CN107512738B - Porous MnFe2O4Nano material and preparation method thereof - Google Patents

Porous MnFe2O4Nano material and preparation method thereof Download PDF

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CN107512738B
CN107512738B CN201610451559.5A CN201610451559A CN107512738B CN 107512738 B CN107512738 B CN 107512738B CN 201610451559 A CN201610451559 A CN 201610451559A CN 107512738 B CN107512738 B CN 107512738B
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杨桂生
计娉婷
朱敏
廖雄兵
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Hefei Genius New Materials Co Ltd
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Abstract

The invention discloses a porous MnFe2O4The nano material is a porous structure material with the aperture of 3-5 microns, which is finally synthesized by taking sodium citrate as a surfactant through a simple solvothermal method to effectively influence the growth speed of crystals in all crystal plane directions, and a synthesized sample shows typical ferromagnetic properties at room temperature. The specific surface area of the material is improved by the porous structure, and the adsorption experiment on Congo red and heavy metal ion CrVI and PbII solution proves that the surface porous structure MnFe2O4The particles can remove pollutants in water more efficiently in the sewage treatment process, and a sample is recovered by a magnetic separation technology so as to be recycled, so that the wastewater purification rate is improved.

Description

Porous MnFe2O4Nano material and preparation method thereof
Technical Field
The invention relates to porous MnFe2O4A nano material and a preparation method thereof, in particular to a solvothermal synthesis method taking sodium citrate as a surfactant.
Background
The sewage discharged from industrial production contains a large amount of organic pollutants and a plurality of heavy metal ions, and most of the organic pollutants exist in the form of water-soluble sodium salts. Because of its stable chemical structure, it does not undergo decomposition reactions with light, water and many chemicals, and therefore, once released into the aqueous environment, the dye is extremely difficult to remove and must be adsorbed before being placed into the receiving stream. Meanwhile, heavy metal ions in the sewage interact with serum proteins in human and animal blood plasma, and metabolism of glucose, fat and protein of organisms is influenced. Therefore, the adsorption effect of the adsorbent is improved to remove organic pollutants and a plurality of heavy metals in the sewageBelongs to one of effective ways of ions. Currently, the adsorbents used are activated carbon, natural organic and inorganic adsorbents and synthetic adsorbents. The adsorption capacity of the wheat bran, the rice bran, the clay and the kaolin to the CR solution is about 10-40 mg/g, and the adsorption capacity to heavy metal ions Cr is about 10-40 mg/g6+Has an adsorption of about 10 to 30mg/g for Pb2+The adsorption of (a) is about 20 to 60 mg/g. Experimentally prepared MnFe2O4The ferrite nano particles have rough surface characteristics, and are favorable for adsorbing various organic solvents, thereby being favorable for solving the problem of sewage treatment. In addition, the particles have stronger ferromagnetism under the action of an external magnetic field, and can be repeatedly used through a simple magnetic separation process. In the magnetic nano-particles, the magnetic particles,
the manganese ferrite is a spinel structure having high magnetic permeability, good electrical conductivity and low loss, and is widely used in many fields. In particular, in the field of sewage treatment, the use of magnetic separation technology to clean wastewater is a relatively new water treatment technology. At present, how to efficiently and deeply remove heavy metal ions in sewage is an urgent problem to be solved, and methods which have been proposed or adopted include chemical precipitation, ion exchange, adsorption, membrane filtration, electrochemical technology, ozone oxidation and the like. Among these techniques, the adsorption method is very flexible in design and operation, and has the effect of producing high-quality water treatment. Due to the reversible property of the adsorption process, the characteristic of high separation efficiency of the magnetic nanoparticles is utilized, toxic components in the wastewater can be detected and separated in a short time, so that the workload is effectively reduced, and a plurality of desorption processes are low in cost, high in efficiency and easy to operate.
Currently available nano metal oxide adsorbents, including nano iron oxides, manganese oxides, zinc oxides, titanium oxides, magnesium oxides and cerium oxides, are listed as promising water systems for heavy metal removal. Besides the traditional nano metal oxide, the magnetic oxide can be separated from water under the action of an external magnetic field due to certain magnetic properties. Therefore, the adsorbent is easily recovered and regenerated in the sewage treatment process. The size, morphology, dispersion and surface properties of magnetic nanoparticles have a large influence on their properties, since the surface of the nanoparticle crystal has different atomic arrangementsColumns and electronic structures, making them different in performance and magnetization capability. Thus, for MnFe2O4The research on the shape control synthesis of the micro/nano particles has important significance. The method synthesizes the MnFe with porous morphology by a simple solvothermal process and controlling the addition of the surfactant2O4Nanocrystals of MnFe2O4For Congo red and heavy metal ions Pb2+、Cr6+The adsorption capacity of the solution further expands the application field of the magnetic material.
Disclosure of Invention
The invention aims to provide porous MnFe prepared by a solvothermal method by using sodium citrate as a surfactant2O4Nanomaterial, porous structure of MnFe2O4Nanocrystals of MnFe2O4For Congo red and heavy metal ions Pb2+、Cr6+The adsorption capacity of the solution further expands the application field of the magnetic material.
The invention relates to porous MnFe2O4The nanometer material has porous structure, pore size of 3-5 microns, and specific surface area of 30-100m2Per g, has ferromagnetism.
The porous MnFe of the invention2O4The preparation method of the nano material comprises the following steps:
dissolving FeSO4 and MnSO4 in ethylene glycol, stirring to form a uniform mixed solution, adding a sodium citrate solution, stirring for 10-40 minutes, transferring the uniform mixed solution into a high-pressure reaction kettle, keeping the temperature of 160-220 ℃ for 15-40 hours, cooling, filtering and separating, washing with ethanol, and drying at room temperature to obtain MnFe with a porous structure2O4A nanocrystal.
In the preparation method, the addition amount of FeSO4 and MnSO4 is 2:1 in molar ratio.
In the preparation method, the addition amount of the ethylene glycol is as follows: 15-50mL of ethylene glycol per 0.1g of FeSO4 was required.
In the preparation method, the addition amount of the sodium citrate is as follows: 0.05-0.4g of sodium citrate is added into every 0.1g of FeSO 4.
Porous MnFe of the invention2O4The nanometer material can be used for azo dyes such as Congo red or heavy metal ions such as Pb2+、Cr6+Adsorption of (3).
The invention provides porous MnFe prepared by a solvothermal method by using sodium citrate as a surfactant2O4Nanomaterial, resulting porous MnFe2O4Nanocrystals of MnFe2O4For Congo red and heavy metal ions Pb2+、Cr6+The adsorption capacity of the solution further expands the application field of the magnetic material.
Drawings
FIG. 1 shows porous MnFe of the present invention2O4And (5) taking a first SEM picture of the nano material.
FIG. 2 shows porous MnFe of the present invention2O4And a second nanometer material SEM picture.
Detailed Description
Example 1:
dissolving 0.231g of FeSO4 and 0.302g of MnSO4 in 70mL of ethylene glycol, stirring to form a uniform mixed solution, adding 0.693g of sodium citrate, stirring for 30 minutes, transferring the uniform mixed solution to a high-pressure reaction kettle, keeping the temperature at 180 ℃ for 30 hours, cooling, filtering and separating, washing with ethanol, and drying at room temperature to obtain MnFe with a porous structure2O4A nanocrystal.
Example 2:
dissolving 0.346g of FeSO4 and 0.453g of MnSO4 in 52mL of ethylene glycol, stirring to form a uniform mixed solution, adding 0.173g of sodium citrate, stirring for 40 minutes, transferring the uniform mixed solution into a high-pressure reaction kettle, keeping the mixture at 160 ℃ for 15 hours, cooling, filtering and separating, washing with ethanol, and drying at room temperature to obtain MnFe with a porous structure2O4A nanocrystal.
Example 3:
dissolving 0.693g of FeSO4 and 0.906g of MnSO4 in 152mL of ethylene glycol, stirring to form a uniform mixed solution, adding 2.77g of sodium citrate, and stirring for 10 minutesTransferring the uniformly mixed solution into a high-pressure reaction kettle after the reaction is finished, keeping the temperature at 220 ℃ for 40 hours, cooling, filtering and separating, washing with ethanol, and drying at room temperature to obtain the porous MnFe2O4A nanocrystal.
Example 4:
dissolving 0.693g of FeSO4 and 0.906g of MnSO4 in 152mL of ethylene glycol, stirring to form a uniform mixed solution, adding 1.584g of sodium citrate, stirring for 10 minutes, transferring the uniform mixed solution to a high-pressure reaction kettle, keeping the temperature at 170 ℃ for 20 hours, cooling, filtering and separating, washing with ethanol, and drying at room temperature to obtain MnFe with a porous structure2O4A nanocrystal.
Example 5
Dissolving 0.346g of FeSO4 and 0.453g of MnSO4 in 52mL of ethylene glycol, stirring to form a uniform mixed solution, adding 0.218g of sodium citrate, stirring for 35 minutes, transferring the uniform mixed solution into a high-pressure reaction kettle, keeping the mixture at 210 ℃ for 35 hours, cooling, filtering and separating, washing with ethanol, and drying at room temperature to obtain MnFe with a porous structure2O4A nanocrystal. Adsorption experiment:
congo red [ CR, chemical formula ═ C32H22N6Na2O6S2Molecular weight of 696.68, lambdamax＝497nm]Is benzidine radical anion azo dye, namely dye with two azo groups. Adding CR into deionized water to prepare CR solutions with different concentrations; separately dissolve Pb (NO)3)2And K2Cr2O7Obtaining Pb2+And Cr6+(1g/L) standard solution. Measuring absorbance of samples with different predetermined concentrations with UV-visible spectrophotometer under conditions of λ max 497, 283.3 and 357.9nm, respectively, and correcting CR and Pb2+And Cr6+And (3) adding an adsorbent into the solution, measuring the equilibrium concentration of the solution after the MnFe2O4 nano-particles are magnetically separated by using atomic absorption spectrometry when the adsorption equilibrium is reached, and calculating the total adsorption amount by using a mass conservation equation. The results are shown in the following table:
Figure BDA0001021722660000031
the experimental results show that the MnFe prepared by the invention2O4For Congo red and heavy metal ions Pb2+、Cr6+Compared with the traditional adsorbing material, the adsorbing capacity of the composite material is obviously excellent.

Claims (4)

1. Porous MnFe2O4The preparation method of the nano material is characterized by comprising the following steps:
FeSO with the molar ratio of 3:44And MnSO4Dissolving in ethylene glycol, stirring to form a uniform mixed solution, adding sodium citrate, stirring for 10-40 min, transferring the uniform mixed solution into a high-pressure reaction kettle, keeping at 160-220 ℃ for 15-40 h, cooling, filtering, separating, washing with ethanol, and drying at room temperature to obtain the porous MnFe2O4Nanocrystals of said MnFe2O4The nano crystal has porous structure, pore diameter of 3-5 μm, and specific surface area of 30-100m2/g。
2. The porous MnFe of claim 12O4The preparation method of the nano material is characterized in that the addition amount of the ethylene glycol is as follows: per 0.1gFeSO415-50mL of ethylene glycol is required.
3. The porous MnFe of claim 12O4The preparation method of the nano material is characterized in that the addition amount of the sodium citrate is as follows: every 0.1g of FeSO4Adding 0.05-0.4g of sodium citrate.
4. Porous MnFe obtained by the production method according to any one of claims 1 to 32O4The application of the nano material in the adsorption of azo dyes or heavy metal ions.
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CN108704611B (en) * 2018-06-11 2021-03-30 华南理工大学 Magnetic ferromanganese oxide loaded mesoporous cellulose biochar composite material and preparation method and application thereof
CN110102246B (en) * 2019-04-28 2021-11-12 华东交通大学 Magnetic layered double-metal hydroxide adsorbent and application thereof in removing phosphorus and chromium
CN112142154B (en) * 2019-06-28 2024-08-06 安徽大学 Method for adsorbing heavy metal lead ions and Congo red dye by using cobalt selenide
CN112062162B (en) * 2020-09-18 2022-11-01 浙江理工大学 MnFe2O4@MoS2Lamellar spherical magnetic composite material and preparation method thereof
CN113769756A (en) * 2021-08-05 2021-12-10 宁波神筹环保设备有限公司 Novel iron-manganese oxide catalyst and application thereof

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CN103223322A (en) * 2013-05-13 2013-07-31 洛阳师范学院 Preparation method of nanosilver and sulfydryl jointly modified magnetic microspheres
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