CN104671287A - Environment-friendly preparation method of nano manganese oxide composite material - Google Patents
Environment-friendly preparation method of nano manganese oxide composite material Download PDFInfo
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- CN104671287A CN104671287A CN201510038984.7A CN201510038984A CN104671287A CN 104671287 A CN104671287 A CN 104671287A CN 201510038984 A CN201510038984 A CN 201510038984A CN 104671287 A CN104671287 A CN 104671287A
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- manganese oxide
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Abstract
The invention discloses an environment-friendly preparation method of a nano manganese oxide composite material. The environment-friendly preparation method comprises the following steps: (1) dissolving a certain amount of potassium permanganate into deionized water; (2) dispersing nano-conducting materials into a mixed solution of water and an organic solvent, and adding acid or alkali to regulate the pH value; (3) mixing the two solutions at a stirring or ultrasonic condition; and (4) drying to obtain manganese oxide composite powder after reaction for a period of time at a certain temperature. The prepared nano manganese oxide composite material has the characteristics that the particle size distribution is uniform, the shapes of products are regular and various, and the particle size is easily controlled. The preparation method has the beneficial effects that the preparation speed is high, the technological process is simple, the operation is convenient, the controllability is strong, the cost is low, the environmental pollution is avoided, and the application value is extremely high.
Description
Technical field
The present invention relates to a kind of environment-friendly preparation method thereof of nano manganese oxide matrix material, specifically relate to the technology that a kind of organic mixed solvent fast restore potassium permanganate prepares manganese oxide, belong to technical field of nanometer material preparation.
Background technology
The basic structural unit of manganese oxide nanometer material is manganese oxygen octahedra, and manganese oxygen octahedra basic structural unit is by limit or corner-sharing mode grow the manganese oxide nanometer material defining and have tunnel or laminate structure in a certain direction altogether.Usually, manganese oxide material exists with multiple crystal formation, and common crystal formation has α, β, γ, δ type, also has ε, ρ type.When manganese oxygen octahedra basic structural unit forms tunnel structure with different number and mode by corner-sharing, just generate α and the β crystal configuration of different pore passage structure, the tunnel structure of its different size makes such material have ion(ic)sieve and molecular sieve function.Result of study shows, the factor such as crystal formation, size, pattern, dimension of nanoparticle affects the performance such as optics, electricity, magnetics of nano material in various degree, and thus the controlledly synthesis of different crystal forms and pattern manganese oxide nanometer material is one of Important Problems of paying close attention to of investigator always.
Manganese oxide resource is extensive, cheap, environment is friendly, have multiple oxidation state.The manganese oxide nanometer material of different-shape and structure has many special physics and chemistry character such as ion(ic)sieve, molecular sieve, catalysis and electrochemistry, thus shows wide application prospect in the field such as positive electrode material and novel magnetic materials of sorbing material, catalytic material, ultracapacitor, lithium-ion secondary cell.In manganese oxide, manganese element has high Oxidation Number (Mn
3+, Mn
4+), high surface oxygen concentration and be present in the great amount of hydroxy group on manganese and oxygen compound surface, makes it also be used widely at catalytic field.Porousness manganese oxide has good ion-exchange and molecular adsorption performance, makes it be used as ion(ic)sieve or molecular sieve.If the manganese oxide of spinel type is to the Li in seawater and dilute solution
+there is excellent selective adsorption effect.Manganese oxide material has good electrochemical properties, is the most potential anode material for lithium secondary battery, and studying more manganese oxidate for lithium has spinel LiMn
2o
4with stratiform LiMnO
2two kinds of structures.Manganese oxide is a kind of cheap and respond well novel capacitor material equally, there is high specific surface area and unformed structure can make manganese oxide lattice dilation, proton is easy to remain in the inside, show higher capacitive character, and the micron order manganese oxide of the crystalline structure that the usual precipitator method obtain do not have these features.
Hydrothermal method, solvent-thermal method, template and vapour deposition etc. are the conventional methods preparing manganese oxide nanometer material, investigator has prepared the manganese oxide nanometer material of a large amount of different crystal forms and pattern by these methods, but most of method complex process, output are little, are difficult to realize industrialization and produce.Potassium permanganate comprises septivalency manganese, has extremely strong oxidisability, but usually adopts long hydrothermal decomposition to prepare manganese oxide at present, or adopts carbon material reduction potassium permanganate, and reduction rate is difficult to realize volume production extremely slowly.We have proposed and adopt organic solvent to carry out fast restore to potassium permanganate, the method has the advantage that raw material sources are extensive, technical process simple, product specific surface area is large, size-grade distribution good, foreign matter content is low, with low cost.
Summary of the invention
The object of the present invention is to provide a kind of environment-friendly preparation method thereof of nano manganese oxide matrix material, the method mainly utilizes reductibility organic solvent to carry out reduction treatment to potassium permanganate, prepared manganese oxide shape has flower-shaped, accordion, spherical etc., nanoparticle size distribution is concentrated, size adjustable (10nm ~ 1000nm), quality product be high, is a kind of simple and easy, low cost, high-level efficiency, prepares the excellent process of nano manganese oxide in enormous quantities.
Technical scheme: above-mentioned purpose of the present invention is achieved by following technical solution, a kind of environment-friendly preparation method thereof of nano manganese oxide matrix material, the method concrete steps are as follows:
Step one: a certain amount of potassium permanganate is dissolved in deionized water;
Step 2: be dispersed in by nanometer conductive material in the mixing solutions of water and organic solvent, adds acid or alkali adjust ph;
Step 3: above-mentioned two kinds of solution are mixed under stirring or ultrasound condition;
Step 4: after reacting for some time at a certain temperature, be dried to manganese oxide composite powder.
Wherein, in above-mentioned steps one, described potassium permanganate and organic solvent mol ratio are 1:0.1 ~ 100, and preferred ratio is 1:1 ~ 10.;
Wherein, in above-mentioned steps two, described nanometer conductive material is one or more mixing in Graphene, carbon nanotube, acetylene black, carbon black, carbon microspheres, nanometer gold, nanometer silver, Platinum Nanoparticles, Nanometer Copper, nano aluminum, nano nickel, preferably Graphene, carbon nanotube, acetylene black and carbon black.
Wherein, in above-mentioned steps two, described organic solvent is one or more mixing in methyl alcohol, ethanol, n-propyl alcohol, Virahol, ethylene glycol, propylene glycol, glycerol.The preferably mixture of methyl alcohol, ethanol, Virahol and water.
Wherein, in above-mentioned steps two, the ratio of described organic solvent in mixed solvent is 10% ~ 90%.
Wherein, in above-mentioned steps two, described alkali is one or more mixing in sodium hydroxide, potassium hydroxide, calcium hydroxide, hydrated barta, lithium hydroxide, ammoniacal liquor, organic bases, and preferred alkaline conditioner is sodium hydroxide, potassium hydroxide and ammoniacal liquor.
Wherein, in above-mentioned steps two, described acid is one or more mixing in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, perchloric acid, Hydrogen bromide, hydrofluoric acid, sulfurous acid, acetic acid, preferably hydrochloric acid, sulfuric acid and nitric acid.
Wherein, in above-mentioned steps four, described temperature of reaction is below mixed solvent vaporization temperature, and preferred temperature of reaction is 20 degrees Celsius to 50 degrees Celsius.
Wherein, in above-mentioned steps four, the described reaction times is 5 minutes-30 hours, and the preferred reaction times is 5 minutes ~ 3 hours.
The invention has the beneficial effects as follows:
Nano oxidized manganese material prepared by present method, efficient fast, technique is simple, easy and simple to handle, with low cost, short without the need to accurate Controlling Technology parameter, preparation time, do not pollute, easily expand scale, suitability for industrialized production can be realized fast.
Accompanying drawing explanation
Fig. 1 is the transmission electron microscope photo of flower-shaped manganese oxide prepared by embodiment 1.
Fig. 2 is the stereoscan photograph of flower-shaped manganese oxide prepared by embodiment 1.
Fig. 3 is the stereoscan photograph of fold manganese oxide prepared by embodiment 2.
Fig. 4 is the stereoscan photograph of spherical manganese oxide prepared by embodiment 3.
Fig. 5 is the transmission electron microscope photo of manganese oxide/graphene composite material prepared by embodiment 4.
Fig. 6 is the stereoscan photograph of manganese oxide/graphene composite material prepared by embodiment 4.
Fig. 7 is the transmission electron microscope photo of manganese oxide/carbon nano tube compound material prepared by embodiment 5.
Fig. 8 is the transmission electron microscope photo of manganese oxide/acetylene black matrix material prepared by embodiment 6.
Fig. 9 is FB(flow block) of the present invention.
Embodiment
See Fig. 1-9, below in conjunction with embodiment, the present invention will be further described.
Embodiment 1, with in the mixed solvent of 50% volume ratio Virahol and water, does not add electro-conductive material, not adjust ph, utilizes present method to prepare nano manganese oxide for embodiment:
Step one: 500 milligrams of potassium permanganate are dissolved in the deionized water of 40ml;
Step 2: 250 milliliters of Virahols are added 250 ml deionized water mixings;
Step 3: under 300 turns of per minute stirring velocitys, is slowly added drop-wise to potassium permanganate solution in mixed organic solvents;
Step 4: after reacting about 1 hour at normal temperatures, adopt organic filter membrane suction filtration of 0.45 micron pore size, repetitive scrubbing 3 times, prepares nano manganese oxide powder after drying.
As shown in Figure 1, stereoscan photograph as shown in Figure 2 for the nano flower-like manganese oxide transmission electron microscope photo obtained.
Embodiment 2, with in the mixed solvent of 30% volume ratio ethanol and water, does not add electro-conductive material, pH about 1, utilizes present method to prepare nano manganese oxide for embodiment:
Step one: 300 milligrams of potassium permanganate are dissolved in the deionized water of 30ml;
Step 2: 150 milliliters of ethanol are added 350 ml deionized water mixings;
Step 3: under 500 turns of per minute stirring velocitys, drips hydrochloric acid soln and pH value is adjusted to 1, be then slowly added drop-wise in mixed organic solvents by potassium permanganate solution;
Step 4: after reacting about 1 hour at normal temperatures, adopt organic filter membrane suction filtration of 0.45 micron pore size, repetitive scrubbing 3 times, prepares nano manganese oxide powder after drying.
The fold manganese oxide stereoscan photograph obtained as shown in Figure 3.
Embodiment 3, with in the mixed solvent of 60% vol/vol methanol and water, does not add electro-conductive material, pH about 13, utilizes present method to prepare nano manganese oxide for embodiment:
Step one: 400 milligrams of potassium permanganate are dissolved in the deionized water of 30ml;
Step 2: 300 ml methanol are added 200 ml deionized water mixings;
Step 3: under 600 turns of per minute stirring velocitys, drip sodium hydroxide solution and pH value is adjusted to 13, then potassium permanganate solution is slowly added drop-wise in mixed organic solvents;
Step 4: after reacting about 0.5 hour at normal temperatures, adopt organic filter membrane suction filtration of 0.45 micron pore size, repetitive scrubbing 3 times, prepares nano manganese oxide powder after drying.
The spherical manganese oxide stereoscan photograph obtained as shown in Figure 4.
Embodiment 4, with in the mixed solvent of 50% volume ratio Virahol and water, interpolation Graphene is electro-conductive material, utilizes present method to prepare nano manganese oxide/graphene composite material for embodiment:
Step one: 400 milligrams of potassium permanganate are dissolved in the deionized water of 30ml;
Step 2: 250 milliliters of Virahols are added 250 ml deionized water mixings, add about 20 milligrams of Graphene powder, ultrasonic about 10 hours;
Step 3: under 600 turns of per minute stirring velocitys, is slowly added drop-wise to potassium permanganate solution in mixed organic solvents;
Step 4: after reacting about 1 hour at normal temperatures, adopts organic filter membrane suction filtration of 0.45 micron pore size, repetitive scrubbing 3 times, prepares nano manganese oxide/Graphene composite powder after drying.
As shown in Figure 5, stereoscan photograph as shown in Figure 6 for the nano manganese oxide/Graphene composite powder transmission electron microscope photo obtained.
Embodiment 5, with in the mixed solvent of 50% vol/vol methanol and water, temperature of reaction 40 degrees Celsius, interpolation carbon nanotube is electro-conductive material, utilizes present method to prepare nano manganese oxide/carbon nano tube compound material for embodiment:
Step one: 300 milligrams of potassium permanganate are dissolved in the deionized water of 30ml;
Step 2: 250 milliliters of ethanol are added 250 ml deionized water mixings, add about 10 milligrams of multi-walled carbon nano-tubes powder, ultrasonic about 10 hours;
Step 3: under 500 turns of per minute stirring velocitys, is slowly added drop-wise to potassium permanganate solution in mixed organic solvents;
Step 4: react about 0.5 hour under 40 degree after, adopts organic filter membrane suction filtration of 0.45 micron pore size, repetitive scrubbing 3 times, prepares nano manganese oxide/carbon nano-tube composite powder end after drying.
The nano manganese oxide obtained/carbon nano-tube composite powder end stereoscan photograph as shown in Figure 7.
Embodiment 6, with in the mixed solvent of 40% volume ratio ethanol and water, interpolation acetylene black is electro-conductive material, temperature of reaction about 50 degree, and utilizing present method to prepare nano manganese oxide/acetylene black matrix material is embodiment:
Step one: 300 milligrams of potassium permanganate are dissolved in the deionized water of 30ml;
Step 2: 200 milliliters of ethanol are added 300 ml deionized water mixings, add about 20 milligrams of acetylene black powder, ultrasonic about 5 hours;
Step 3: under 300 turns of per minute stirring velocitys, is slowly added drop-wise to potassium permanganate solution in mixed organic solvents;
Step 4: react about 0.5 hour under 50 degree after, adopts organic filter membrane suction filtration of 0.45 micron pore size, repetitive scrubbing 3 times, prepares nano manganese oxide/acetylene black composite powder after drying.
Nano manganese oxide/acetylene black composite powder the stereoscan photograph obtained as shown in Figure 8.
Obviously, above-mentioned case study on implementation of the present invention is only used to clearly demonstrate example of the present invention, and the restriction not to embodiments of the present invention.For the those of ordinary skill in described field, other multi-form change or variations can also be made on the basis of the above description.Here cannot give exhaustive to all embodiments, every belong to technical scheme of the present invention the apparent change of amplifying out or variation be still in the row of protection scope of the present invention.
Claims (9)
1. an environment-friendly preparation method thereof for nano manganese oxide matrix material, is characterized in that: the method concrete steps are as follows:
Step one: a certain amount of potassium permanganate is dissolved in deionized water;
Step 2: be dispersed in by nanometer conductive material in the mixing solutions of water and organic solvent, adds acid or alkali adjust ph;
Step 3: above-mentioned two kinds of solution are mixed under stirring or ultrasound condition;
Step 4: after reacting for some time at a certain temperature, be dried to manganese oxide composite powder.
2. the environment-friendly preparation method thereof of a kind of nano manganese oxide matrix material according to claim 1, is characterized in that: in step one, and described potassium permanganate and organic solvent mol ratio are 1:0.1 ~ 100, and preferred ratio is 1:1 ~ 10.
3. the environment-friendly preparation method thereof of a kind of nano manganese oxide matrix material according to claim 1, it is characterized in that: in step 2, described nanometer conductive material is one or more mixing in Graphene, carbon nanotube, acetylene black, carbon black, carbon microspheres, nanometer gold, nanometer silver, Platinum Nanoparticles, Nanometer Copper, nano aluminum, nano nickel, preferably Graphene, carbon nanotube, acetylene black and carbon black.
4. the environment-friendly preparation method thereof of a kind of nano manganese oxide matrix material according to claim 1, it is characterized in that: in step 2, described organic solvent is one or more mixing in methyl alcohol, ethanol, n-propyl alcohol, Virahol, ethylene glycol, propylene glycol, glycerol, the preferably mixture of methyl alcohol, ethanol, Virahol and water.
5. the environment-friendly preparation method thereof of a kind of nano manganese oxide matrix material according to claim 1, is characterized in that: in step 2, and the ratio of described organic solvent in mixed solvent is 10% ~ 90%.
6. the environment-friendly preparation method thereof of a kind of nano manganese oxide matrix material according to claim 1, it is characterized in that: in step 2, described alkali is one or more mixing in sodium hydroxide, potassium hydroxide, calcium hydroxide, hydrated barta, lithium hydroxide, ammoniacal liquor, organic bases, and preferred alkaline conditioner is sodium hydroxide, potassium hydroxide and ammoniacal liquor.
7. the environment-friendly preparation method thereof of a kind of nano manganese oxide matrix material according to claim 1, it is characterized in that: in step 2, described acid is one or more mixing in hydrochloric acid, sulfuric acid, nitric acid, phosphoric acid, perchloric acid, Hydrogen bromide, hydrofluoric acid, sulfurous acid, acetic acid, preferably hydrochloric acid, sulfuric acid and nitric acid.
8. the environment-friendly preparation method thereof of a kind of nano manganese oxide matrix material according to claim 1, is characterized in that: in step 4, and described temperature of reaction is below mixed solvent vaporization temperature, and preferred temperature of reaction is 20 degrees Celsius to 50 degrees Celsius.
9. the environment-friendly preparation method thereof of a kind of nano manganese oxide matrix material according to claim 1, is characterized in that: in step 4, and the described reaction times is 5 minutes-30 hours, and the preferred reaction times is 5 minutes ~ 3 hours.
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| CN105481018A (en) * | 2016-01-14 | 2016-04-13 | 上海大学 | Structurally-adjustable 3D network-structured mesoporous manganese dioxide and preparation method thereof |
| CN105854802A (en) * | 2016-05-17 | 2016-08-17 | 遵义师范学院 | Cadmium-containing sewage treatment nano-composite material and preparing method thereof |
| CN106442687A (en) * | 2016-09-21 | 2017-02-22 | 许昌学院 | Modified electrode, as well as preparation method and application thereof to pigment detection |
| CN107265504A (en) * | 2017-05-27 | 2017-10-20 | 安徽师范大学 | One-dimensional MnO2Nanotube and its preparation method and application |
| CN114823167A (en) * | 2022-03-18 | 2022-07-29 | 电子科技大学 | Rapid preparation C @ MnO 2 Method and application of nanoparticles |
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Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105481018A (en) * | 2016-01-14 | 2016-04-13 | 上海大学 | Structurally-adjustable 3D network-structured mesoporous manganese dioxide and preparation method thereof |
| CN105481018B (en) * | 2016-01-14 | 2018-04-06 | 上海大学 | Adjustable 3D network structures meso-porous titanium dioxide manganese of structure and preparation method thereof |
| CN105854802A (en) * | 2016-05-17 | 2016-08-17 | 遵义师范学院 | Cadmium-containing sewage treatment nano-composite material and preparing method thereof |
| CN106442687A (en) * | 2016-09-21 | 2017-02-22 | 许昌学院 | Modified electrode, as well as preparation method and application thereof to pigment detection |
| CN107265504A (en) * | 2017-05-27 | 2017-10-20 | 安徽师范大学 | One-dimensional MnO2Nanotube and its preparation method and application |
| CN107265504B (en) * | 2017-05-27 | 2019-04-16 | 安徽师范大学 | One-dimensional MnO2Nanotube and its preparation method and application |
| CN114823167A (en) * | 2022-03-18 | 2022-07-29 | 电子科技大学 | Rapid preparation C @ MnO 2 Method and application of nanoparticles |
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