CN101698512A - Method for preparing nano manganese dioxide of different crystal forms and appearances by adopting microwave hydrothermal method - Google Patents
Method for preparing nano manganese dioxide of different crystal forms and appearances by adopting microwave hydrothermal method Download PDFInfo
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Abstract
The invention discloses a method for preparing nano manganese dioxide of different crystal forms and appearances by adopting microwave hydrothermal method. The steps are as flows: (1) dissolving potassium hypermanganate in water, adding hydrochloric acid, and stirring to prepare a reaction solution; (2) pouring the reaction solution into a sealable reactor, placing the reactor in a microwave field for microwave radiation with microwave frequency being 2.45GHz, temperature being 105-115 DEG C, and heat preservation time being 0.5-2h, separating, washing and drying the generated precursor to obtain petal-shaped nano delta-phase manganese dioxide. In step (2), the temperature of the reaction solution is 135-145 DEG C, and the product of the reaction is alpha-phase manganese dioxide nanotube. The invention features simple technique, low cost, controllable product quality, extensive applicability and the like, the prepared nano manganese dioxide is applicable to fundamental theoretical research in such fields as battery, molecular sieve, catalyst and magnetic materials, and the research and development of related function materials.
Description
Technical field:
The present invention relates to a kind of preparation method of nano-manganese dioxide, relate in particular to a kind of method that adopts microwave-hydrothermal method to prepare different crystal forms and pattern nano-manganese dioxide, belong to field of inorganic nonmetallic material.
Background technology:
The basic structural unit of Manganse Dioxide is the hexagonal closs packing structure and the cubic close packing structure of being given by 1 manganese atom and 6 oxygen atom ligands.In close-packed structure, each atomic shell forms tetrahedron and octahedral hole.Modal structure promptly is [MnO
6] octahedra and adjacent octahedra shared rib and top, shared angle, and form protean complex network, these networks can hold various positively charged ion and coordination thing, this just causes nano-manganese dioxide to occur with different crystal formations and pattern, as five kinds of comparatively common different crystal forms of α, β, δ, γ and ε, and by the control to the preparation method, the Manganse Dioxide of various crystal formations can obtain different patterns again.Therefore nano-manganese dioxide has abundant and unique physics and chemical property, and characteristics such as its cheap and easy to get and environmental friendliness in addition make this material background that has a wide range of applications in fields such as electronics, catalysis, molecular sieve and potteries.
At present, various chemical methods are mainly adopted in the preparation of nano-manganese dioxide, and wherein hydrothermal method occupies an important position, and (J.Phys.Chem.C 2008 for " the physical chemistry magazine C " that american chemical association publishes, 112,5307-5315), " crystal growth and design " (Crystal Growth ﹠amp; Design, Vol.9, No.1,2009,528-533), " the European chemical proceedings " that European chemical association publishes (Chem.Eur.J.2009,15,492-500) nano-manganese dioxide of Hydrothermal Preparation different crystal forms different-shape is reported; Chinese invention patent 02100707.1 discloses a kind of method of synthetic different crystal form one-dimensional single crystal mangnesium dioxide nano wire, this method adopts hydrothermal method, with manganous salt and ammonium persulphate is raw material, is the one-dimensional single crystal nano wire that material additive has synthesized different crystal forms Manganse Dioxide with ammonium sulfate.The common issue with of above-mentioned the whole bag of tricks is: traditional hot conduction heating mode is adopted in reaction, make hydro-thermal reaction for up to 10～20 hours, thereby cause reaction product crystal formation and pattern to be difficult to control.
Summary of the invention:
The objective of the invention is to overcome the shortcoming of traditional Hydrothermal Preparation nano-manganese dioxide, a kind of method that adopts microwave-hydrothermal method to prepare different crystal forms and pattern nano-manganese dioxide is provided.This method has not only overcome the shortcoming of traditional hydrothermal method, and have that raw material is cheap and easy to get, technology is simple, product crystal formation and pattern are easy to realize the advantage controlled.
The present invention is achieved by the following technical programs:
A kind of method that adopts microwave-hydrothermal method to prepare different crystal forms and pattern nano-manganese dioxide, adopt following steps:
(1) potassium permanganate is soluble in water, add hydrochloric acid then, and stir, be made into reaction soln, the concentration of potassium permanganate is 0.01～0.1mol/L, the pH value of reaction soln is 2～3;
(2) above-mentioned reaction soln is poured in the sealable reaction vessel, place microwave field to carry out microwave exposure, microwave frequency is 2.45GHz, the reaction soln temperature is 105～115 ℃, soaking time is 0.5～2 hour, reaction finishes the back precursor that generates is separated, washs and drying, and the product that obtains is a nm delta phase Manganse Dioxide;
Wherein the temperature of reaction in the step (2) is preferred 110 ℃, preferred 0.5～1.5 hour of soaking time, and nm delta phase Manganse Dioxide has the petal pattern, corolla diameter 1～2 μ m, petal thickness 5～10nm.
A kind of method that adopts microwave-hydrothermal method to prepare different crystal forms and pattern nano-manganese dioxide, adopt following steps:
(1) potassium permanganate is soluble in water, add hydrochloric acid then, and stir, be made into reaction soln, the concentration of potassium permanganate is 0.01～0.1mol/L, the pH value of reaction soln is 2～3;
(2) reaction soln is poured in the sealable reaction vessel, place microwave field to carry out microwave exposure, microwave frequency is 2.45GHz, the reaction soln temperature is 135～145 ℃, soaking time is 0.5～2 hour, reaction finishes the back precursor that generates is separated, washs and drying, and the product that obtains is a α phase manganese dioxide nano pipe;
Wherein the temperature of reaction in the step (2) is preferred 140 ℃, preferred 0.5～1.5 hour of soaking time, and the α phase Manganse Dioxide of gained is square 1-dimention nano pipe, the nanotube length of side 80～120nm, thickness of pipe 8～10nm.
Reaction reagent of the present invention only needs potassium permanganate and two kinds of raw materials of deionized water, add the effect that small amount of hydrochloric acid plays conditioned reaction solution acid alkalinity pH value, adopt same reaction system, under the microwave exposure effect, by control to temperature of reaction and time, synthesize the nano-manganese dioxide with different crystal forms and shape characteristic fast, the α phase manganese dioxide nano pipe of preparation and the δ with petal pattern nano-manganese dioxide mutually all have bigger specific surface area.It is simple that the present invention has technology, and cost is low, controllable product quality, and characteristics such as suitability is wide, the nano-manganese dioxide of preparation can be used for the research and development of field fundamental researches such as battery, molecular sieve, catalysis, magneticsubstance and correlation function material.
Description of drawings
Fig. 1 is the XRD figure spectrum of embodiment 1 products therefrom δ phase Manganse Dioxide, and wherein X-coordinate is 2 θ diffraction angle, and ordinate zou is a diffracted intensity.
Fig. 2 is the field emission scanning electron microscope figure of embodiment 1 gained δ phase Manganse Dioxide.
Fig. 3 is the high-resolution-ration transmission electric-lens figure of embodiment 1 gained δ phase Manganse Dioxide.
Fig. 4 is the XRD figure spectrum of embodiment 2 products therefrom α phase Manganse Dioxide, and wherein X-coordinate is 2 θ diffraction angle, and ordinate zou is a diffracted intensity.
Fig. 5 is the field emission scanning electron microscope figure of embodiment 2 gained α phase Manganse Dioxide.
Fig. 6 is the high-resolution-ration transmission electric-lens figure of embodiment 2 gained α phase Manganse Dioxide.
Embodiment
Below in conjunction with embodiment and accompanying drawing the present invention is described in detail.
The chemical equation of reaction is expressed as follows:
4KMnO
4+2H
2O→4MnO
2+4KOH+3O
2
Embodiment 1
Take by weighing the analytically pure potassium permanganate KMnO of 2.53g earlier
4Be dissolved in the 300ml deionized water, measuring 5～6ml mass concentration again and be 36% concentrated hydrochloric acid joins in this solution, adding water makes the solution total amount to 400ml, after stirring treats that solution evenly, the solution for preparing poured into place microwave field (microwave frequency is 2.45GHz) to carry out microwave exposure in the sealable reaction vessel, solution temperature is controlled at 110 ℃, soaking time 1 hour, and reaction finishes the back precursor that generates is separated, washs and drying.Fig. 1～Fig. 3 is for characterizing the picture of gained to the product of embodiment 1 gained, wherein, Fig. 1 is the XRD figure spectrum of product, and the δ that has rhombohedral structure in this spectral line and the JCPDS database spectral line No.52-0556 of Manganse Dioxide mutually is very identical, shows that this product is a δ phase Manganse Dioxide; The δ that the electromicroscopic photograph of this product (Fig. 2 and Fig. 3) shows gained Manganse Dioxide mutually has the nanometer flower-shaped looks of the dendritic ramose of three-dimensional tree of similar biological tissue, the corolla diameter is at 1～2 μ m, petal thickness is 5～10nm, and the δ phase nano-manganese dioxide with this shape characteristic has big specific surface area.To same reaction system, with temperature of reaction respectively at 105 ℃, 110 ℃ and 115 ℃, soaking time was carried out at 0.5 hour, 1 hour, 1.5 hours and 2 hours respectively, products therefrom is the δ phase Manganse Dioxide of nano flower-like after tested, the corolla diameter is at 1～2 μ m, and petal thickness is 5～10nm.
Embodiment 2
Take by weighing the analytically pure potassium permanganate KMnO of 2.53g earlier
4Be dissolved in the 300ml deionized water, measuring 5～6ml mass concentration again and be 36% concentrated hydrochloric acid joins in this solution, adding water makes the solution total amount to 400ml, after stirring treats that solution evenly, the solution for preparing poured into place microwave field (microwave frequency is 2.45GHz) to carry out microwave exposure in the sealable reaction vessel, solution temperature is controlled at 140 ℃, soaking time 1 hour, and reaction finishes the back precursor that generates is separated, washs and drying.Fig. 4～Fig. 6 is for characterizing the picture of gained to the product of embodiment 1 gained, wherein, Fig. 4 is the XRD figure spectrum of product, and the α that has the tetragonal body structure in this spectral line and the JCPDS database spectral line No.72-1982 of Manganse Dioxide mutually is very identical, shows that this product is a α phase Manganse Dioxide; The α that the electromicroscopic photograph of this product (Fig. 5 and Fig. 6) shows gained Manganse Dioxide mutually is a square nanotube shape, and the length of side of nanometer square tube is at 80～120nm, and thickness of pipe is 8～10nm.To same reaction system, with temperature of reaction respectively at 135 ℃, 140 ℃ and 145 ℃, soaking time was carried out at 0.5 hour, 1 hour, 1.5 hours and 2 hours respectively, products therefrom is the α phase Manganse Dioxide of nanometer square tube type after tested, the length of side of nanometer square tube is at 80～120nm, and thickness of pipe is 8～10nm.
Claims (6)
1. method that adopts microwave-hydrothermal method to prepare different crystal forms and pattern nano-manganese dioxide is characterized in that adopting following steps:
(1) potassium permanganate is soluble in water, add hydrochloric acid then, and stir, be made into reaction soln, the concentration of potassium permanganate is 0.01～0.1mol/L, the pH value of reaction soln is 2～3;
(2) above-mentioned reaction soln is poured in the sealable reaction vessel, place microwave field to carry out microwave exposure, microwave frequency is 2.45GHz, the reaction soln temperature is 105～115 ℃, soaking time is 0.5～2 hour, reaction finishes the back precursor that generates is separated, washs and drying, and the product that obtains is a nm delta phase Manganse Dioxide.
2. the method for preparing different crystal forms and pattern nano-manganese dioxide according to claim 1 is characterized in that: the temperature of reaction in the step (2) is 110 ℃, and soaking time is 0.5～1.5 hour.
3. the method for preparing different crystal forms and pattern nano-manganese dioxide according to claim 1 is characterized in that: the product of step (2) is the nm delta phase Manganse Dioxide of petal pattern, corolla diameter 1～2 μ m, petal thickness 5～10nm.
4. method that adopts microwave-hydrothermal method to prepare different crystal forms and pattern nano-manganese dioxide is characterized in that adopting following steps:
(1) potassium permanganate is soluble in water, add hydrochloric acid then, and stir, be made into reaction soln, the concentration of potassium permanganate is 0.01～0.1mol/L, the pH value of reaction soln is 2～3;
(2) reaction soln is poured in the sealable reaction vessel, place microwave field to carry out microwave exposure, microwave frequency is 2.45GHz, the reaction soln temperature is 135～145 ℃, soaking time is 0.5～2 hour, reaction finishes the back precursor that generates is separated, washs and drying, and the product that obtains is a α phase manganese dioxide nano pipe.
5. the method for preparing different crystal forms and pattern nano-manganese dioxide according to claim 4 is characterized in that: the temperature of reaction in the step (2) is 140 ℃, and soaking time is 0.5～1.5 hour.
6. the method for preparing different crystal forms and pattern nano-manganese dioxide according to claim 4 is characterized in that: the product of step (2) is a α phase Manganse Dioxide square 1-dimention nano pipe, the nanotube length of side 80～120nm, thickness of pipe 8～10nm.
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