CN101531402A - Method for preparing manganese dioxide one-dimensional nanometer material - Google Patents
Method for preparing manganese dioxide one-dimensional nanometer material Download PDFInfo
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- CN101531402A CN101531402A CN200910049408A CN200910049408A CN101531402A CN 101531402 A CN101531402 A CN 101531402A CN 200910049408 A CN200910049408 A CN 200910049408A CN 200910049408 A CN200910049408 A CN 200910049408A CN 101531402 A CN101531402 A CN 101531402A
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Abstract
The invention provides a method for preparing a manganese dioxide one-dimensional nanometer material in the field of inorganic nanometer material. The method comprises the following steps: solvent a and solvent b are prepared, wherein the solvent a is prepared by dissolving manganese chloride in pure water, adding a dressing agent into the water to be mixed, and the ratio of molar weight of the manganese chloride and the dressing agent is 3:2-1:2; the solvent b is prepared by dissolving potassium permanganate in the pure water; the solvent a and the solvent b in the step one are mixed, wherein the mixing is carried out according to the molar ratio of the manganese chloride and the potassium permanganate of 3:2; the mixed solvent is stirred, and the mixed solution is transferred into a high pressure autoclave containing a polyfluortetraethylene liner to react for 2 to 24 hours at a temperature of between 100 and 200 DEG C, then naturally cooled; a product obtained after cooling in the step two is washed and dried to obtain the manganese dioxide one-dimensional nanometer material. The method has the advantages of simple and convenient operation, high yield, even and controllable product crystal formation and appearance and the like.
Description
Technical field
The present invention relates to a kind of preparation method of field of inorganic nano material, specifically is a kind of preparation method of manganese dioxide one-dimensional nano material.
Technical background
Manganse Dioxide is a kind of important inorganic materials, and its source is abundant, cheap, environmentally friendly, has purposes widely, can be used for molecular sieve, magneticsubstance, glass, pottery, advanced catalysts, electrode of rechargeable battery material etc.Particularly the nano-manganese dioxide chemical property is better, have superior ion/electron conductivity and relative high current potential, make it very important application be arranged, for example as alkaline Mn cell positive electrode material, high-energy-density anode material of lithium battery and electrode material for super capacitor etc. in electrochemical field.A lot of preparation methods about nano-manganese dioxide are arranged at present, such as: sol-gel method, low temperature solid-phase synthesis, microemulsion method, chemical precipitation method, hydrothermal method, template etc.Wherein hydrothermal method is with its mild condition, controllability is good, the output advantages of higher becomes nano-manganese dioxide main synthetic method.
Find that through literature search Yao China, Shi Liyi, Zhong Qingdong have delivered the 29th～35 page of the 34th the 6th phase of volume of " New Chemical Materials " June in 2006 and be entitled as " nanometer α-MnO to prior art
2The pre-test of pattern regulate and control method " literary composition, mention in the literary composition: with KMnO
4, dodecyl alcohol polyoxyethylene (3) ether (AEO-3), poly(oxyethylene glycol) 400 (PEG400) is raw material, adopts normal temperature liquid-phase reduction reaction method successfully to prepare spherical and rod-like nano α-MnO
2But need be 400 ℃ of following calcinations 4 hours, and pattern be irregular inhomogeneous; The 705th～708 page of Zhang Yuanguang, Liu Yi, Guo Fanzai " artificial lens journal " the 35th the 4th phase of volume of August in 2006 delivered and has been entitled as " bar-shaped MnOOH of Hydrothermal Growth and MnO
2Crystal " literary composition, mention in the literary composition: with potassium permanganate (KMnO
4) and ammonium sulfate ((NH
4)
2SO
4) be main raw material, 150 ℃ the reaction 16h, Hydrothermal Growth bar-shaped MnOOH crystal, be precursor with the bar-shaped MnOOH crystal of synthetic then, in sulphuric acid soln, 130 ℃ of hydro-thermal reaction 12h, bar-shaped MnO has grown
2Crystal was divided into for two steps and synthesizes MnO
2But these methods are all more loaded down with trivial details, and multistep is synthetic that degree of purity of production and output are greatly reduced, so the nanometer MnO of the synthetic pattern homogeneous and controllable of single stage method
2Particularly important, adopt simple inorganic salt to control MnO simultaneously at present
2The crystal formation and the pattern of product yet there are no report.
Summary of the invention
The objective of the invention is to overcome the deficiencies in the prior art, a kind of preparation method of manganese dioxide one-dimensional nano material is provided.Method of the present invention is oversimplified the synthetic method of nano material of manganese dioxide, has advantages such as easy and simple to handle, output height, product crystal formation and pattern homogeneous and controllable.
The present invention is achieved by the following technical solutions, the present invention includes following steps:
Step 1, preparation solution a and solution b:
Solution a: Manganous chloride tetrahydrate is dissolved in the pure water, adds modifier then, stir, form solution a; Wherein, Manganous chloride tetrahydrate is 3:2～1:2 with the molar weight ratio of modifier;
Solution b: potassium permanganate is dissolved in the pure water, forms solution b;
Step 2 is mixed the solution a in the step 1 and solution b, wherein mixes mol ratio according to Manganous chloride tetrahydrate and potassium permanganate and is the ratio of 3:2 and carry out; Stir, afterwards mixed solution is transferred in the autoclave that contains polytetrafluoroethylliner liner, 100 ℃～200 ℃ were reacted naturally cooling 2～24 hours down;
Step 3, the product that obtains after washing step two coolings, drying obtains manganese dioxide one-dimensional nano material.
In the step 1, described modifier is a kind of in sodium sulfate, sodium-chlor, Sodium Fluoride, SODIUMNITRATE, the Neutral ammonium fluoride.
In the step 3, described washing is meant: the solid product that utilizes the whizzer resulting separation, again with the centrifugation in pure water of solid product ultra-sonic dispersion, carry out repeatedly 3～4 times, again pure water is changed into the centrifugation of ethanol dispersible solid product, carry out repeatedly 2～3 times, the solid product that obtains at last carries out drying treatment, and the rotating speed of whizzer is 3000～5000rpm.
In the step 3, described drying conditions is, dries 4～6 hours in 60 ℃.
The present invention changes the crystal formation and the pattern of product in kind that changes simple inorganic salt modifier and amount.The resulting product of the present invention has α-MnO
2And β-MnO
2, can find that under Electronic Speculum product has multiple pattern, the product pattern difference that the amount of different modifiers and different modifying agent of adding obtains can prepare the nanometer wire, material such as nanotube-shaped and nano bar-shape.
The present invention has following beneficial effect: but the present invention's single stage method synthesizes nano material of manganese dioxide, and in kind that changes simple inorganic salt modifier and amount, change the crystal formation and the pattern of product; Method of the present invention is easy, and operation is easily gone, and the output height is convenient to control; The Manganse Dioxide of the present invention's preparation can be widely used in industry and sphere of lifes such as catalysis, energy storage, biology, electromagnetism.
Description of drawings
Fig. 1 is the nano wire electron scanning micrograph that embodiment 1 prepares;
Fig. 2 is the nanotube electron scanning micrograph that embodiment 2 prepares;
Fig. 3 is the nanometer rod electron scanning micrograph that embodiment 3 prepares;
Fig. 4 is the nanometer rod electron scanning micrograph that embodiment 7 prepares.
Embodiment
Following example will the invention will be further described in conjunction with the accompanying drawings.Present embodiment has provided detailed embodiment and process being to implement under the prerequisite with the technical solution of the present invention, but protection scope of the present invention is not limited to following embodiment.The experimental technique of unreceipted actual conditions in the following example, usually according to normal condition, or the condition of advising according to manufacturer.
Embodiment 1
In 50 milliliters beaker, inject 10 milliliters pure water,, 3 mmole Sodium Fluorides are dissolved in wherein obtain solution a again 1.5 mmole Manganous chloride tetrahydrates formation settled solution soluble in water.Get the pure water that 50 ml beakers inject 10 milliliters in addition, with the 1 mmole potassium permanganate solution b that obtains soluble in water.Solution a and solution b mixed stir that to change volume after 30 minutes over to be in 35 milliliters the stainless steel autoclave that contains polytetrafluoroethylliner liner, replenish pure water,, put into 180 ℃ high temperature oven reaction 24 hours the still sealing to still volumetrical 70%～90%.With putting into 60 ℃ of baking oven oven dry 6 hours after pure water and the washing with alcohol centrifugation for several times, obtain α-MnO behind the product naturally cooling that obtains
2Monodimension nanometer material.Fig. 1 is the nano wire electron scanning micrograph that present embodiment is prepared.
Embodiment 2
In 50 milliliters beaker, inject 10 milliliters pure water,, 1 mmole Sodium Fluoride is dissolved in wherein obtains solution a again 1.5 mmole Manganous chloride tetrahydrates formation settled solution soluble in water.Get the pure water that 50 ml beakers inject 10 milliliters in addition, with the 1 mmole potassium permanganate solution b that obtains soluble in water.Solution a and solution b mixed stir that to change volume after 30 minutes over to be in 35 milliliters the stainless steel autoclave that contains polytetrafluoroethylliner liner, replenish pure water to still volumetrical 70%～90%.With the still sealing, the high temperature oven of putting into 180 ℃ reacted 24 hours.With putting into 60 ℃ of baking oven oven dry 6 hours after pure water and the washing with alcohol centrifugation for several times, obtain β-MnO behind the product naturally cooling that obtains
2Monodimension nanometer material.Fig. 2 is the nano wire electron scanning micrograph that present embodiment is prepared.
Embodiment 3
In 50 milliliters beaker, inject 10 milliliters pure water,, 1 mmole sodium sulfate is dissolved in wherein obtains solution a again 1.5 mmole Manganous chloride tetrahydrates formation settled solution soluble in water.Get the pure water that 50 ml beakers inject 10 milliliters in addition, with the 1 mmole potassium permanganate solution b that obtains soluble in water.Solution a and solution b mixed stir that to change volume after 30 minutes over to be in 35 milliliters the stainless steel autoclave that contains polytetrafluoroethylliner liner, replenish pure water to still volumetrical 70%～90%.With the still sealing, the high temperature oven of putting into 180 ℃ reacted 24 hours.With putting into 60 ℃ of baking oven oven dry 6 hours after pure water and the washing with alcohol centrifugation for several times, obtain β-MnO behind the product naturally cooling that obtains
2Monodimension nanometer material.Fig. 3 is the nano wire electron scanning micrograph that present embodiment is prepared.
Embodiment 4
In 50 milliliters beaker, inject 10 milliliters pure water,, 1 mmole Sodium Fluoride is dissolved in wherein obtains solution a again 1.5 mmole Manganous chloride tetrahydrates formation settled solution soluble in water.Get the pure water that 50 ml beakers inject 10 milliliters in addition, with the 1 mmole potassium permanganate solution b that obtains soluble in water.Solution a and solution b mixed stir that to change volume after 30 minutes over to be in 35 milliliters the stainless steel autoclave that contains polytetrafluoroethylliner liner, replenish pure water to still volumetrical 70%～90%.With the still sealing, the high temperature oven of putting into 180 ℃ reacted 2 hours.With putting into 60 ℃ of baking oven oven dry 6 hours after pure water and the washing with alcohol centrifugation for several times, obtain β-MnO behind the product naturally cooling that obtains
2Monodimension nanometer material.The nano wire electron scanning micrograph that present embodiment is prepared is similar to Fig. 2.
Embodiment 5
In 50 milliliters beaker, inject 10 milliliters pure water,, 1 mmole Sodium Fluoride is dissolved in wherein obtains solution a again 1.5 mmole Manganous chloride tetrahydrates formation settled solution soluble in water.Get the pure water that 50 ml beakers inject 10 milliliters in addition, with the 1 mmole potassium permanganate solution b that obtains soluble in water.Solution a and solution b mixed stir that to change volume after 30 minutes over to be in 35 milliliters the stainless steel autoclave that contains polytetrafluoroethylliner liner, replenish pure water to still volumetrical 70%～90%.With the still sealing, the high temperature oven of putting into 100 ℃ reacted 24 hours.With putting into 60 ℃ of baking oven oven dry 6 hours after pure water and the washing with alcohol centrifugation for several times, obtain α-MnO behind the product naturally cooling that obtains
2Monodimension nanometer material.The nano wire electron scanning micrograph that present embodiment is prepared is similar to Fig. 1.
Embodiment 6
In 50 milliliters beaker, inject 10 milliliters pure water,, 1 mmole Neutral ammonium fluoride is dissolved in wherein obtains solution a again 1.5 mmole Manganous chloride tetrahydrates formation settled solution soluble in water.Get the pure water that 50 ml beakers inject 10 milliliters in addition, with the 1 mmole potassium permanganate solution b that obtains soluble in water.Solution a and solution b mixed stir that to change volume after 30 minutes over to be in 35 milliliters the stainless steel autoclave that contains polytetrafluoroethylliner liner, replenish pure water to still volumetrical 70%～90%.With the still sealing, the high temperature oven of putting into 180 ℃ reacted 24 hours.With putting into 60 ℃ of baking oven oven dry 6 hours after pure water and the washing with alcohol centrifugation for several times, obtain β-MnO behind the product naturally cooling that obtains
2Monodimension nanometer material.The nano wire electron scanning micrograph that present embodiment is prepared is similar to Fig. 2.
Embodiment 7
In 50 milliliters beaker, inject 10 milliliters pure water,, 1 mmole sodium-chlor is dissolved in wherein obtains solution a again 1.5 mmole Manganous chloride tetrahydrates formation settled solution soluble in water.Get the pure water that 50 ml beakers inject 10 milliliters in addition, with the 1 mmole potassium permanganate solution b that obtains soluble in water.Solution a and solution b mixed stir that to change volume after 30 minutes over to be in 35 milliliters the stainless steel autoclave that contains polytetrafluoroethylliner liner, replenish pure water to still volumetrical 70%～90%.With the still sealing, the high temperature oven of putting into 180 ℃ reacted 24 hours.With putting into 60 ℃ of baking oven oven dry 6 hours after pure water and the washing with alcohol centrifugation for several times, obtain β-MnO behind the product naturally cooling that obtains
2Monodimension nanometer material.Fig. 4 is the nano wire electron scanning micrograph that present embodiment is prepared.
Embodiment 8
In 50 milliliters beaker, inject 10 milliliters pure water,, 1 mmole SODIUMNITRATE is dissolved in wherein obtains solution a again 1.5 mmole Manganous chloride tetrahydrates formation settled solution soluble in water.Get the pure water that 50 ml beakers inject 10 milliliters in addition, with the 1 mmole potassium permanganate solution b that obtains soluble in water.Solution a and solution b mixed stir that to change volume after 30 minutes over to be in 35 milliliters the stainless steel autoclave that contains polytetrafluoroethylliner liner, replenish pure water to still volumetrical 70%～90%.With the still sealing, the high temperature oven of putting into 180 ℃ reacted 24 hours.With putting into 60 ℃ of baking oven oven dry 6 hours after pure water and the washing with alcohol centrifugation for several times, obtain β-MnO behind the product naturally cooling that obtains
2Monodimension nanometer material.The nano wire electron scanning micrograph that present embodiment is prepared is similar to Fig. 4.
Claims (4)
1, a kind of preparation method of manganese dioxide one-dimensional nano material is characterized in that, comprises the steps:
Step 1, preparation solution a and solution b:
Solution a: Manganous chloride tetrahydrate is dissolved in the pure water, adds modifier then, stir, form solution a; Wherein, Manganous chloride tetrahydrate is 3:2～1:2 with the molar weight ratio of modifier;
Solution b: potassium permanganate is dissolved in the pure water, forms solution b;
Step 2 is mixed the solution a in the step 1 and solution b, wherein mixes mol ratio according to Manganous chloride tetrahydrate and potassium permanganate and is the ratio of 3:2 and carry out; Stir, afterwards mixed solution is transferred in the autoclave that contains polytetrafluoroethylliner liner, 100 ℃～200 ℃ were reacted naturally cooling 2～24 hours down;
Step 3, the product that obtains after washing step two coolings, drying obtains 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, in the step 1, described modifier is a kind of in sodium sulfate, sodium-chlor, Sodium Fluoride, SODIUMNITRATE, the Neutral ammonium fluoride.
3, the preparation method of manganese dioxide one-dimensional nano material according to claim 1, it is characterized in that, in the step 3, described washing is specially, and utilizes the solid product of whizzer resulting separation, again with the centrifugation in pure water of solid product ultra-sonic dispersion, carry out repeatedly 3～4 times, again pure water is changed into the centrifugation of ethanol dispersible solid product, carry out repeatedly 2～3 times, the solid product that obtains at last carries out drying treatment, and the rotating speed of whizzer is 3000～5000rpm.
4, the preparation method of manganese dioxide one-dimensional nano material according to claim 1 is characterized in that, in the step 3, described drying conditions is specially, and dries 4～6 hours in 60 ℃.
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| CN101891297A (en) * | 2010-07-19 | 2010-11-24 | 江南大学 | Ozonization water treatment method using manganese dioxide one-dimensional nano material as catalyst |
| CN101950681A (en) * | 2010-09-09 | 2011-01-19 | 江西财经大学 | Method for preparing manganese oxide electrode material for super capacitor by solvothermal method |
| 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 |
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| 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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| CN101891297A (en) * | 2010-07-19 | 2010-11-24 | 江南大学 | Ozonization water treatment method using manganese dioxide one-dimensional nano material as catalyst |
| CN101950681A (en) * | 2010-09-09 | 2011-01-19 | 江西财经大学 | Method for preparing manganese oxide electrode material for super capacitor by solvothermal method |
| CN101950681B (en) * | 2010-09-09 | 2012-07-04 | 江西财经大学 | Method for preparing manganese oxide electrode material for super capacitor by solvothermal method |
| 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 |
| CN101966976B (en) * | 2010-09-21 | 2013-01-30 | 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 |
| CN103153870A (en) * | 2010-12-20 | 2013-06-12 | 海洋王照明科技股份有限公司 | Preparation method and use of manganese dioxide nano-rod |
| CN103153870B (en) * | 2010-12-20 | 2015-04-15 | 海洋王照明科技股份有限公司 | Preparation method and use of manganese dioxide nano-rod |
| CN103752815A (en) * | 2013-12-15 | 2014-04-30 | 北京工业大学 | Preparation method and application for one-dimensional silver/manganese oxide composite nano-materials with different morphologies |
| CN104599857A (en) * | 2015-01-22 | 2015-05-06 | 武汉理工大学 | Coaxial nanometer wire with porous graphene/MnO2 pipe and middle line structure, preparation method and application thereof |
| CN104599857B (en) * | 2015-01-22 | 2017-07-11 | 武汉理工大学 | Porous graphene/MnO2Pipe centerline construction coaxial nanowire and its preparation method and application |
| CN104773760A (en) * | 2015-04-14 | 2015-07-15 | 湖南有色金属研究院 | Preparation method and applications of nano-manganese oxide |
| CN107915260A (en) * | 2017-11-30 | 2018-04-17 | 中国科学院大连化学物理研究所 | A kind of nanometer MnO of high entropy of transition2The preparation method of particle |
| CN107915260B (en) * | 2017-11-30 | 2019-10-11 | 中国科学院大连化学物理研究所 | A kind of nanometer MnO of high entropy of transition2The preparation method of particle |
| CN110556249A (en) * | 2018-06-01 | 2019-12-10 | 南京理工大学 | Preparation method of alpha-MnO 2 nanorod array |
| CN109796048A (en) * | 2019-03-27 | 2019-05-24 | 中国人民解放军陆军工程大学 | A kind of control synthetic method of different crystal forms manganese dioxide |
| CN110171851A (en) * | 2019-06-06 | 2019-08-27 | 中国科学院过程工程研究所 | One-dimensional manganese bioxide material and its preparation method and application |
| CN110171851B (en) * | 2019-06-06 | 2021-01-26 | 中国科学院过程工程研究所 | One-dimensional manganese dioxide material and preparation method and application thereof |
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