CN101798118A - Preparation method of manganese dioxide one-dimensional nanomaterial - Google Patents
Preparation method of manganese dioxide one-dimensional nanomaterial Download PDFInfo
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Abstract
The invention discloses a preparation method of manganese dioxide one-dimensional nanomaterial. The method comprises the following steps: 1. dissolving potassium permanganate in distilled water or deionized water, stirring to obtain a purple-red solution, wherein the concentration is 0.05mol/L-2.0mol/L; 2. dissolving manganese acetate in distilled water or deionized water, stirring to obtain a colorless and transparent solution, wherein the concentration is 0.05mol/L-3.0mol/L; 3. mixing and stirring the solution A and B obtained in the step 1 and 2, transferring the obtained solution in a stainless steel hydrothermal reaction tank with a polytetrafluoroethylene lining, reacting at 50-200 DEG C for 1-36h; and 4. after the reaction, performing natural cooling, and filtering, washing and drying the precipitate in turn to obtain the manganese dioxide one-dimensional nanomaterial. The method has the advantages that the process is simple, the raw materials are accessible, the cost is low, the pollution is low and is easy to perform purification treatment, the method is suitable for industrialization, etc.
Description
Technical field
The present invention relates to a kind of preparation method of manganese dioxide one-dimensional nano material, relate in particular to a kind of simple and convenient process for preparing that is used for the manganese dioxide one-dimensional nano material of ultracapacitor.
Background technology
At present, the electrode for super capacitor material mainly is divided three classes: carbon material, metal oxide and conductive polymers.Wherein, metal oxide ruthenium oxide hydration RuO
2H
2O has very big than electric capacity, but its expensive cost and to the pollution of environment has limited its large-scale commercial production.And MnO
2The people's attention extremely with characteristics such as its resource is extensive, cheap, environment is friendly, electrochemical window broad is candidate's electrode materials that the development ultracapacitor has potentiality.A lot of preparation methods about nano-manganese dioxide are arranged now, such as: sol-gel method, solid phase method, liquid phase oxidation, chemical precipitation method, hydrothermal method etc.Hydrothermal method is with its mild condition, controllability is good, the output advantages of higher becomes nano-manganese dioxide main synthetic method.To the nanometer research of manganese bioxide electrode material, improved the capacitive property of material greatly.Chinese patent CN101597086A has announced a kind of method for preparing the different crystal forms nano-manganese dioxide, and adopting potassium permanganate and acid solution is raw material, under the low temperature, has prepared the δ type nano-manganese dioxide or the α type nano-manganese dioxide of single crystal form.Chinese patent CN101585555A has announced a kind of method for preparing monolayer manganese dioxide nano-plates, at first manganous nitrate is generated the NaxMnO2 of preface laminate structure with the highly basic reaction in the presence of oxygenant, again it is joined in the strong base solution, obtain HxMnO2 by hydrothermal method, generate monolayer manganese dioxide nano-plates with the TBAH reaction then.
Summary of the invention
The technical problem to be solved in the present invention provides that a kind of technology is simple, raw material is easy to get, cost is low, pollution is little and is easy to purifying treatment, is easy to advantage such as industrialization, belongs to the preparation method of eco-friendly manganese dioxide one-dimensional nano material.
For solving the problems of the technologies described above, the inventive method may further comprise the steps: a kind of preparation method of manganese dioxide one-dimensional nano material, step is: 1. potassium permanganate is dissolved in distilled water or the deionized water, stirs and obtain purplish red solution, its concentration is 0.05mol/L~2.0mol/L; 2. manganese acetate is dissolved in distilled water or the deionized water, stir colourless transparent solution, its concentration is 0.05mol/L~3.0mol/L; 3. 1. and change over to behind the A 2., B solution mixing and stirring and have in the teflon-lined stainless steel hydrothermal reaction kettle, 50 ℃~200 ℃ reactions 1~36 hour down with step; 4. naturally cooling after 3. step is reacted and finished, with throw out after filtration, after the washing, drying manganese dioxide one-dimensional nano material.
Further: in the preparation method of above-mentioned manganese dioxide one-dimensional nano material, described step 3. in, it is that molar ratio according to potassium permanganate and manganese acetate is to carry out in 2: 3~2: 3.2 that A and B solution mix.The concrete wash conditions of described step in 4. is that reaction product is dispersed in distilled water or the deionized water, adopts the mode of decompress filter or centrifugation, and repetitive scrubbing 3~4 times is till washing lotion pH neutrality.The drying conditions of step in 4. be, drying temperature is 50 ℃~120 ℃, and be 6 hours~24 hours time of drying, adopts normal pressure or Minton dryer to carry out.
The present invention has the following advantages compared to existing technology:
Potassium permanganate solution provided by the invention and manganese acetate aqueous feed solution are easy to get, cost is low, and do not produce harmful, toxic chemical substance in the preparation process, pollute little and are easy to purifying treatment.Change over to after A, the B solution mixing and stirring and have in the teflon-lined stainless steel hydrothermal reaction kettle, 50 ℃~200 ℃ reactions 1~36 hour down; The back naturally cooling is finished in reaction, with throw out after filtration, must manganese dioxide one-dimensional nano material after the washing, drying.So be easy to produce in batches manganese dioxide one-dimensional nano material.
Description of drawings:
Fig. 1 is the XRD spectra of the manganese dioxide one-dimensional nano material of embodiment 1 preparation;
Fig. 2 is that embodiment 2 prepared materials are as the cyclic voltammetry curve figure of ultracapacitor in the sodium sulfate electrolyte solution;
Fig. 3 is the prepared MnO that goes out of embodiment 1
2The scanning electron microscope image of monodimension nanometer material;
Fig. 4 is the prepared MnO that goes out of embodiment 2
2The scanning electron microscope image of monodimension nanometer material;
Fig. 5 is the prepared MnO that goes out of embodiment 3
2The scanning electron microscope image of monodimension nanometer material;
Fig. 6 is the prepared MnO that goes out of embodiment 4
2The scanning electron microscope image of monodimension nanometer material;
Fig. 7 is the prepared MnO that goes out of embodiment 5
2The scanning electron microscope image of monodimension nanometer material;
Fig. 8 is the prepared MnO that goes out of embodiment 6
2The scanning electron microscope image of monodimension nanometer material;
Embodiment
Purport of the present invention be select for use be simple and easy to the potassium permanganate solution and the manganese acetate aqueous solution in thermal and hydric environment, react and make manganese dioxide one-dimensional nano material, in operating process, do not produce harmful, toxic chemical substance, pollute little and be easy to purifying treatment, technology is controlled easily, and is not dangerous.Below in conjunction with embodiment content of the present invention is described in further detail, mentioned content is not a limitation of the invention among the embodiment, and the time in the method and the selection of temperature can be suited measures to local conditions and the result be there is no substantial effect.
In 100 ml beakers, add 30 ml distilled waters or deionized water, with the 2 mmole potassium permanganate solution a that obtains soluble in water.In 100 ml beakers, add 20 ml distilled waters or deionized water in addition, with the 3 mmole manganese acetates solution b that obtains soluble in water.It is 100 milliliters containing in the teflon-lined stainless steel hydrothermal reaction kettle that solution a and solution b are mixed, stir, change over to volume, and with the still sealing, the thermostat container of putting into 100 ℃ reacted 12 hours.Behind the product naturally cooling, adopting the filtering and washing mode, is neutral with distilled water or deionized water and absolute ethanol washing to pH, in 50 ℃ of normal pressure baking ovens dry 12 hours, obtains MnO
2Monodimension nanometer material.Its XRD spectra is resolved XRD spectra and is shown that prepared sample has good crystalline structure as shown in Figure 1, and crystalline structure is α-MnO
2
Prepared material adopts LEO1525 type sem observation pattern as shown in Figure 3.As can be seen from Figure 3, its length of prepared material is about 2 μ m, and diameter is the MnO with very big length-to-diameter ratio about 100nm
2Nanometer filamentary material, and good dispersion.
Embodiment 2
In 100 ml beakers, add 30 ml distilled waters or deionized water, with the 5 mmole potassium permanganate solution a that obtains soluble in water.In 100 ml beakers, add 20 ml distilled waters or deionized water in addition, with the 7.5 mmole manganese acetates solution b that obtains soluble in water.It is 100 milliliters containing in the teflon-lined stainless steel hydrothermal reaction kettle that solution a and solution b are mixed, stir, change over to volume, and with the still sealing, the thermostat container of putting into 140 ℃ reacted 8 hours.Behind the naturally cooling, adopting the mode of centrifuge washing solid-liquid separation, is neutral with distilled water or deionized water wash to pH, and 80 ℃ of vacuum-drying is 10 hours then, obtains MnO
2Monodimension nanometer material.
MnO with preparation
2For active substance, acetylene black AB are that conductive agent, poly(vinylidene fluoride) PVDF are binding agent, MnO
2: the mass ratio of AB: PVDF is to make the electrode of ultracapacitor at 80: 10: 10.At first, active substance is mixed with acetylene black, fully grinds, then with ground powder and the PVDF thorough mixing that is dissolved among the N-N-methyl-2-2-pyrrolidone N-NMP, mix well pulping, be uniformly coated on then on the collector nickel foil, dry 10h under 90 ℃ promptly gets electrode slice.With the 2mol/L metabisulfite solution is electrolytic solution, is assembled into symmetric two electrode system ultracapacitors, and in 0~1V voltage range, the CHI660A electrochemical workstation that utilizes Shanghai occasion China instrument company to produce carries out the cyclic voltammetric test.Unipolarly adopt following formula to calculate than electric capacity:
C, I, m and v represent that respectively ultracapacitor is unipolar than electric capacity (F/g) in the formula, the electric current (A) that cyclic voltammetry curve intermediate potential point is corresponding, active substance MnO
2Quality (g) and scanning speed (V/s).
The cyclic voltammetry curve figure of this ultracapacitor in the sodium sulfate electrolyte solution is 245F/g than capacitance as shown in Figure 2, superior performance.Prepared material adopts LEO1525 type sem observation pattern as shown in Figure 4.As can be seen from Figure 4, its length of prepared material is about 1 μ m, and diameter is 50nm~100nm, is to have the very MnO of big L/D ratio
2Nanometer filamentary material, and good dispersion.
Embodiment 3
In 100 ml beakers, add 30 ml distilled waters or deionized water, with the 7.5 mmole potassium permanganate solution a that obtains soluble in water.In 100 ml beakers, add 20 ml distilled waters or deionized water in addition, with the 11.25 mmole manganese acetates solution b that obtains soluble in water.It is 100 milliliters containing in the teflon-lined stainless steel hydrothermal reaction kettle that solution a and solution b are mixed, stir, change over to volume, and with the still sealing, the thermostat container of putting into 150 ℃ reacted 6 hours.Behind the naturally cooling, adopting the mode of centrifuge washing solid-liquid separation, is neutral with distilled water or deionized water wash to pH, and 100 ℃ of vacuum-drying is 6 hours then, obtains MnO
2Monodimension nanometer material.
Prepared material adopts LEO1525 type sem observation pattern as shown in Figure 5.As can be seen from Figure 5, its length of prepared material is about 1.2 μ m, and diameter is 50nm~100nm, is the MnO with very big length-to-diameter ratio
2Nanometer filamentary material, and good dispersion.
Embodiment 4
In 100 ml beakers, add 30 ml distilled waters or deionized water, with the 10 mmole potassium permanganate solution a that obtains soluble in water.In 100 ml beakers, add 20 ml distilled waters or deionized water in addition, with the 15 mmole manganese acetates solution b that obtains soluble in water.It is 100 milliliters containing in the teflon-lined stainless steel hydrothermal reaction kettle that solution a and solution b are mixed, stir, change over to volume, and with the still sealing, the thermostat container of putting into 180 ℃ reacted 2 hours.Behind the product naturally cooling that obtains, be neutrality to pH for several times with distilled water or deionized water and absolute ethanol washing after, put into 80 ℃ of baking ovens dry 12 hours, obtain MnO
2Monodimension nanometer material.
Prepared material adopts LEO1525 type sem observation pattern as shown in Figure 6.As can be seen from Figure 6, its length of prepared material is about 1 μ m, and diameter is the MnO that has than big L/D ratio about 100nm
2Nanometer filamentary material, and good dispersion.
Embodiment 5
In 100 ml beakers, add 30 ml distilled waters or deionized water, with the 20 mmole potassium permanganate solution a that obtains soluble in water.In 100 ml beakers, add 20 ml distilled waters or deionized water in addition, with the 30 mmole manganese acetates solution b that obtains soluble in water.It is 100 milliliters containing in the teflon-lined stainless steel hydrothermal reaction kettle that solution a and solution b are mixed, stir, change over to volume, and with the still sealing, the thermostat container of putting into 200 ℃ reacted 1 hour.Behind the product naturally cooling, adopting the filtering and washing mode, is neutral with distilled water or deionized water wash to pH, and drying is 10 hours in 100 ℃ of normal pressure baking ovens, obtains MnO
2Monodimension nanometer material.
Prepared material adopts LEO1525 type sem observation pattern as shown in Figure 7.As can be seen from Figure 7, its length of prepared material is about 0.8 μ m, and diameter is the MnO with certain length-to-diameter ratio about 100nm
2Nanometer filamentary material, and good dispersion.
Embodiment 6
In 100 ml beakers, add 30 ml distilled waters or deionized water, with the 20 mmole potassium permanganate solution a that obtains soluble in water.In 100 ml beakers, add 20 ml distilled waters or deionized water in addition, with the 32 mmole manganese acetates solution b that obtains soluble in water.It is 100 milliliters containing in the teflon-lined stainless steel hydrothermal reaction kettle that solution a and solution b are mixed, stir, change over to volume, and with the still sealing, the thermostat container of putting into 200 ℃ reacted 2 hours.Behind the product naturally cooling, adopting the filtering and washing mode, is neutral with distilled water or deionized water wash to pH, and drying is 10 hours in 100 ℃ of normal pressure baking ovens, obtains MnO
2Monodimension nanometer material.
Prepared material adopts LEO1525 type sem observation pattern as shown in Figure 8.As can be seen from Figure 8, its length of prepared material is about 0.4 μ m, and diameter is the MnO with certain length-to-diameter ratio about 100nm
2Nanometer filamentary material, and good dispersion.
Claims (4)
1. the preparation method of a manganese dioxide one-dimensional nano material, step is:
1. potassium permanganate is dissolved in distilled water or the deionized water, stirs and obtain purplish red solution, its concentration is 0.05mol/L~2.0mol/L;
2. manganese acetate is dissolved in distilled water or the deionized water, stir colourless transparent solution, its concentration is 0.05mol/L~3.0mol/L;
3. 1. and change over to behind the A 2., B solution mixing and stirring and have in the teflon-lined stainless steel hydrothermal reaction kettle, 50 ℃~200 ℃ reactions 1 hour~36 hours down with step;
4. naturally cooling after 3. step is reacted and finished, with throw out after filtration, after the washing, drying manganese dioxide one-dimensional nano material.
2. the preparation method of manganese dioxide one-dimensional nano material according to claim 1 is characterized in that: described step 3. in, it is that molar ratio according to potassium permanganate and manganese acetate is to carry out in 2: 3~2: 3.2 that A and B solution mix.
3. the preparation method of manganese dioxide one-dimensional nano material according to claim 1 and 2, it is characterized in that: the concrete wash conditions of described step in 4. is that reaction product is dispersed in distilled water or the deionized water, adopt the mode of decompress filter or centrifugation, repetitive scrubbing 3~4 times is till washing lotion pH neutrality.
4. the preparation method of manganese dioxide one-dimensional nano material according to claim 1 and 2, it is characterized in that: the drying conditions of step in 4. is, drying temperature is 50 ℃~120 ℃, and be 6 hours~24 hours time of drying, adopts normal pressure or Minton dryer to carry out.
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CN101966976A (en) * | 2010-09-21 | 2011-02-09 | 南京理工大学 | Manganese dioxide-silver oxide composite oxide nanowire and preparation method thereof adopting single-walled carbon nanotubes as templates |
WO2012083511A1 (en) * | 2010-12-20 | 2012-06-28 | 海洋王照明科技股份有限公司 | Preparation method and use of manganese dioxide nano-rod |
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CN108630457A (en) * | 2018-05-09 | 2018-10-09 | 上海电力学院 | A kind of amorphous manganese dioxide and preparation method thereof and its application |
CN109300706A (en) * | 2018-09-30 | 2019-02-01 | 西安理工大学 | A kind of preparation method of manganese dioxide composite electrode |
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CN116550320B (en) * | 2023-05-12 | 2024-02-02 | 河北地质大学 | Synthesis method of manganese dioxide nano material with neuron-like cell structure |
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