CN107281999B - Iron oxide/manganese dioxide nano composite material and preparation method and application thereof - Google Patents
Iron oxide/manganese dioxide nano composite material and preparation method and application thereof Download PDFInfo
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Abstract
An iron oxide/manganese dioxide nano composite material and a preparation method and application thereof, belonging to the technical field of composite materials. Adding soluble ferrous salt and divalent manganese salt into an ethanol water solution, then adding an ammonium carbonate solution, reacting to obtain an iron-manganese compound precursor, and adding the iron-manganese compound precursor into a potassium permanganate solution for reacting to obtain the microsphere with a porous structure and composed of nano particles. Used for adsorbing heavy metal ions in water.
Description
Technical Field
The invention relates to an iron oxide/manganese dioxide composite material and a preparation method and application thereof, belonging to the technical field of composite materials.
Background
The heavy metal ion content in underground water in many areas of China exceeds the national safe drinking water standard, and the life and health of people are seriously threatened. The nano adsorbent has a good effect of removing heavy metal ions, and a plurality of nano materials are applied to water treatment at present.
Meanwhile, the nano iron oxide has high specific surface area and good affinity for heavy metal ions, is low in cost, safe and non-toxic, and is one of the most common water pollutant removal materials2O3) Amorphous hydrated iron oxide, maghemite (-Fe)2O3) Magnetite (Fe)3O4) And iron/iron oxide (Fe @ Fe)xOy) And the like. Over the past decades, nanostructured manganese oxidesCompounds have also been developed for adsorbing cationic or anionic contaminants such as heavy metal ions, arsenates and phosphates in water. Among the manganese oxides widely studied include Hydrated Manganese Oxide (HMO) and nanoporous/nanotunneling manganese oxide. The manganese dioxide has redox characteristics, so that the manganese dioxide can react with pollutants in water, and heavy metal ions which are high in toxicity and difficult to adsorb can be oxidized and reduced into ions which are lower in toxicity and easier to adsorb.
The synergistic effect of the components is utilized to prepare the composite material, which is a feasible measure for improving the comprehensive performance of the nano material. Because underground water usually contains various heavy metal ions, the iron oxide and the manganese dioxide are compounded to prepare the safe and efficient multifunctional water treatment material, which has important significance for reducing the preparation cost and simplifying the process. Meanwhile, the heavy metal ions in water in different regions are different, and the adjustment of the adsorption performance of the adsorption material is realized by simply regulating and controlling the components of the adsorption material, so that the application range of the material in water treatment is also expanded.
Disclosure of Invention
The invention aims to provide an iron oxide/manganese dioxide composite material and a method thereof
The invention provides a method for preparing an iron oxide/manganese dioxide composite material, which comprises the following steps:
(1) weighing a certain amount of soluble ferrous salt and divalent manganese salt according to the molar ratio of iron to manganese of 2/8-8/2, adding the soluble ferrous salt and divalent manganese salt into a mixed solution of ethanol and water, and stirring and dissolving to obtain a solution A; the concentration ranges of the ferrous salt and the divalent manganese salt in the solution are both 0.025-0.1 mmol/L; the volume ratio of water to ethanol in the mixed liquid of ethanol and water is preferably 7: 1;
(2) adding ammonium carbonate into water, stirring and dissolving to obtain an ammonium carbonate aqueous solution B with the concentration of 0.01-0.1 mol/L;
(3) under the stirring condition, adding an ammonium carbonate aqueous solution B into the solution A (preferably quickly adding the ammonium carbonate aqueous solution B for 1-10 s), continuously stirring for 2-4 h, preferably 3h to obtain an iron-manganese compound precursor dispersion liquid, and standing to obtain a brown precipitate; washing the precipitate, and drying at 60-100 ℃ to obtain a precursor of the iron-manganese compound;
(4) and (4) adding the compound precursor obtained in the step (3) into a potassium permanganate solution to react for 10-20 hours, separating and washing the precipitate, and drying at 60-100 ℃ to obtain a final product.
In the preparation method, the ferrous salt can be one or the mixture of two of ferrous chloride and ferrous sulfate heptahydrate; the manganese salt can be one or more of manganese sulfate, manganese chloride and manganese nitrate.
The total molar ratio of ammonium carbonate to iron and manganese in the step (3) is 1 (1-4), preferably 1: 3;
the concentration of the potassium permanganate solution in the step (4) is 0.02-0.05 mol/L; preferably, 1-300mg of the compound precursor is correspondingly added into every 10ml of the potassium permanganate aqueous solution;
wherein in the further step (1), the compound structure obtained when the molar ratio of iron to manganese is Fe/Mn 7/3 is FeOOH/MnO2(ii) a The Fe/Mn ratio of Fe/Mn is 5:5, the structure of the compound is Fe2O3/MnO2(ii) a When Fe/Mn is 3:7, the ferric oxide is in an amorphous structure.
Stirring in the step (1), wherein the temperature is room temperature, and the time is not less than 5min, specifically 10-40 min;
the iron oxide/manganese dioxide composite material provided by the invention is a microsphere with a porous structure and composed of nano particles.
The iron oxide/manganese dioxide prepared by the method is used for adsorbing heavy metal ions in water. Such as: at least one of lead ions, cadmium ions, mercury ions and arsenate ions.
The invention provides a safe, simple and economical method for preparing an iron oxide/manganese dioxide composite material. Compared with the prior art, the method has the following characteristics:
1) in the invention, the reaction condition is mild, the reaction can be completed at room temperature, the preparation process of the material is simple and safe, the energy consumption is low, and the large-scale production is convenient to realize.
2) The raw materials adopted by the invention are economic, green and environment-friendly, and do not relate to the addition of a surfactant.
3) The surface of the composite material obtained by the invention is a porous structure consisting of nano particles, so that the specific surface area is very high.
4) In the preparation process, the iron oxide/manganese dioxide composite material composed of different mechanisms can be obtained by simply regulating and controlling the raw material proportion
5) The iron oxide/manganese dioxide composite material obtained by the invention shows excellent capability of synchronously removing various heavy metal ions in the water treatment process.
Drawings
FIG. 1 is an X-ray powder diffraction pattern (XRD) of the products obtained in examples 1-3 using different Fe/Mn ratios, respectively. Curves 1, 2 and 3 show the diffraction patterns of the products obtained with Fe/Mn ratios 7/3, 1/1 and 3/7, respectively.
FIG. 2 is a Scanning Electron Microscope (SEM) photograph of the products obtained in examples 1-3, respectively, using different Fe/Mn ratios. Wherein panels (a), (b), and (c) are SEM photographs of the products obtained at Fe/Mn ratios of 7/3, 1/1, and 3/7, respectively.
FIG. 3 is a graph showing the adsorption isotherms of the products obtained in examples 1-3 using different Fe/Mn ratios for the lead ions and the arsenate ions of the contaminants, respectively. Wherein, the graphs (a) and (b) are respectively the adsorption isotherm curves of the iron oxide/manganese dioxide composite material on lead ions and arsenate.
Detailed Description
The present invention will be further illustrated with reference to the following specific examples, but the present invention is not limited to the following examples. The method is a conventional method unless otherwise specified. The starting materials are commercially available from the open literature unless otherwise specified.
Example 1
Adding 7mmol of ferrous sulfate heptahydrate and 3mmol of manganese chloride tetrahydrate into a mixed solution of 70 ml of water and 10ml of ethanol, and stirring to dissolve to obtain a solution A. 30mmol of ammonium carbonate was added to 70 ml of water and dissolved by stirring to obtain a solution B. And under the condition of stirring at normal temperature, quickly pouring the solution B into the solution A, continuously stirring for 3 hours to obtain the iron-manganese compound precursor dispersion liquid, and standing to obtain brown precipitate. Washing the precipitate, and drying at 60 ℃ to obtain a precursor of the iron-manganese complex for later use. 200mg of iron-manganese complex precursor is added into a solution with the concentration of 0.032M and the volume of 10mLAfter the potassium manganate solution reacts for 12 hours, the solid is centrifugally separated, washed by deionized water and dried at the temperature of 60 ℃ to obtain FeOOH/MnO2Brown solid powder.
Characterization of the nanomaterial: analysis and determination of FeOOH/MnO by X-ray diffractometer2The result is shown by curve 1 in fig. 1.
Scanning electron microscope pictures show that the obtained composite material is a spherical structure with the diameter of about 2 mu m, the surface of the composite material consists of nano particles and is of a porous structure; the results are shown in FIG. 2 (a).
Example 2
The same procedure as in example 1 was followed, except that 5mmol of each of the reactants ferrous sulfate heptahydrate and manganese chloride tetrahydrate was added.
Characterization of the nanomaterial: analysis and determination of Fe by X-ray diffractometer2O3/MnO2The result is shown in fig. 1 as curve 2.
Scanning electron microscope pictures show that the obtained composite material is a spherical structure with the diameter of about 2 mu m, the surface of the composite material consists of nano particles, the surface roughness of the composite material is smaller than that of the product obtained in the embodiment 1, and the composite material is of a porous structure; the results are shown in FIG. 2 (b).
Example 3
The same procedure as in example 1 was followed, except that the reactants ferrous sulfate heptahydrate and manganese chloride tetrahydrate were added in amounts of 3mmol and 7mmol, respectively.
Characterization of the nanomaterial: analysis by X-ray diffractometry showed iron oxide to be amorphous, and the results are shown in curve 3 in fig. 1.
Scanning electron microscope pictures show that the obtained composite material is a spherical structure with the diameter of about 2 mu m, the surface of the composite material consists of nano particles, the surface roughness of the composite material is smaller than that of the product obtained in the example 2, and the composite material is a porous structure; the results are shown in FIG. 2 (c).
Example 4
The iron oxide/manganese dioxide nano composite material absorbs lead ions in water. With lead nitrate (Pb (NO)3)2) Preparing lead ions (Pb) with deionized water2+) Lead ion solutions with the concentration of 10-200mg/L are respectively reserved.
Separately measure Pb with different concentrations of 20mL2+Then 5mg of the iron oxide/manganese dioxide nanocomposite prepared according to any one of examples 1 to 3 were added thereto. After stirring at room temperature for 12h, the mixture was subjected to solid-liquid separation, and the clear solution was collected. Method for detecting Pb in solution by adopting inductively coupled plasma atomic emission spectroscopy2+And (4) concentration. According to the solubility difference of heavy metal ions before and after adsorption, the Pb of each adsorbent can be calculated2+The maximum adsorption amount of (c). The results are shown in Table 1.
Example 5
The iron oxide/manganese dioxide nano composite material adsorbs arsenate ions in water. With sodium arsenate (Na)2HAsO4.12H2O) and deionized water to prepare solutions with the concentration of arsenate ions of 10-200mg/L respectively for later use. The specific adsorption procedure was the same as in example 4.
The results are shown in Table 1.
TABLE 1 adsorption test results of iron oxide/manganese dioxide nanocomposite
Note: in Table 1, iron oxide/manganese dioxide nanocomposites were obtained with the amounts of Fe/Mn species in the reactants of examples 1-3 in ratios of 3/7, 1/1 and 7/3, respectively, as represented by Fe/Mn-3/7, Fe/Mn-1/1 and Fe/Mn-7/3, respectively.
As can be seen from Table 1, the iron oxide/manganese dioxide nanocomposite provided by the invention has excellent removal effects on heavy metal ions, namely lead ions and arsenate ions in water, and can be used as a practical heavy metal ion adsorbent.
Claims (7)
1. The preparation method of the iron oxide/manganese dioxide composite material is characterized by comprising the following steps of:
(1) weighing a certain amount of soluble ferrous salt and divalent manganese salt according to the molar ratio of iron to manganese of 2/8-8/2, adding the soluble ferrous salt and divalent manganese salt into a mixed solution of ethanol and water, and stirring and dissolving to obtain a solution A; the concentration ranges of the ferrous salt and the divalent manganese salt in the solution are both 0.025-0.1 mmol/L; the volume ratio of water to ethanol in the mixed solution of ethanol and water is 7: 1;
(2) adding ammonium carbonate into water, stirring and dissolving to obtain an ammonium carbonate aqueous solution B with the concentration of 0.01-0.1 mol/L;
(3) adding an ammonium carbonate aqueous solution B into the solution A under the stirring condition, continuously stirring for 2-4 h to obtain a ferro-manganese compound precursor dispersion liquid, and standing to obtain a brown precipitate; washing the precipitate, and drying at 60-100 ℃ to obtain a precursor of the iron-manganese compound;
(4) and (4) adding the compound precursor obtained in the step (3) into a potassium permanganate solution to react for 10-20 hours, separating and washing the precipitate, and drying at 60-100 ℃ to obtain a final product.
2. The method according to claim 1, characterized in that the ammonium carbonate aqueous solution B is added to the solution A rapidly over a period of 1 to 10 seconds.
3. The process according to claim 1, characterized in that the molar ratio of ammonium carbonate to the total of iron and manganese in step (3) is 1 (1-4).
4. A process according to claim 3, characterised in that the molar ratio of ammonium carbonate to the sum of iron and manganese in step (3) is 1: 3.
5. The method according to claim 1, characterized in that the concentration of the potassium permanganate solution in step (4) is 0.02 to 0.05 mol/L; 1-300mg of the complex precursor is added into each 10ml of potassium permanganate aqueous solution.
6. A method according to claim 1, characterized in that the molar ratio of iron to manganese is Fe/Mn 7/3, giving a composite structure of FeOOH/MnO2(ii) a The mol ratio of Fe to Mn is 5:5, and the structure of the obtained compound is Fe2O3/MnO2(ii) a When Fe/Mn is 3:7, the ferric oxide is in an amorphous structure.
7. Use of the iron oxide/manganese dioxide composite material prepared by the method of any one of claims 1 to 6, as an adsorbent for adsorbing heavy metal ions in water, including at least one of lead ions, cadmium ions, mercury ions and arsenate ions.
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| CN112387246B (en) * | 2020-11-27 | 2023-02-10 | 宁夏医科大学 | Ferroferric oxide-manganese dioxide/molybdenum sulfide complex and preparation method and application thereof |
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| CN115029139B (en) * | 2022-04-29 | 2023-12-05 | 中南大学 | Heavy metal contaminated soil stabilization medicament and preparation method and application thereof |
| CN115301194A (en) * | 2022-07-22 | 2022-11-08 | 南开大学 | Nano composite material and preparation method and application thereof |
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