CN112607785A - MnFe2O4/C nano composite microsphere and preparation method thereof - Google Patents
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Abstract
MnFe2O4The preparation method of the/C nano composite microsphere comprises the steps of preparing MnFe by taking ferric trichloride hexahydrate and manganese chloride tetrahydrate as an iron source and a manganese source, taking hexamethyltetramine as a carbon source, taking ethylene glycol as a solvent and taking sodium citrate as a complexing agent2O4/C nano composite microsphere, and MnFe prepared from the same2O4the/C nano composite microsphere particles are uniform, have good dispersibility, are formed by binding strip clusters, have rough surfaces, can be recycled and regenerated in sewage treatment due to the characteristic of high separation efficiency of the magnetic particles, and are high-performance water treatment adsorbents.
Description
Technical Field
The invention relates to the field of preparation of environmental nano materials, in particular to MnFe2O4a/C nano composite microsphere and a preparation method thereof.
Background
With the development of energy industries such as coal, petroleum and natural gas and traditional light industries such as paper making and printing and dyeing, a large amount of industrial wastewater is generated along with the development of the energy industries such as coal, petroleum and natural gas, and the traditional light industries such as paper making and printing and dyeing, so that how to efficiently and deeply remove heavy metal ions in sewage is a difficult problem to be solved urgently, and proposed or adopted methods comprise 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. The currently available metal oxide adsorbent comprises iron oxide, manganese oxide, zinc oxide, titanium oxide, magnesium oxide, cerium oxide and the like, wherein MnFe2O4 is a ferro-manganese ferrite which has a special physical and chemical structure and a stable crystal structure, and the surface of the ferro-manganese ferrite contains divalent iron and trivalent iron, so that the ferro-manganese bimetallic oxide has the advantages of high stability, strong magnetism, good catalytic performance and the like, and can effectively reduce the workload by detecting and separating toxic components in wastewater in a short time by utilizing the characteristic of high separation efficiency of magnetic particles, and can be recovered and regenerated in the sewage treatment process, so that the ferro-manganese bimetallic oxide is considered to be a high-performance water treatment adsorbent. However, MnFe2O4The particle size, morphology, dispersion and surface characteristics of micro/nanoparticles and their compounding with other materials have a significant impact on their properties. Therefore, based on MnFe2O4The research on the shape control synthesis of the micro/nano particles has important significance.
Disclosure of Invention
In order to solve the technical problems, the invention provides MnFe2O4/C nano composite microspheres and a preparation method thereof, and the method takes ferric trichloride hexahydrate and manganese chloride tetrahydrate as an iron source and a manganese source, hexamethyltetramine as a carbon source and sodium citrate as a complexing agent, and prepares the MnFe2O4/C nano composite microspheres by one-step solvothermal preparation.
In order to achieve the purpose, the technical scheme adopted by the invention is as follows:
MnFe2O4The preparation method of the/C nano composite microsphere comprises the following steps;
dissolving ferric trichloride hexahydrate, manganese chloride tetrahydrate and hexamethyltetramine in a glycol solution, and fully stirring and dissolving to prepare a mixed solution A;
dissolving sodium citrate in a certain amount of glycol solution, fully stirring and dissolving to prepare a solution B;
slowly pouring the solution B into the solution A, and continuously stirring uniformly to obtain a mixed solution C;
step four, transferring the mixed solution C in the step three to a reaction kettle, placing the reaction kettle in a thermostat, reacting for 4-12h at the temperature of 150-;
step five, calcining the reaction primary product in the step four in one step to obtain MnFe2O4the/C nano composite microspheres.
Further, in the first step, the molar mass ratio of ferric trichloride hexahydrate to manganese chloride tetrahydrate is (2.5-1): 1, the mass ratio of the hexamethyltetramine to the ferric trichloride hexahydrate is (8-3): 1.
further, the dosage of the ethylene glycol in the step one is 10ml-40 ml.
Further, the molar mass ratio of the sodium citrate in the step two to the ferric chloride hexahydrate in the step one is 5: 1-1: 1, the dosage of the glycol solution is 10ml-40 ml.
Further, in the second step, the sodium citrate and the glycol solution are fully stirred and dissolved by magnetic force at the temperature of 50-80 ℃ in a water bath.
Further, the mixing time of the mixed solution C in the third step is 30-120 min.
Further, the atmosphere of the calcination in the step five is nitrogen, and the flow rate of the nitrogen is 100-3At the temperature raising rate of 2-20 deg.c/min and the calcining temperature of 350-600 deg.c, and during reactionThe time interval is 60-180 min.
In order to achieve the above purpose, another aspect of the present invention adopts the following technical solutions:
MnFe2O4/C nanocomposite microspheres of said MnFe2O4the/C nano composite microspheres are spherical, and the spheres are formed by binding strip-shaped clusters.
Compared with the prior art, the invention has the following beneficial effects:
1. the invention provides a green synthesis strategy for obtaining high-quality MnFe2O4the/C nano composite microspheres adopt ferric trichloride hexahydrate and manganese chloride tetrahydrate as an iron source and a manganese source, sodium citrate as a complexing agent and hexamethyltetramine as a carbon source, and have the advantages of easily available raw materials, simple, convenient and efficient operation, improved production efficiency of materials, reduced production energy consumption and convenience for large-scale production;
2. MnFe prepared by the invention2O4the/C nano composite microspheres have good monodispersity and uniform size, and consist of strip MnFe2O4The steel has coarse surface, larger specific surface area and pure MnFe2O4The composition of the material and the material C is favorable for increasing the activity of the material and improving the adsorption performance.
Drawings
FIG. 1 shows MnFe obtained in example 1 of the present invention2O4Scanning electron microscope image of/C nano composite microsphere.
FIG. 2 shows MnFe obtained in example 1 of the present invention2O4An electronic energy spectrum of the/C nano composite microsphere.
FIG. 3 shows MnFe obtained in example 2 of the present invention2O4Scanning electron microscope image of/C nano composite microsphere.
FIG. 4 shows MnFe obtained in example 3 of the present invention2O4Scanning electron microscope image of/C nano composite microsphere.
FIG. 5 shows MnFe obtained in example 4 of the present invention2O4Scanning electron microscope image of/C nano composite microsphere.
FIG. 6 shows a graph showing a graph obtained in example 5 of the present inventionMnFe2O4Scanning electron microscope image of/C nano composite microsphere.
Detailed Description
The following describes embodiments of the present invention in detail and completely. The following examples are only used to more clearly illustrate the technical solutions of the present invention, and therefore, only serve as a part of the implementation examples, and the protection scope of the present invention is not limited thereby. Based on the implementation examples in the present invention, other implementation examples obtained by a person of ordinary skill in the art without any creative effort belong to the protection scope of the present invention.
Example one
MnFe2O4The preparation method of the/C nano composite microsphere comprises the following steps:
step one, dissolving 0.4g of ferric trichloride hexahydrate, 0.14g of manganese chloride tetrahydrate and 0.5g of hexamethyltetramine in 20ml of ethylene glycol, and magnetically stirring for 30min to fully dissolve the materials to prepare a solution A;
step two, dissolving 0.5g of sodium citrate in 20ml of ethylene glycol, performing magnetic stirring for 30 minutes at 60 ℃ to fully dissolve the sodium citrate to prepare a solution B;
slowly pouring the solution B into the solution A, and continuously magnetically stirring for 30min to obtain a mixed solution C;
transferring the mixed solution C into a reaction kettle of 80ml, setting the temperature of a constant temperature box to be 180 ℃, keeping the reaction for 12 hours, fully washing the reaction product with water and ethanol, and drying the reaction product in a vacuum drying oven at 60 ℃ for 12 hours to obtain a reaction initial product;
step five, transferring the reaction primary product to a tubular furnace in nitrogen atmosphere at the nitrogen flow rate of 200cm3At a heating rate of 5 ℃/min and a calcination temperature of 450 ℃ for 120min to obtain MnFe2O4/C nanocomposite microspheres, wherein, MnFe2O4The picture of the/C nano composite microsphere scanning electron microscope is shown in figure 1, the corresponding energy spectrum is shown in figure 2, and the MnFe2O4the/C nano composite microspheres are spherical in shape, are formed by binding strip-shaped clusters, and have rough surfaces.
Example two
MnFe2O4The preparation method of the/C nano composite microsphere comprises the following steps:
step one, dissolving 0.4g of ferric trichloride hexahydrate, 0.14g of manganese chloride tetrahydrate and 0.5g of hexamethyltetramine in 20ml of ethylene glycol, and magnetically stirring for 30min to fully dissolve the materials to prepare a solution A;
step two, dissolving 0.5g of sodium citrate in 20ml of ethylene glycol, performing magnetic stirring for 30 minutes at 60 ℃ to fully dissolve the sodium citrate to prepare a solution B;
slowly pouring the solution B into the solution A, and continuously magnetically stirring for 30min to obtain a mixed solution C;
transferring the mixed solution C into a reaction kettle of 80ml, setting the temperature of a constant temperature box to be 160 ℃, keeping the reaction for 12 hours, fully washing the reaction product with water and ethanol, and drying the reaction product in a vacuum drying oven at 60 ℃ for 12 hours to obtain a reaction initial product;
step five, transferring the reaction primary product to a tubular furnace in nitrogen atmosphere at the nitrogen flow rate of 200cm3At a heating rate of 5 ℃/min and a calcination temperature of 450 ℃ for 120min to obtain MnFe2O4/C nanocomposite microspheres, wherein, MnFe2O4The picture of the/C nano composite microsphere scanning electron microscope is shown in figure 3, and the MnFe2O4the/C nano composite microspheres are spherical in shape, are formed by binding strip-shaped clusters, and have rough surfaces.
EXAMPLE III
MnFe2O4The preparation method of the/C nano composite microsphere comprises the following steps:
step one, dissolving 0.2g of ferric trichloride hexahydrate, 0.08g of manganese chloride tetrahydrate and 1g of hexamethyltetramine in 20ml of ethylene glycol, and magnetically stirring for 30min to fully dissolve the materials to prepare a solution A;
step two, dissolving 0.5g of sodium citrate in 20ml of ethylene glycol, performing magnetic stirring for 30 minutes at 60 ℃ to fully dissolve the sodium citrate to prepare a solution B;
slowly pouring the solution B into the solution A, and continuously magnetically stirring for 30min to obtain a mixed solution C;
transferring the mixed solution C into a reaction kettle of 80ml, setting the temperature of a constant temperature box to be 180 ℃, keeping the reaction for 12 hours, fully washing the reaction product with water and ethanol, and drying the reaction product in a vacuum drying oven at 60 ℃ for 12 hours to obtain a reaction initial product;
step five, transferring the reaction primary product to a tubular furnace in nitrogen atmosphere at the nitrogen flow rate of 200cm3At a heating rate of 5 ℃/min and a calcination temperature of 500 ℃ for 120min to obtain MnFe2O4/C nanocomposite microspheres, wherein, MnFe2O4the/C nano composite microsphere scanning electron microscope picture is shown in figure 4, the relative content of the hexamethyltetramine is increased, and a large amount of porous fluffy structures appear on the surface of the composite microsphere.
Example four
MnFe2O4The preparation method of the/C nano composite microsphere comprises the following steps:
step one, dissolving 0.4g of ferric trichloride hexahydrate, 0.14g of manganese chloride tetrahydrate and 0.5g of hexamethyltetramine in 20ml of ethylene glycol, and magnetically stirring for 30min to fully dissolve the materials to prepare a solution A;
step two, dissolving 1g of sodium citrate in 20ml of ethylene glycol, performing magnetic stirring for 30 minutes at 60 ℃ to fully dissolve the sodium citrate to prepare a solution B;
slowly pouring the solution B into the solution A, and continuously magnetically stirring for 30min to obtain a mixed solution C;
transferring the mixed solution C into a reaction kettle of 80ml, setting the temperature of a constant temperature box to be 180 ℃, keeping the reaction for 12 hours, fully washing the reaction product with water and ethanol, and drying the reaction product in a vacuum drying oven at 60 ℃ for 12 hours to obtain a reaction initial product;
step five, transferring the reaction primary product to a tubular furnace in nitrogen atmosphere at the nitrogen flow rate of 200cm3At a heating rate of 5 ℃/min and a calcination temperature of 450 ℃ for 180min, thus obtaining MnFe2O4/C nanocomposite microspheres, wherein, MnFe2O4The picture of the/C nano composite microsphere scanning electron microscope is shown in figure 5, and the MnFe2O4the/C nano composite microspheres are spherical and are clustered by strip-shaped clustersBinding formation and rough surface.
EXAMPLE five
MnFe2O4The preparation method of the/C nano composite microsphere comprises the following steps:
step one, dissolving 0.4g of ferric trichloride hexahydrate, 0.14g of manganese chloride tetrahydrate and 0.5g of hexamethyltetramine in 20ml of ethylene glycol, and magnetically stirring for 30min to fully dissolve the materials to prepare a solution A;
step two, dissolving 0.5g of sodium citrate in 20ml of ethylene glycol, performing magnetic stirring for 30 minutes at 60 ℃ to fully dissolve the sodium citrate to prepare a solution B;
slowly pouring the solution B into the solution A, and continuously magnetically stirring for 30min to obtain a mixed solution C;
transferring the mixed solution C into a reaction kettle of 80ml, setting the temperature of a constant temperature box to be 170 ℃, keeping the reaction for 12 hours, fully washing the reaction product with water and ethanol, and drying the reaction product in a vacuum drying oven at 60 ℃ for 12 hours to obtain a reaction initial product;
step five, transferring the reaction primary product to a tubular furnace in nitrogen atmosphere at the nitrogen flow rate of 200cm3At a heating rate of 5 ℃/min and a calcination temperature of 450 ℃ for 120min to obtain MnFe2O4/C nanocomposite microspheres, wherein, MnFe2O4The picture of the/C nano composite microsphere scanning electron microscope is shown in figure 6, and the MnFe2O4the/C nano composite microspheres are spherical in shape, are formed by binding strip-shaped clusters, and have rough surfaces.
EXAMPLE six
MnFe2O4The preparation method of the/C nano composite microsphere comprises the following steps:
step one, dissolving 0.4g of ferric trichloride hexahydrate, 0.14g of manganese chloride tetrahydrate and 0.1g of hexamethyltetramine in 20ml of ethylene glycol, and magnetically stirring for 30min to fully dissolve the materials to prepare a solution A;
step two, dissolving 0.5g of sodium citrate in 20ml of ethylene glycol, performing magnetic stirring for 30 minutes at 60 ℃ to fully dissolve the sodium citrate to prepare a solution B;
slowly pouring the solution B into the solution A, and continuously magnetically stirring for 30min to obtain a mixed solution C;
transferring the mixed solution C into a reaction kettle of 80ml, setting the temperature of a constant temperature box to be 180 ℃, keeping the reaction for 6 hours, fully washing the reaction product with water and ethanol, and drying the reaction product in a vacuum drying oven at 60 ℃ for 12 hours to obtain a reaction initial product;
step five, transferring the reaction primary product to a tubular furnace in nitrogen atmosphere at the nitrogen flow rate of 200cm3At a heating rate of 5 ℃/min and a calcination temperature of 600 ℃ for 120min to obtain MnFe2O4/C nanocomposite microspheres, wherein the MnFe2O4the/C nano composite microspheres are spherical in shape, are formed by binding strip-shaped clusters, and have rough surfaces.
EXAMPLE seven
MnFe2O4The preparation method of the/C nano composite microsphere comprises the following steps:
step one, dissolving 0.4g of ferric trichloride hexahydrate, 0.14g of manganese chloride tetrahydrate and 0.5g of hexamethyltetramine in 40ml of ethylene glycol, and magnetically stirring for 30min to fully dissolve the materials to prepare a solution A;
step two, dissolving 0.5g of sodium citrate in 20ml of ethylene glycol, performing magnetic stirring for 30 minutes at 60 ℃ to fully dissolve the sodium citrate to prepare a solution B;
slowly pouring the solution B into the solution A, and continuously magnetically stirring for 30min to obtain a mixed solution C;
transferring the mixed solution C into a reaction kettle of 80ml, setting the temperature of a constant temperature box to be 180 ℃, keeping the reaction for 12 hours, fully washing the reaction product with water and ethanol, and drying the reaction product in a vacuum drying oven at 60 ℃ for 12 hours to obtain a reaction initial product;
step five, transferring the reaction primary product to a tubular furnace in nitrogen atmosphere at the nitrogen flow rate of 200cm3At a heating rate of 5 ℃/min and a calcination temperature of 450 ℃ for 120min to obtain MnFe2O4/C nanocomposite microspheres, wherein the MnFe2O4the/C nano composite microspheres are spherical in shape, are formed by binding strip-shaped clusters, and have rough surfaces.
Example eight
As shown in figure 1, the MnFe2O4/C nano-composite microspheres are spherical, are formed by binding strip-shaped clusters, and have rough surfaces.
The above-mentioned embodiments are only used for illustrating the technical solutions of the present invention, and not for limiting the same; although the present invention has been described in detail with reference to the foregoing embodiments, it will be understood by those skilled in the art that various changes in form and details may be made therein without departing from the spirit and scope of the invention; and such modifications or substitutions do not depart from the spirit and scope of the corresponding technical solutions of the embodiments of the present invention.
Claims (8)
1. MnFe2O4The preparation method of the/C nano composite microspheres is characterized by comprising the following steps: comprises the following steps;
dissolving ferric trichloride hexahydrate, manganese chloride tetrahydrate and hexamethyltetramine in a glycol solution, and fully stirring and dissolving to prepare a mixed solution A;
dissolving sodium citrate in a certain amount of glycol solution, fully stirring and dissolving to prepare a solution B;
slowly pouring the solution B into the solution A, and continuously stirring uniformly to obtain a mixed solution C;
step four, transferring the mixed solution C in the step three to a reaction kettle, placing the reaction kettle in a thermostat, reacting for 4-12h at the temperature of 150-;
step five, calcining the reaction primary product in the step four in one step to obtain MnFe2O4the/C nano composite microspheres.
2. MnFe of claim 12O4The preparation method of the/C nano composite microspheres is characterized by comprising the following steps: in the first step, the molar mass ratio of ferric trichloride hexahydrate to manganese chloride tetrahydrate is (2.5-1): substances of 1, hexamethyltetramine and ferric trichloride hexahydrateThe quantity ratio is (8-3): 1.
3. MnFe of claim 12O4The preparation method of the/C nano composite microspheres is characterized by comprising the following steps: the dosage of the ethylene glycol in the step one is 10ml-40 ml.
4. MnFe of claim 12O4The preparation method of the/C nano composite microspheres is characterized by comprising the following steps: the molar mass ratio of the sodium citrate in the step two to the ferric trichloride hexahydrate in the step one is 5: 1-1: 1, the dosage of the glycol solution is 10ml-40 ml.
5. MnFe of claim 12O4The preparation method of the/C nano composite microspheres is characterized by comprising the following steps: and in the second step, the sodium citrate and the glycol solution are fully stirred and dissolved by magnetic force at the temperature of 50-80 ℃ in water bath.
6. MnFe of claim 12O4The preparation method of the/C nano composite microspheres is characterized by comprising the following steps: and the mixing solution C in the third step is stirred for 30-120 min.
7. MnFe of claim 12O4The preparation method of the/C nano composite microspheres is characterized by comprising the following steps: the atmosphere of the calcination in the step five is nitrogen, and the flow rate of the nitrogen is 100-3The temperature rise rate is 2-20 ℃/min, the calcination temperature is 350-.
8. MnFe prepared according to any one of claims 1 to 72O4the/C nano composite microsphere is characterized in that: the MnFe2O4the/C nano composite microspheres are spherical, and the spheres are formed by binding strip-shaped clusters.
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| CN113511732A (en) * | 2021-04-09 | 2021-10-19 | 安徽中科索纳新材料科技有限公司 | Capacitive deionization selective adsorption electrode, capacitive deionization device and application |
| 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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