CN113351153B - MgFe-LDO-MnO 2 Preparation method and application of composite material - Google Patents
MgFe-LDO-MnO 2 Preparation method and application of composite material Download PDFInfo
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- B01J20/00—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof
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- B01J20/04—Solid sorbent compositions or filter aid compositions; Sorbents for chromatography; Processes for preparing, regenerating or reactivating thereof comprising inorganic material comprising compounds of alkali metals, alkaline earth metals or magnesium
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Abstract
The invention discloses MgFe-LDO-MnO 2 A preparation method and application of a composite material belong to the technical field of environmental functional material preparation and heavy metal treatment. Adding a certain amount of Mg 2+ And Fe 3+ Dropwise adding NaOH alkali liquor into the metal mixed solution at 60 ℃ under the stirring condition, keeping the pH value at 10-12, continuously and violently stirring for 4 hours after dropwise adding, then performing water bath aging at 70-80 ℃ for 24-48 hours, and dropwise adding KMnO under the stirring condition at room temperature 4 Then, the mixture is stirred vigorously for 4 hours, and MnCl is added dropwise 2 ·4H 2 Stirring vigorously for 2h after O, aging for 12h at room temperature, centrifuging, washing, drying, and grinding to obtain MgFe-LDH-MnO 2 Calcining the composite material at different temperatures to obtain MgFe-LDO-MnO with super-strong adsorption locking performance 2 A composite material. The preparation method has simple process, convenient operation and mild condition, and the prepared composite material has good effect on As (III) and Pb in water 2+ Strong adsorption capacity and wide application prospect.
Description
Technical Field
The invention belongs to the technical field of preparation of environment function materials and heavy metal ion treatment, and particularly relates to MgFe-LDO-MnO 2 A preparation method and application of the composite material.
Background
Heavy metal ion pollution of water bodies is always a subject of close attention of people, heavy metals are difficult to degrade in nature, and the heavy metals can enter human bodies and animal bodies along with the activities and food chains of human beings, so that the heavy metals can cause harm to the health of the human bodies and the animal bodies even at a trace level. Lead is a typical toxic heavy metal cation in industrial wastewater, and enters the body mainly through the skin, digestive tract and respiratory tract, resulting in anemia, neurological dysfunction, kidney damage and other diseases. Metallic arsenic is an environmental pollutant with high toxicity and carcinogenicity, and is classified as a carcinogen by the international cancer research center. According to the official of the world health organization, at least 5000 million people around the world are facing the threat of local arsenic poisoning, wherein most countries are Asian countries, and China is one of the most seriously harmed countries by arsenic poisoning.
At present, the treatment methods for wastewater containing heavy metals mainly include a chemical precipitation method, an ion exchange method, an adsorption method, a biological method and the like, wherein the adsorption method is widely applied to the treatment of the wastewater containing heavy metals due to the advantages of low cost, simple operation, high efficiency and the like. The selection of a proper adsorbent is very important for quickly and efficiently removing heavy metal ions, common adsorbents include inorganic adsorption materials such as activated carbon, silica gel materials and clay minerals, natural polymer adsorption materials such as cellulose base, chitosan base, lignin base and starch base, biological adsorption materials including bacteria and algae, and industrial wastes such as fly ash and slag are also used as adsorption materials for treating heavy metal-containing wastewater. However, many adsorbents have low adsorption capacity, and the adsorption effect is significantly affected by environmental conditions, easily inhibited by competitive adsorption of other ions, and poor in regeneration effect, so that the actual requirements cannot be met. In view of the above situation, research and development of cheap and efficient adsorbing materials has become one of the key points of research by domestic and foreign scholars.
Layered Double Hydroxides (LDHs) are multimetal compounds with huge specific surface area and high anion exchange capacity, easy artificial synthesis and Layered structure, and the general formula can be expressed as
M is metal, A is an ion, wherein M is 2+ 、M 3+ Each represents divalent (Ca) 2 + 、Mg 2+ 、Zn 2+ 、Mn 2+ And Ni 2+ Etc.) and trivalent (Al) 3+ 、Fe 3+ And Cr 3+ Etc.) metal cations, A n -represents an exchangeable interlayer anion (e.g. Cl-, NO) 3 -、CO 3 2 -etc.), x denotes the plate charge density, M 3+ /(M 2+ +M 3+ ) In the range of 0.17 to 0.33, m is the number of moles of interlayer crystal water, and a value obtained by assuming that m is 1 to Nx/N, wherein N is the number of sites occupied by the anion, and N is the number of charges of the anion. A large number of experiments prove that the Layered metal hydroxide and the composite material thereof can be used as an adsorbent to remove heavy metal ions in water, the adsorption effect is obvious, and meanwhile, the double metal oxides (LDOs) are obtained by a calcination method, so that the adsorption performance of the LDOs on the heavy metals is improved. The research report of fixing elements in the composite material synthesis process by utilizing the LDHs interlayer anion exchange effect is rare. In addition, MnO 2 Is one of the most important compounds in manganese-containing materials, and the most common manganese compound in soil and environmental sediments is MnO in delta type 2 MnO in this form 2 Because the nano-crystalline silicon dioxide has fine particles, low crystallization degree and strong oxidation adsorption performance, the nano-crystalline silicon dioxide can influence the migration and transformation of pollutants in the environment and is often used for repairing polluted wastewater. The manganese oxide and the LDHs are compounded, so that the adsorption capacity of heavy metal ions can be effectively improved, the composite material can be used as an adsorbent for removing the heavy metal ions in wastewater, and the composite material is an ideal adsorption material. Therefore, aiming at the problem of heavy metal pollution, the research takes MgFe-LDH as a precursor and loads manganese dioxide on the precursor to develop MgFe-LDH-MnO 2 Calcining the composite material at 400-600 ℃ for 4-6 h to obtain MgFe-LDO-MnO with super-strong adsorption locking performance 2 A composite material. The preparation of the materials and the application of the materials in the heavy metal polluted water body provide new ideas and techniques for the actual emergency treatment of heavy metal pollutionThe operation support has very important practical significance for the sustainable development of the environment.
Disclosure of Invention
The invention aims to provide MgFe-LDO-MnO 2 A preparation method and application of the composite material. Magnesium nitrate and ferric nitrate are used As mixed metal salt solution, sodium hydroxide alkali solution is used for preparing MgFe-LDH material by adopting a coprecipitation method, manganese compound is loaded on the MgFe-LDH material, and the MgFe-LDH material is calcined for 4-6 hours at 400-600 ℃ to obtain the composite material for As (III) and Pb in water 2+ MgFe-LDO-MnO with high-efficiency removal capability 2 A composite material.
The invention provides a method for preparing MgFe-LDO-MnO 2 The composite material comprises the following specific steps:
(1) adding mixed metal salt with the total metal molar concentration of 0.06-0.1 mol/L into a beaker filled with 200ml of ultrapure water, uniformly mixing, putting on a magnetic stirrer, dropwise adding alkali liquor NaOH under the condition of vigorous stirring at 60 ℃, keeping the pH value of 10-12 after dropwise adding, continuing to vigorously stir at 60 ℃ for 4 hours, and then carrying out water bath aging on the obtained mixture for 24-48 hours at 70-80 ℃;
(2) cooling the precipitate obtained in the step (1) to room temperature, and slowly dropping 200mLKMno under the condition of vigorous stirring 4 Then stirring vigorously for 4 h;
(3) slowly dropping 200mL of MnCl into the mixed solution in the step (2) at room temperature under the condition of stirring 2 After vigorously stirring for 2 hours, carrying out water bath aging at room temperature for 12-24 hours;
(4) washing the precipitate obtained in the step (3) with ultrapure water for 3-6 times, drying for 24-48 hours at the temperature of 75 ℃, finally grinding and sieving with a 200-mesh sieve to obtain the MgFe-LDH-MnO 2 A composite material;
(5) MgFe-LDH-MnO in the step (4) 2 Calcining the composite material for 4-6 hours at the temperature of 400-600 ℃ to obtain MgFe-LDO-MnO 2 A composite material.
The invention provides a method for preparing MgFe-LDO-MnO 2 The composite material is respectively applied to As (III) and Pb in water 2+ The adsorption lock of (1), characterized in that: in the step (1), mixed metal salt solution Mg 2+ /Fe 3+ ＝(2～4)：1，(Mg 2+ +Fe 3 + )/Mn＝(6～10):1。
The dropping mode of the mixed metal salt solution and the alkali solution in the step (1) is a coprecipitation method. Wherein the molar concentration of the NaOH solution is 0.3-0.5 mol/L.
The invention has the advantages that: the preparation method has simple process, convenient operation and mild condition, and the prepared MgFe-LDO-MnO 2 Composite materials for As (III) and Pb in water 2+ Has super strong removal capability, can be used for removing heavy metal ions in wastewater, and has wide application prospect.
Drawings
FIG. 1 shows MgFe-LDO-MnO prepared in the example of the present invention 2 Scanning electron micrographs of the composite (400 ℃).
FIG. 2 shows MgFe-LDO-MnO prepared in the example of the present invention 2 (400 ℃) X-ray diffraction pattern of the composite material.
FIG. 3 shows MgFe-LDO-MnO prepared in the example of the present invention 2 And (3) a graph showing the change of the adsorption removal rate of the composite material (calcined at 400-600 ℃) on As (III).
FIG. 4 shows MgFe-LDH-MnO prepared in the example of the present invention 2 、MgFe-LDO-MnO 2 (400 ℃ calcination) composite material has a graph showing the change of As (III) adsorption removal rate at different initial pH values.
FIG. 5 is MgFe-LDH-MnO prepared in the example of the present invention 2 、MgFe-LDO-MnO 2 (400 ℃ calcination) the amount of the added material was varied in the As (iii) adsorption removal rate at pH 5.
FIG. 6 shows MgFe-LDO-MnO prepared in the example of the present invention 2 Composite material (calcined at 400-600 ℃) for Pb 2+ Graph showing the change in adsorption removal rate.
FIG. 7 shows MgFe-LDH-MnO prepared in the example of the present invention 2 、MgFe-LDO-MnO 2 (400 ℃ calcination) of the composite at different initial pH values for Pb 2+ Graph showing the change in adsorption removal rate.
FIG. 8 shows MgFe-LDH-MnO prepared in the example of the present invention 2 、MgFe-LDO-MnO 2 (calcined at 400 ℃) the composite material was dosed with Pb in an amount corresponding to the pH 5 2+ Graph showing the change in adsorption removal rate.
Detailed Description
Example 1:
preparation of MgFe-LDH-MnO 2 、MgFe-LDO-MnO 2 The composite material comprises the following components:
(1) mixing metal salt (Mg) with total metal molar concentration of 0.08mol/L 2+ /Fe 3+ 1) adding the mixture into a beaker filled with 200ml of ultrapure water, uniformly mixing, putting the mixture on a magnetic stirrer, dropwise adding 0.4mol/L NaOH alkali liquor under the condition of vigorous stirring at 60 ℃, keeping the pH value at 10.5, continuing to vigorously stir at 60 ℃ for 4 hours, and carrying out water bath aging on the obtained mixture for 48 hours at 80 ℃;
(2) cooling the precipitate obtained in step (1) to 30 deg.C, and slowly dropping 200mL KMnO with concentration of 4mmol/L under vigorous stirring 4 Keeping the temperature at 30 ℃ and stirring vigorously for 4 hours;
(3) 200mL of 6mmol/L MnCl solution is slowly dropped into the mixed solution in the step (2) at the temperature of 30 ℃ under the stirring condition 2 After vigorously stirring for 2h, aging for 12h in water bath at room temperature;
(4) washing the precipitate obtained in the step (3) with ultrapure water for 3-6 times, drying for 24 hours at the temperature of 75 ℃, finally grinding and sieving with a 200-mesh sieve to obtain MgFe-LDH-MnO 2 A composite material;
(5) MgFe-LDH-MnO in the step (4) 2 Calcining the composite material at 400-600 ℃ for 5 hours to obtain MgFe-LDO-MnO 2 A composite material.
Example 2:
FIG. 1 shows MgFe-LDO-MnO prepared in this example 2 (400 ℃ calcination) SEM image of the composite (characterized using a field emission scanning electron microscope (SEM, JGM-1900-F)).
FIG. 2 shows MgFe-LDO-MnO prepared in this example 2 (calcined at 400 ℃) XRD pattern of the composite (characterised by X-ray diffractometry (XRD, X' Pert3 Powder)).
Example 3:
with MgFe-LDH-MnO prepared in the examples of the present invention 2 、MgFe-LDO-MnO 2 The composite material was subjected to adsorption experiments for removing As (III).
(1) 0.03g of MgFe-LDO-MnO prepared in this example was weighed out separately 2 (400-600 ℃ calcination) the composite material is placed in a series of 50mL plastic centrifuge tubes, 30mL of 50mg/L As (III) solution (original pH) is added, the mixture is shaken to balance in a constant temperature oscillator at the temperature of 25 ℃ and the rotation speed of 160rpm, then the mixture is filtered by a 0.22 mu m filter membrane, and the concentration of As (III) is measured by an inductively coupled plasma mass spectrometer. The results are shown in FIG. 3.
(2) 0.03g of MgFe-LDH-MnO prepared in this example was weighed out separately 2 、MgFe-LDO-MnO 2 The composite material (calcined at 400 ℃) is placed in a series of 50mL plastic centrifuge tubes, 30mL of As (III) solution with the concentration of 50mg/L is added, the pH value is adjusted to a set value (2-12) by 0.1mol/L of HCl or NaOH solution, the composite material is shaken to be balanced in a constant temperature oscillator with the temperature of 25 ℃ and the rotating speed of 160rpm, then the composite material is filtered by a filter membrane with the diameter of 0.22 mu m, and the concentration of As (III) is measured by an inductively coupled plasma mass spectrometer. The results are shown in FIG. 4.
(3) 150, 300, 450, 600, 750, 900mg of MgFe-LDH-MnO prepared in this example were weighed out separately 2 、MgFe-LDO-MnO 2 (400 ℃ C. calcination) the composite material was placed in a series of 50mL plastic centrifuge tubes, 30mL of 50mg/L As (III) solution (0.1mol/L HCl or NaOH solution to adjust pH) adjusted to pH 5.0 was added, the mixture was shaken to equilibrium in a constant temperature shaker at 25 ℃ and 160rpm, filtered through a 0.22 μm filter, and the concentration of As (III) was measured using an inductively coupled plasma mass spectrometer. The results are shown in FIG. 5.
Example 4:
with MgFe-LDH-MnO prepared in the examples of the present invention 2 、MgFe-LDO-MnO 2 Composite material for removing Pb 2+ Adsorption experiment of (1).
(1) 0.03g of MgFe-LDO-MnO prepared in this example was weighed out separately 2 (calcined at 400-600 ℃) the composite material is placed in a series of 50mL plastic centrifuge tubes, and 30mL Pb with the concentration of 500mg/L is added 2+ Shaking the original pH solution in a constant temperature oscillator at 25 deg.C and 160rpm to balance, filtering with 0.22 μm filter membrane, and measuring Pb with inductively coupled plasma mass spectrometer 2+ The concentration of (c). The results are shown in FIG. 6.
(2) 0.03g of MgFe-LDH-MnO prepared in this example was weighed out separately 2 、MgFe-LDO-MnO 2 (400 ℃ C. calcination) the composite was placed in a series of 50mL plastic centrifuge tubes and 30mL Pb at 500mg/L was added 2+ Adjusting the pH of the solution to a set value (2-8) by using 0.1mol/L HCl or NaOH solution, oscillating the solution to be balanced in a constant temperature oscillator at the temperature of 25 ℃ and the rotating speed of 160rpm, filtering the solution by using a filter membrane of 0.22 mu m, and measuring Pb by using an inductively coupled plasma mass spectrometer 2+ The concentration of (c). The results are shown in FIG. 7.
(3) 150, 300, 450, 600, 750 and 900mg of MgFe-LDH-MnO prepared in this example were weighed out separately 2 、MgFe-LDO-MnO 2 (400 ℃ C. calcination) the composite was placed in a series of 50mL plastic centrifuge tubes and 30mL of adjusted pb at 500mg/L pH 5.0 was added 2+ Adjusting pH of the solution (0.1mol/L HCl or NaOH solution), oscillating in a constant temperature oscillator at 25 deg.C and 160rpm to balance, filtering with 0.22 μm filter membrane, and measuring Pb with inductively coupled plasma mass spectrometer 2+ The concentration of (c). The results are shown in FIG. 8.
Claims (3)
1. MgFe-LDO-MnO 2 The preparation method of the composite material is characterized by comprising the following specific steps:
(1) adding mixed metal salt with the total metal molar concentration of 0.06-0.1 mol/L into a beaker filled with 200ml of ultrapure water, uniformly mixing, putting on a magnetic stirrer, dropwise adding alkali liquor NaOH under the condition of vigorous stirring at 60 ℃, keeping the pH value of 10-12 after dropwise adding, continuing to vigorously stir at 60 ℃ for 4 hours, and then carrying out water bath aging on the obtained mixture for 24-48 hours at 70-80 ℃;
(2) cooling the precipitate obtained in step (1) to room temperature, and slowly dropping 200mL KMnO under vigorous stirring 4 Then stirring vigorously for 4 h;
(3) slowly dropping 200mL of MnCl into the mixed solution in the step (2) at room temperature under the condition of stirring 2 After vigorously stirring for 2 hours, carrying out water bath aging at room temperature for 12-24 hours;
(4) using the precipitate obtained in step (3)Washing with ultrapure water for 3-6 times, drying at 75 ℃ for 24-48 hours, grinding and sieving with a 200-mesh sieve to obtain MgFe-LDH-MnO 2 A composite material;
(5) MgFe-LDH-MnO in the step (4) 2 Calcining the composite material for 4-6 hours at 400 ℃ to obtain MgFe-LDO-MnO 2 A composite material.
2. The MgFe-LDO-MnO of claim 1 2 The preparation method of the composite material is characterized by comprising the following steps: in the step (1), mixed metal salt solution Mg 2+ /Fe 3+ ＝3:1，(Mg 2+ +Fe 3+ )/Mn＝8:1。
3. MgFe-LDO-MnO prepared by the method of claim 1 or 2 2 The application of the composite material is characterized in that the MgFe-LDO-MnO is 2 Application of composite material in treating As (III) and Pb in water 2+ Adsorption of (3).
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