride. 4.根据权利要求1所述一种MXene强化类芬顿氧化降解重金属络合物和回收重金属的方法，其特征在于：所述MXene是结构式为Mn+1Xn的二维材料，n＝1、2、3，M为Sc、Ti、V、Cr、Zr、Nb、Mo、Hf或Ta，X为C或者N。4. the method for a kind of MXene-enhanced Fenton-like oxidative degradation of heavy metal complexes and recovery of heavy metals according to claim 1, is characterized in that: described MXene is a two-dimensional material whose structural formula is Mn + 1Xn, n = 1, 2, 3, M is Sc, Ti, V, Cr, Zr, Nb, Mo, Hf or Ta, X is C or N. 5.根据权利要求1所述一种MXene强化类芬顿氧化降解重金属络合物和回收重金属的方法，其特征在于：所述氧化剂为过硫酸盐或过氧化氢。5. the method for a kind of MXene strengthening class Fenton oxidative degradation heavy metal complex and reclaiming heavy metal according to claim 1, is characterized in that: described oxidizing agent is persulfate or hydrogen peroxide. 6.根据权利要求5所述一种MXene强化类芬顿氧化降解重金属络合物和回收重金属的方法，其特征在于：所述过硫酸盐为过二硫酸盐和单过硫酸盐。6. the method for a kind of MXene strengthening class Fenton oxidative degradation heavy metal complex and reclaiming heavy metal according to claim 5, is characterized in that: described persulfate is peroxodisulfate and monopersulfate. 7.根据权利要求6所述一种MXene强化类芬顿氧化降解重金属络合物和回收重金属的方法，其特征在于：所述二硫酸盐为过硫酸钠或过硫酸钾；所述单过硫酸盐为过一硫酸氢钾。7. the method for a kind of MXene strengthening class Fenton oxidative degradation heavy metal complex and reclaiming heavy metal according to claim 6, is characterized in that: described disulfate is sodium persulfate or potassium persulfate; Described monopersulfuric acid The salt is potassium hydrogen peroxymonosulfate. 8.根据权利要求1所述的一种MXene强化类芬顿氧化降解重金属络合物和回收重金属的方法，其特征在于：所述的酸洗液为稀盐酸、稀硫酸或稀硝酸。8. the method for a kind of MXene strengthening class Fenton oxidative degradation heavy metal complex and reclaiming heavy metal according to claim 1, is characterized in that: described pickling solution is dilute hydrochloric acid, dilute sulfuric acid or dilute nitric acid. 9.根据权利要求1所述的一种MXene强化类芬顿氧化降解重金属络合物和回收重金属的方法，其特征在于：所述步骤(1)在含50μM重金属络合物的废水中投加10～60mg/L MXene和2～20mM氧化剂，在25℃下搅拌反应20～60分钟。9. the method for a kind of MXene-enhanced Fenton-like oxidative degradation of heavy metal complexes and reclaiming heavy metals according to claim 1, is characterized in that: described step (1) is added in the waste water containing 50 μM heavy metal complexes 10-60 mg/L MXene and 2-20 mM oxidant were stirred at 25°C for 20-60 minutes. 10.根据权利要求1所述的一种MXene强化类芬顿氧化降解重金属络合物和回收重金属的方法，其特征在于：所述步骤(3)清洗后的MXene在-40℃～-10℃冷冻干燥23～25h之后重复利用。10 . The method for MXene-enhanced Fenton-like oxidative degradation of heavy metal complexes and recovery of heavy metals according to claim 1, wherein the MXene after cleaning in the step (3) is at a temperature of -40°C to -10°C. Reuse after freeze-drying for 23-25h.
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CN115676892A (en) * 2022-11-03 2023-02-03 东莞理工学院 A kind of preparation method of trivalent manganese
CN115676892B (en) * 2022-11-03 2024-03-29 东莞理工学院 A method for preparing trivalent manganese
CN116987899A (en) * 2023-08-30 2023-11-03 昆明理工大学 Method for recovering metallic silver from printing film and fixing solution
CN119551798A (en) * 2024-11-27 2025-03-04 中国环境科学研究院 A Fenton-like catalytic system and its application in the degradation of acetaminophen

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