CN110171851A - One-dimensional manganese bioxide material and its preparation method and application - Google Patents
One-dimensional manganese bioxide material and its preparation method and application Download PDFInfo
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- CN110171851A CN110171851A CN201910495189.9A CN201910495189A CN110171851A CN 110171851 A CN110171851 A CN 110171851A CN 201910495189 A CN201910495189 A CN 201910495189A CN 110171851 A CN110171851 A CN 110171851A
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- C01G45/00—Compounds of manganese
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
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- C01P2004/03—Particle morphology depicted by an image obtained by SEM
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- C—CHEMISTRY; METALLURGY
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- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2004/00—Particle morphology
- C01P2004/10—Particle morphology extending in one dimension, e.g. needle-like
Abstract
A kind of one-dimensional manganese bioxide material and its preparation method and application, which includes: to mix manganese dioxide with neutral solution and carry out hydro-thermal reaction；By the mixed liquor separation after hydro-thermal reaction, obtained solid is one-dimensional manganese bioxide material.It is manganese source that the present invention, which has selected manganese dioxide low in cost, environmental-friendly, that physical and chemical performance is stable; neutral solution is materials synthesis environment; one step hydro-thermal has directly synthesized one-dimensional manganese bioxide material; process flow is simple, condition is controllable, production cost is low, it is environmental-friendly, safely, be easy to prepare with scale, have preferable prospects for commercial application.
Description
Technical field
The invention belongs to manganese bioxide material preparation fields, and in particular to a kind of one-dimensional manganese bioxide material and its preparation side
Method and application.
Background technique
Manganese dioxide due to excellent physicochemical characteristics and cheap price, Industrial Catalysis, heavy metal adsorption,
The fields such as battery, supercapacitor, biosensor are widely used.The microstructure of manganese dioxide is with [MnO6] octahedra
It is made up of for basic unit different corner connection types, different [MnO6] octahedral combination will form the not isomorphous
The manganese dioxide of type common are α-MnO2、β-MnO2、γ-MnO2、δ-MnO2Equal crystal forms.Meanwhile different synthesis condition shape
At the microscopic appearance of manganese dioxide be also not quite similar, common are the patterns such as lamella dress, flower-shaped, rodlike, linear.Manganese dioxide
The diversification of crystal form and pattern determine the diversification of its purposes.Wherein one-dimensional manganese dioxide is due to stronger catalysis energy
Power, good chemical property, receive significant attention in various industrial applications and scientific research.Currently, synthesizing one-dimensional dioxy
The method for changing manganese material specifically includes that via sol-gel template method, circumfluence method, high-temperature decomposition, acidic treatment and hydro-thermal method etc..
Hydro-thermal method has energy conservation and environmental protection, with short production cycle, product object mutually first-class advantage for other methods.
Existing material preparation technology is mainly reduction method and oxidizing process.Reduction method be using potassium permanganate as raw material, other
Reducing substances are reducing agent, and mixed liquor is placed in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle and carries out hydro-thermal reaction, after natural cooling,
One-dimensional manganese bioxide material will be obtained after reaction product centrifugation, washing, drying.This method is low in cost, reaction condition is mild,
Product quality is high, but there are problems that being also easy to produce Mn-bearing waste water, leads to environmental pollution.Oxidizing process is with manganous salt for original
Material, other oxidizing substances are oxidant, and mixed liquor is transferred to after mixing evenly in polytetrafluoroethylene (PTFE) hydrothermal reaction kettle and carries out water
Thermal response, after natural cooling, by reaction product centrifugation, washing, it is dry after obtain one-dimensional manganese bioxide material.This method cost
It is cheap, reaction condition is mild, easy to control, but equally exists the problem of being also easy to produce Mn-bearing waste water, lead to environmental pollution.It is above-mentioned
One-dimensional manganese bioxide material preparation process is not described the processing mode of material waste water produced during the preparation process, this
Limit the industrialized production of one-dimensional manganese dioxide.
Summary of the invention
In view of this, one of main object of the present invention is to propose a kind of one-dimensional manganese bioxide material and preparation method thereof
And application, at least be partially solved at least one of above-mentioned technical problem.
To achieve the goals above, as one aspect of the present invention, a kind of system of one-dimensional manganese bioxide material is provided
Preparation Method, comprising the following steps:
(1) manganese dioxide is mixed with neutral solution and carries out hydro-thermal reaction；
(2) mixed liquor after hydro-thermal reaction in step (1) is separated, obtained solid is one-dimensional manganese bioxide material.
As another aspect of the present invention, a kind of one-dimensional dioxy obtained by preparation method as described above is additionally provided
Change manganese material.
As an additional aspect of the present invention, additionally provides a kind of one-dimensional manganese bioxide material as described above and urged in industry
Change, the application of heavy metal adsorption, battery, supercapacitor, field of biosensors.
Based on the above-mentioned technical proposal it is found that one-dimensional manganese bioxide material of the invention and its preparation method and application relative to
The prior art one of at least has the advantage that:
1, it is manganese source that the present invention, which has selected manganese dioxide low in cost, environmental-friendly, that physical and chemical performance is stable, neutral
Solution is materials synthesis environment, and a step hydro-thermal has directly synthesized one-dimensional manganese bioxide material, process flow is simple, condition is controllable,
Production cost is low, it is environmental-friendly, safely, be easy to prepare with scale, there is preferable prospects for commercial application；
2, because the waste water that synthetic material generates can recycle, so the present invention is also able to achieve waste " zero-emission "；
3, material prepared by the present invention can serve as the electrode material of supercapacitor and lithium ion battery, catalyst material and
Heavy-metal adsorption material in environmental protection has preferable prospects for commercial application；
4, the one-dimensional manganese bioxide material of available pure phase through the invention.
Detailed description of the invention
Fig. 1 is the preparation technology flow chart of one-dimensional manganese bioxide material of the invention；
Fig. 2 is the powder XRD spectrum of the one-dimensional manganese bioxide material of the embodiment of the present invention 1；
Fig. 3 is the powder SEM figure of the one-dimensional manganese bioxide material of the embodiment of the present invention 1.
Specific embodiment
To make the objectives, technical solutions, and advantages of the present invention clearer, below in conjunction with specific embodiment, and reference
Attached drawing, the present invention is described in further detail.
The invention discloses a kind of preparation methods of one-dimensional manganese bioxide material, comprising the following steps:
(1) manganese dioxide is mixed with neutral solution and carries out hydro-thermal reaction；
(2) mixed liquor after hydro-thermal reaction in step (1) is separated, obtained solid is the one-dimensional manganese dioxide material
Material.
Wherein, further include carrying out step (3) after step (2): the solid that step (2) is obtained washs drying.
Wherein, neutral solution described in step (1) and the liquid-solid ratio of manganese dioxide are 5-1000mL/g, are, for example, 300mL/
g。
Wherein, the concentration of neutral solution described in step (1) is 0.1-10mol/L, is, for example, 5mol/L.
Wherein, the pH of neutral solution described in step (1) is 6-8, is, for example, 7.
Wherein, neutral solution described in step (1) is LiCl, LiBr, LiI, LiNO3、Li2SO4、NaCl、NaBr、NaI、
NaNO3、Na2SO4、KCl、KBr、KI、KNO3、K2SO4、MgCl2、MgBr2、MgI2、Mg(NO3)2、MgSO4、CaCl2、CaBr2、
CaI2、Ca(NO3)2Any one or more of aqueous solution.
Wherein, manganese dioxide described in step (1) is γ-MnO2、λ-MnO2、ε-MnO2It is any one or more of.
Wherein, the temperature of hydro-thermal reaction described in step (1) is 40-400 DEG C, is, for example, 150 DEG C.
Wherein, the time of hydro-thermal reaction described in step (1) is 2-120h, is, for example, 100h.
Wherein, the preparation by liquid circulation isolated in step (2) for neutral solution described in step (1).
Wherein, the solid in step (2) includes powder.
The invention also discloses a kind of one-dimensional manganese bioxide materials that the preparation method obtains.
Wherein, the diameter of the one-dimensional manganese bioxide material be 100-1000nm, for example, 100,200,300,400,
500、600、700、800、900、1000nm。
Wherein, the draw ratio of the one-dimensional manganese bioxide material be 2-1000, for example, 2,5,10,20,30,50,100,
200、300、500、600、700、800、900、1000。
The invention also discloses a kind of one-dimensional manganese bioxide materials as described above in Industrial Catalysis, heavy metal adsorption, electricity
The application in pond, supercapacitor or field of biosensors.
In an embodiment of the invention, the present invention is for example, by using following technical solution:
Mainly comprising the processes of for the preparation method of the one-dimensional manganese bioxide material mixes manganese dioxide with neutral solution,
It is after hydro-thermal reaction 2-120h that obtained solid washing is dry to get one-dimensional manganese bioxide material under the conditions of 40-400 DEG C.Different
The material of the different-diameter that diameter is 100-1000nm, draw ratio is 2-1000 and/or draw ratio can be obtained in preparation condition.
In a preferred embodiment, the present invention is for example, by using following technical solution:
A kind of preparation method of one-dimensional manganese bioxide material, comprising the following steps:
(1) hydrothermal synthesis: manganese dioxide is mixed with neutral solution and hydro-thermal reaction is carried out under certain temperature and pressure；
(2) it washs drying: being done after the powder that reaction product obtained in step (1) is obtained after being separated by solid-liquid separation is washed
Dry to obtain dry powder, powder is one-dimensional manganese bioxide material, and obtained liquid can be recycled in preparation neutral solution.
Wherein, manganese dioxide is γ-MnO in step (1)2、λ-MnO2、ε-MnO2Deng one of or it is a variety of.
Wherein, the neutral solution in step (1) is LiCl, LiBr, LiI, LiNO3、Li2SO4、NaCl、NaBr、NaI、
NaNO3、Na2SO4、KCl、KBr、KI、KNO3、K2SO4、MgCl2、MgBr2、MgI2、Mg(NO3)2、MgSO4、CaCl2、CaBr2、
Cai2、Ca(NO3)2Deng one of or a variety of solution mixed with water.
Wherein, the liquid-solid ratio of solution and manganese dioxide is 5-1000mL/g in step (1).
Wherein, the concentration of neutral solution is 0.1-10mol/L in step (1).
Wherein, the temperature of hydro-thermal reaction is 40-400 DEG C in step (1).
Wherein, the time of hydro-thermal reaction is 2-120h in step (1).
Wherein, the liquid obtained after being separated by solid-liquid separation in step (2) can be prepared again with compound described in step (1)
It is recycled at neutral solution, and in step (1).
In another preferred embodiment, the present invention is for example, by using following technical solution:
A kind of preparation method of one-dimensional manganese dioxide, comprising the following steps:
(1) hydrothermal synthesis: manganese dioxide is mixed with neutral solution and hydro-thermal reaction is carried out under certain temperature and pressure；
(2) it washs drying: being done after the powder that reaction product obtained in step (1) is obtained after being separated by solid-liquid separation is washed
Dry to obtain dry powder, powder is one-dimensional manganese bioxide material, and obtained liquid can be recycled in preparation neutral solution.
Wherein, manganese dioxide can be γ-MnO in step (1)2、λ-MnO2、ε-MnO2Deng one of or it is a variety of；
Wherein, the neutral solution in step (1) can be LiCl, LiBr, LiI, LiNO3、Li2SO4、NaCl、NaBr、NaI、
NaNO3、Na2SO4、KCl、KBr、KI、KNO3、K2SO4、MgCl2、MgBr2、MgI2、Mg(NO3)2、MgSO4、CaCl2、CaBr2、
CaI2、Ca(NO3)2Deng one of or a variety of solution mixed with water；
Wherein, the liquid-solid ratio of solution and manganese dioxide is 5-1000mL/g in step (1), may be, for example, 5,50,100,
150、200、250、300、350、400、450、500、550、600、650、700、750、800、850、900、950、1000mL/g
Deng；
Wherein, the concentration of neutral solution is 0.1-10mol/L in step (1), may be, for example, 0.1,0.5,1,1.5,2,
2.5,3,3.5,4,4.5,5,5.5,6,6.5,7,7.5,8,8.5,9,9.5,10mol/L etc.；
Wherein, the temperature of hydro-thermal reaction is 40-400 DEG C in step (1), may be, for example, 40,80,120,160,200,240,
280,320,360,400 DEG C etc.；
Wherein, the time of hydro-thermal reaction is 2-120h in step (1), may be, for example, 2,5,10,15,20,25,30,35,
40,45,50,55,60,65,70,75,80,85,90,95,100,105,110,115,120h etc.；
Wherein, the liquid obtained after being separated by solid-liquid separation in step (2) can be prepared again with compound described in step (1)
It is recycled at neutral solution, and in step (1).
Explanation is further elaborated to technical solution of the present invention below by way of specific embodiment combination attached drawing.It should be noted that
, following specific embodiments are only as example, the scope of protection of the present invention is not limited thereto.
Chemicals used in following embodiments and raw material are commercially available gained or are made by oneself by well known preparation method
It obtains.
Embodiment 1
(1) 10g γ-MnO is weighed2, 6g LiCl and 6g NaCl be mixed in 100mL deionized water, thereafter use hydro-thermal
Synthetic method carries out hydro-thermal reaction, time 30h at 150 DEG C；
(2) dry after the powder obtained reaction product obtained in step (1) after being separated by solid-liquid separation is washed, obtain one
Manganese bioxide material is tieed up, obtained liquid is retained, and preparation neutral solution is ready to use in.
The XRD spectrum of the material obtained through this embodiment is as shown in Fig. 2, display β-MnO2Phase, no miscellaneous peak；SEM spectrum
As shown in figure 3, display material is in uniform one-dimensional rod-like pattern, length is 5-10 μm, and diameter is 0.5-1 μm.In conclusion logical
Cross the one-dimensional manganese bioxide material of the available pure phase of this method.When manganese dioxide raw material are in thermal and hydric environment, can be decomposed into
[MnO6] matrix, neutral environment will induction [MnO from different anions and canons6] matrix along high-energy surface grow, ultimately generate crystallization
Spend (as shown in Figure 2), the uniform one-dimensional material (as shown in Figure 3) of pattern.
Embodiment 2
(1) 4g λ-MnO is weighed2、10g NaNO3、4g K2SO4With 0.5g MgI2It is mixed in 50mL deionized water, thereafter
Using hydrothermal synthesis method, hydro-thermal reaction, time 20h are carried out at 300 DEG C；
(2) reaction product obtained in step (1) is dry after same liquid powder obtained after separation is washed, obtain one
Manganese bioxide material is tieed up, obtained liquid is retained, and preparation neutral solution is ready to use in.
The one-dimensional manganese bioxide material of available pure phase through this embodiment.
Embodiment 3
(1) 0.5g ε-MnO is weighed2、5g Li2SO4, 4g KBr and 0.5g NaI be mixed in the neutrality of 80mL recycling
In solution, hydrothermal synthesis method is used thereafter, hydro-thermal reaction, time 6h are carried out at 80 DEG C；
(2) dry after the powder obtained reaction product obtained in step (1) after being separated by solid-liquid separation is washed, obtain one
Manganese bioxide material is tieed up, obtained liquid is retained, and preparation neutral solution is ready to use in.
The one-dimensional manganese bioxide material of available pure phase through this embodiment.
Embodiment 4
(1) 5g γ-MnO is weighed2、10gε-MnO2、25g NaNO3With 25g CaCl2It is mixed in 100mL recycling
In neutral solution, hydrothermal synthesis method is used thereafter, hydro-thermal reaction, time 100h are carried out at 100 DEG C；
(2) dry after the powder obtained reaction product obtained in step (1) after being separated by solid-liquid separation is washed, obtain one
Manganese bioxide material is tieed up, obtained liquid is retained, and preparation neutral solution is ready to use in.
The one-dimensional manganese bioxide material of available pure phase through this embodiment.
Embodiment 5
(1) 4g ε-MnO is weighed2、4g λ-MnO2, 0.5g LiI and 4g MgSO4It is mixed in the neutrality of 40mL recycling
In solution, hydrothermal synthesis method is used thereafter, hydro-thermal reaction, time 60h are carried out at 350 DEG C；
(2) dry after the powder obtained reaction product obtained in step (1) after being separated by solid-liquid separation is washed, obtain one
Manganese bioxide material is tieed up, obtained liquid is retained, and preparation neutral solution is ready to use in.
The one-dimensional manganese bioxide material of available pure phase through this embodiment.
Embodiment 6
(1) 12g γ-MnO is weighed2、4g λ-MnO2、0.67g Ca(NO3)2With 1g MgCl2Being mixed in 100mL circulation makes
In neutral solution, hydrothermal synthesis method is used thereafter, hydro-thermal reaction, time 110h are carried out at 370 DEG C；
(2) dry after the powder obtained reaction product obtained in step (1) after being separated by solid-liquid separation is washed, obtain one
Manganese bioxide material is tieed up, obtained liquid is retained, and preparation neutral solution is ready to use in.
The one-dimensional manganese bioxide material of available pure phase through this embodiment.
Embodiment 7
(1) 6g γ-MnO is weighed2、3g λ-MnO2、4g ε-MnO2, 10g LiBr, 10g K1 and 6g Na2SO4It is mixed in
In the neutral solution that 90mL is recycled, hydrothermal synthesis method is used thereafter, hydro-thermal reaction, time 70h are carried out at 170 DEG C；
(2) dry after the powder obtained reaction product obtained in step (1) after being separated by solid-liquid separation is washed, obtain one
Manganese bioxide material is tieed up, obtained liquid is retained, and preparation neutral solution is ready to use in.
The one-dimensional manganese bioxide material of available pure phase through this embodiment.
In conclusion a kind of preparation method of one-dimensional manganese bioxide material of the present invention can simple, controllable, batch, safety,
Environmentally friendly ground synthesizing one-dimensional manganese bioxide material.
Particular embodiments described above has carried out further in detail the purpose of the present invention, technical scheme and beneficial effects
Describe in detail bright, it should be understood that the above is only a specific embodiment of the present invention, is not intended to restrict the invention, it is all
Within the spirit and principles in the present invention, any modification, equivalent substitution, improvement and etc. done should be included in protection of the invention
Within the scope of.
Claims (10)
1. a kind of preparation method of one-dimensional manganese bioxide material, which comprises the following steps:
(1) manganese dioxide is mixed with neutral solution and carries out hydro-thermal reaction；
(2) mixed liquor after hydro-thermal reaction in step (1) is separated, obtained solid is the one-dimensional manganese bioxide material.
2. preparation method according to claim 1, which is characterized in that
Also carry out step (3) after step (2): the solid that step (2) is obtained washs drying.
3. preparation method according to claim 1, which is characterized in that
Neutral solution described in step (1) and the liquid-solid ratio of manganese dioxide are 5-1000mL/g, preferably 300mL/g.
4. preparation method according to claim 1, which is characterized in that
The concentration of neutral solution described in step (1) is 0.1-10mol/L, preferably 5mol/L；
Preferably, the pH of neutral solution described in step (1) is 6-8, preferably 7.
5. preparation method according to claim 1, which is characterized in that
Neutral solution described in step (1) is LiCl, LiBr, LiI, LiNO3、Li2SO4、NaCl、NaBr、NaI、NaNO3、
Na2SO4、KCl、KBr、KI、KNO3、K2SO4、MgCl2、MgBr2、MgI2、Mg(NO3)2、MgSO4、CaCl2、CaBr2、CaI2、Ca
(NO3)2Any one or more of aqueous solution.
6. preparation method according to claim 1, which is characterized in that
Manganese dioxide described in step (1) is γ-MnO2、λ-MnO2、-MnO2It is any one or more of.
7. preparation method according to claim 1, which is characterized in that
The temperature of hydro-thermal reaction described in step (1) is 40-400 DEG C, preferably 150 DEG C；
Preferably, the time of hydro-thermal reaction described in step (1) is 2-120h, preferably 100h.
8. preparation method according to claim 1, which is characterized in that
Preparation by liquid circulation isolated in step (2) for neutral solution in step (1)；
Preferably, the solid in step (2) includes powder.
9. the one-dimensional manganese bioxide material being prepared such as the described in any item preparation methods of claim 1-8；
Preferably, the diameter of the one-dimensional manganese bioxide material is 100-1000nm；
Preferably, the draw ratio of the one-dimensional manganese bioxide material is 2-1000.
10. one-dimensional manganese bioxide material as claimed in claim 9 is in Industrial Catalysis, heavy metal adsorption, battery, super capacitor
The application of device, field of biosensors.
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| CN114700032A (en) * | 2022-03-17 | 2022-07-05 | 中南大学 | Cryptomelane whisker and preparation and application thereof |
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