CN114180632A - Method for rapidly preparing porous trimanganese tetroxide nano material with large specific surface area in one step - Google Patents
Method for rapidly preparing porous trimanganese tetroxide nano material with large specific surface area in one step Download PDFInfo
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- CN114180632A CN114180632A CN202210056862.0A CN202210056862A CN114180632A CN 114180632 A CN114180632 A CN 114180632A CN 202210056862 A CN202210056862 A CN 202210056862A CN 114180632 A CN114180632 A CN 114180632A
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- AMWRITDGCCNYAT-UHFFFAOYSA-L hydroxy(oxo)manganese;manganese Chemical compound [Mn].O[Mn]=O.O[Mn]=O AMWRITDGCCNYAT-UHFFFAOYSA-L 0.000 title claims abstract description 100
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 55
- 238000000034 method Methods 0.000 title claims abstract description 46
- CESXSDZNZGSWSP-UHFFFAOYSA-L manganese(2+);diacetate;tetrahydrate Chemical compound O.O.O.O.[Mn+2].CC([O-])=O.CC([O-])=O CESXSDZNZGSWSP-UHFFFAOYSA-L 0.000 claims abstract description 21
- 229940082328 manganese acetate tetrahydrate Drugs 0.000 claims abstract description 18
- PWHULOQIROXLJO-UHFFFAOYSA-N Manganese Chemical compound [Mn] PWHULOQIROXLJO-UHFFFAOYSA-N 0.000 claims abstract description 16
- 229910052748 manganese Inorganic materials 0.000 claims abstract description 14
- 239000011572 manganese Substances 0.000 claims abstract description 14
- 238000001354 calcination Methods 0.000 claims description 9
- 239000000463 material Substances 0.000 abstract description 17
- 239000002994 raw material Substances 0.000 abstract description 6
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 abstract description 6
- PTFCDOFLOPIGGS-UHFFFAOYSA-N Zinc dication Chemical compound [Zn+2] PTFCDOFLOPIGGS-UHFFFAOYSA-N 0.000 abstract description 4
- QHGJSLXSVXVKHZ-UHFFFAOYSA-N dilithium;dioxido(dioxo)manganese Chemical compound [Li+].[Li+].[O-][Mn]([O-])(=O)=O QHGJSLXSVXVKHZ-UHFFFAOYSA-N 0.000 abstract description 4
- 230000007613 environmental effect Effects 0.000 abstract description 4
- 238000004519 manufacturing process Methods 0.000 abstract description 4
- 238000005516 engineering process Methods 0.000 abstract description 2
- 238000011031 large-scale manufacturing process Methods 0.000 abstract 1
- 239000011148 porous material Substances 0.000 abstract 1
- 239000000047 product Substances 0.000 description 18
- GEYXPJBPASPPLI-UHFFFAOYSA-N manganese(III) oxide Inorganic materials O=[Mn]O[Mn]=O GEYXPJBPASPPLI-UHFFFAOYSA-N 0.000 description 17
- 238000002360 preparation method Methods 0.000 description 14
- 230000000052 comparative effect Effects 0.000 description 8
- 238000010438 heat treatment Methods 0.000 description 7
- 239000002105 nanoparticle Substances 0.000 description 6
- 238000001878 scanning electron micrograph Methods 0.000 description 6
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 description 4
- 238000002441 X-ray diffraction Methods 0.000 description 4
- 238000000026 X-ray photoelectron spectrum Methods 0.000 description 4
- 239000013078 crystal Substances 0.000 description 4
- 230000000694 effects Effects 0.000 description 4
- 235000006748 manganese carbonate Nutrition 0.000 description 4
- 239000011656 manganese carbonate Substances 0.000 description 4
- 229940093474 manganese carbonate Drugs 0.000 description 4
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 description 4
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 description 4
- 238000002159 adsorption--desorption isotherm Methods 0.000 description 3
- 238000010586 diagram Methods 0.000 description 3
- 239000012535 impurity Substances 0.000 description 3
- PPNAOCWZXJOHFK-UHFFFAOYSA-N manganese(2+);oxygen(2-) Chemical compound [O-2].[Mn+2] PPNAOCWZXJOHFK-UHFFFAOYSA-N 0.000 description 3
- VASIZKWUTCETSD-UHFFFAOYSA-N manganese(II) oxide Inorganic materials [Mn]=O VASIZKWUTCETSD-UHFFFAOYSA-N 0.000 description 3
- 239000000126 substance Substances 0.000 description 3
- 230000005540 biological transmission Effects 0.000 description 2
- 239000006227 byproduct Substances 0.000 description 2
- 229910002092 carbon dioxide Inorganic materials 0.000 description 2
- 239000001569 carbon dioxide Substances 0.000 description 2
- 238000006555 catalytic reaction Methods 0.000 description 2
- 238000006243 chemical reaction Methods 0.000 description 2
- 150000002696 manganese Chemical class 0.000 description 2
- 229940099596 manganese sulfate Drugs 0.000 description 2
- 235000007079 manganese sulphate Nutrition 0.000 description 2
- 239000011702 manganese sulphate Substances 0.000 description 2
- SQQMAOCOWKFBNP-UHFFFAOYSA-L manganese(II) sulfate Chemical compound [Mn+2].[O-]S([O-])(=O)=O SQQMAOCOWKFBNP-UHFFFAOYSA-L 0.000 description 2
- 239000002245 particle Substances 0.000 description 2
- 229910052596 spinel Inorganic materials 0.000 description 2
- 239000011029 spinel Substances 0.000 description 2
- QTBSBXVTEAMEQO-UHFFFAOYSA-M Acetate Chemical compound CC([O-])=O QTBSBXVTEAMEQO-UHFFFAOYSA-M 0.000 description 1
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000003917 TEM image Methods 0.000 description 1
- DJTZIDSZSYWGKR-UHFFFAOYSA-N acetic acid tetrahydrate Chemical compound O.O.O.O.CC(O)=O DJTZIDSZSYWGKR-UHFFFAOYSA-N 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003990 capacitor Substances 0.000 description 1
- 238000007796 conventional method Methods 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 239000003792 electrolyte Substances 0.000 description 1
- 238000004146 energy storage Methods 0.000 description 1
- 150000004679 hydroxides Chemical class 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 229940071125 manganese acetate Drugs 0.000 description 1
- 150000002697 manganese compounds Chemical class 0.000 description 1
- UOGMEBQRZBEZQT-UHFFFAOYSA-L manganese(2+);diacetate Chemical compound [Mn+2].CC([O-])=O.CC([O-])=O UOGMEBQRZBEZQT-UHFFFAOYSA-L 0.000 description 1
- WPBNNNQJVZRUHP-UHFFFAOYSA-L manganese(2+);methyl n-[[2-(methoxycarbonylcarbamothioylamino)phenyl]carbamothioyl]carbamate;n-[2-(sulfidocarbothioylamino)ethyl]carbamodithioate Chemical compound [Mn+2].[S-]C(=S)NCCNC([S-])=S.COC(=O)NC(=S)NC1=CC=CC=C1NC(=S)NC(=O)OC WPBNNNQJVZRUHP-UHFFFAOYSA-L 0.000 description 1
- 229910052751 metal Inorganic materials 0.000 description 1
- 239000002184 metal Substances 0.000 description 1
- 238000002156 mixing Methods 0.000 description 1
- 230000007935 neutral effect Effects 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002243 precursor Substances 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 238000005979 thermal decomposition reaction Methods 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
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- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01G—COMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
- C01G45/00—Compounds of manganese
- C01G45/02—Oxides; Hydroxides
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B82—NANOTECHNOLOGY
- B82Y—SPECIFIC USES OR APPLICATIONS OF NANOSTRUCTURES; MEASUREMENT OR ANALYSIS OF NANOSTRUCTURES; MANUFACTURE OR TREATMENT OF NANOSTRUCTURES
- B82Y40/00—Manufacture or treatment of nanostructures
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/12—Surface area
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- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Organic Chemistry (AREA)
- Nanotechnology (AREA)
- Inorganic Chemistry (AREA)
- Physics & Mathematics (AREA)
- Condensed Matter Physics & Semiconductors (AREA)
- General Physics & Mathematics (AREA)
- Manufacturing & Machinery (AREA)
- Crystallography & Structural Chemistry (AREA)
- Inorganic Compounds Of Heavy Metals (AREA)
Abstract
The invention discloses a method for rapidly preparing a porous trimanganese tetroxide nano material with a large specific surface area by one step, which is implemented by the following steps: in the air atmosphere, manganese acetate tetrahydrate is used as a manganese source, and the manganese acetate tetrahydrate is calcined for a period of time to obtain a porous mangano-manganic oxide nano material with a large specific surface area; the method is a brand-new method technology for quickly and simply preparing the porous trimanganese tetroxide nano material with large specific surface area, the obtained trimanganese tetroxide material has small size, rich pore structure and large specific surface area, is expected to be used as a preferred material for preparing lithium manganate and is expected to be applied to a water system zinc ion battery to improve the electrochemical performance of the water system zinc ion battery; the method has the advantages of cheap and easily-obtained raw materials, convenient operation, low production cost, environmental protection, no pollution, high product purity and potential for mass large-scale production.
Description
Technical Field
The invention belongs to the technical field of manganese compound preparation, and particularly relates to a method for rapidly preparing a porous trimanganese tetroxide nano material with a large specific surface area in one step.
Background
Manganous manganic oxide is an important manganese oxide material and is a mixed valence oxide of manganese, the valence of manganese element is +3 valence and +2 valence, and the manganous manganic oxide and manganous manganic oxide are considered to be formed by mixing two crystal structures of manganous oxide and manganous oxide. Manganomanganic oxide has a spinel structure with manganese 3 and manganese 2 occupying octahedral and tetrahedral sites of the spinel structure, respectively. Due to the special structure, the manganese oxide has the characteristics of low price, environmental friendliness, abundant reserves, good electrochemical performance in neutral/alkaline electrolyte and the like, and the mangano-manganic oxide plays a very important role in the aspects of catalysis, preparation of lithium manganate serving as a positive material of a super capacitor and a lithium ion battery, preparation of soft magnetic ferrite and the like, and is widely concerned by researchers in application;
the currently reported preparation methods of the trimanganese tetroxide nano material mainly comprise a high-valence manganese oxide method, a manganese salt method, a manganese carbonate method and a metal manganese method. The high valence manganese oxide method has strict technological requirements, high roasting temperature, poor physical properties of the prepared material and the like, and limits the wide application of the method. The manganese salt method has the advantages of high purity of prepared products, good activity and the like, but has the defects of by-products, high production cost, non-green and non-environmental protection. Manganese carbonate, manganese sulfate and manganese oxide are mostly used as raw materials in the manganese carbonate method, and the manganese carbonate, manganese sulfate and manganese oxide are roasted and oxidized at high temperature to generate trimanganese tetroxide, so that the preparation conditions are harsh, the specific surface area is low and the like. The manganese metal method has low technical content and easy operation, but has high production cost, uneven granularity of prepared samples, larger grain diameter and generally higher content of various impurities. In a word, the existing method for preparing the manganous-manganic oxide material has the problems of complex production process flow, insufficient product purity, poor physical and chemical activity and the like. And reports about the porous trimanganese tetroxide nano material with large specific surface area are less, and reports about the simple and rapid preparation of the porous trimanganese tetroxide nano material with large specific surface area by a one-step method are less. Therefore, how to rapidly, simply and industrially prepare the porous trimanganese tetroxide nano material with large specific surface area is particularly important.
The invention aims to provide a novel preparation method of a large-specific-surface-area porous manganous-manganic oxide nano material, and mainly solves the problems of long and complicated preparation process flow, low purity of prepared products, poor physical and chemical activity caused by large grain size of the products and the like in the conventional method, so that the method for rapidly preparing the large-specific-surface-area porous manganous-manganic oxide nano material in one step is provided for the fields of catalysis and energy storage, and the rapid development of the manganous-manganic oxide nano material in the fields is promoted.
Disclosure of Invention
The invention aims to provide a method for rapidly preparing a porous trimanganese tetroxide nano material with a large specific surface area by one step, and solves the problems of poor physical and chemical activity and the like caused by long and complicated preparation process flow, low purity of prepared products, large grain size of the products and the like in the existing method.
The technical scheme adopted by the invention is that the method for rapidly preparing the porous trimanganese tetroxide nano material with large specific surface area by one step is implemented by the following steps: in the air atmosphere, manganese acetate tetrahydrate is used as a manganese source, and the manganese acetate tetrahydrate is calcined for a period of time to obtain the porous mangano-manganic oxide nano material with large specific surface area.
The invention is also characterized in that:
wherein the calcination temperature is 400-500 ℃;
wherein the calcination time is 1-6 h;
wherein the heating rate during calcination is 5 ℃/min.
The invention has the beneficial effects that:
(1) according to the method, by utilizing the characteristics that the tetrahydrate manganese acetate is easy to remove water molecules and carbon dioxide gas in the thermal decomposition process and the divalent manganese is unstable and easy to oxidize in the air under the heated condition, the tetrahydrate manganese acetate is calcined in the air atmosphere to obtain the porous trimanganese tetroxide nano material with the large specific surface area, and a brand new method technology for simply and quickly preparing the porous trimanganese tetroxide nano material with the large specific surface area is provided;
(2) the porous trimanganese tetroxide nanoparticles with large specific surface area prepared by the method have small size and porous structure, and the specific surface area is as high as 190m2The lithium manganate is expected to be used as a preferred material for preparing lithium manganate and is expected to be applied to a water-system zinc ion battery to improve the electrochemical performance of the water-system zinc ion battery;
(3) the method has the advantages of cheap and easily-obtained raw materials, simple preparation process and low cost, and the obtained mangano-manganic oxide nano material has high purity, small size and large specific surface area;
(4) the method has the advantages of controllable material preparation process, environmental protection, no pollution, no byproduct generation, high yield and large-scale industrial production.
Drawings
FIG. 1 is an X-ray diffraction pattern of a manganomanganic oxide nano material prepared in example 1 in the one-step rapid preparation method of a porous manganomanganic oxide nano material with a large specific surface area;
FIG. 2 is an X-ray photoelectron spectrum of Mn2p of the mangano-manganic oxide nano-material prepared in example 1 in the method for rapidly preparing the porous mangano-manganic oxide nano-material with large specific surface area by one step;
FIG. 3 is an X-ray photoelectron spectrum of Mn3s of the manganomanganic oxide nano-material prepared in example 1 in the method for rapidly preparing the porous manganomanganic oxide nano-material with large specific surface area by one step;
FIG. 4 shows the N of the manganous-manganic oxide nano material prepared in example 1 in the method for rapidly preparing the porous manganous-manganic oxide nano material with large specific surface area by one step2Adsorption-desorption isotherm diagram;
FIG. 5 is a scanning electron microscope photomicrograph showing the low magnification of the manganic oxide nano material prepared in example 1 in the method for rapidly preparing the porous manganic oxide nano material with large specific surface area by one step;
FIG. 6 is a high-power scanning electron microscope photograph of the mangano-manganic oxide nano-material prepared in example 1 in the method for rapidly preparing the porous mangano-manganic oxide nano-material with large specific surface area by one step;
FIG. 7 is a transmission electron microscope photograph of the manganomanganic oxide nano-material prepared in example 1 in the method for rapidly preparing the porous manganomanganic oxide nano-material with large specific surface area by one step;
FIG. 8 is a scanning electron microscope photograph of the mangano-manganic oxide nano-material prepared in example 2 in the method for rapidly preparing the porous mangano-manganic oxide nano-material with large specific surface area by one step;
FIG. 9 is a scanning electron microscope photograph of the mangano-manganic oxide nano-material prepared in example 3 in the method for rapidly preparing the porous mangano-manganic oxide nano-material with large specific surface area by one step;
FIG. 10 is a scanning electron micrograph of untreated manganic acetate tetrahydrate in comparative example 1 in a one-step rapid preparation method of a porous mangano-manganic oxide nano material with a large specific surface area;
FIG. 11 is a high-power scanning electron micrograph of untreated manganous acetate tetrahydrate in comparative example 1 in the method for rapidly preparing the porous manganous manganic oxide nano material with the large specific surface area in one step;
FIG. 12 is a scanning electron microscope photograph of the material prepared in comparative example 2 in the method for rapidly preparing the porous trimanganese tetroxide nano-material with large specific surface area by one step;
FIG. 13 is a scanning electron microscope photograph of the material prepared in comparative example 3 in the method for rapidly preparing the porous trimanganese tetroxide nano-material with large specific surface area by one step;
FIG. 14 is an X-ray diffraction pattern of the material prepared in comparative example 3 in the one-step rapid preparation method of the large-specific-surface-area porous trimanganese tetroxide nano-material of the invention.
Detailed Description
The present invention will be described in detail below with reference to the accompanying drawings and specific embodiments.
The raw material of manganese acetate tetrahydrate is cheap and easy to obtain, has a large lamellar structure, is easy to decompose by heating to remove water molecules and carbon dioxide gas, and is easy to form a porous structure, and the porous structure generally has a large specific surface area, has a large contact area as a reaction object, and is easy to effectively contact other materials to generate physical and chemical reactions; the invention utilizes the characteristics that manganese acetate tetrahydrate easily loses crystal water at high temperature, acetate is easily decomposed by heating, and bivalent manganese is easily oxidized in air due to unstable heating, takes manganese acetate tetrahydrate as a manganese source and a precursor, and prepares the porous trimanganese tetroxide nano material with large specific surface area simply and quickly by a one-step pyrolysis method.
The invention provides a method for rapidly preparing a porous trimanganese tetroxide nano material with a large specific surface area in one step, which comprises the steps of taking manganese acetate tetrahydrate as a manganese source in an air atmosphere, and directly calcining the manganese acetate tetrahydrate at 400-500 ℃ for 1-6 hours at a heating rate of 5 ℃/min to obtain the porous trimanganese tetroxide nano material with the large specific surface area.
The manganese acetate tetrahydrate used in the following examples may be an unground raw material block, a ground powder, or manganese acetate containing no crystal water.
Example 1
Preparing a porous manganous-manganic oxide nano material with a large specific surface area:
in the air atmosphere, manganese acetate tetrahydrate is used as a manganese source, and the manganese source is directly calcined at 400 ℃ for 3 hours at the heating rate of 5 ℃/min to obtain the product.
Respectively adopting an X-ray diffractometer, an X-ray photoelectron spectrum, a scanning electron microscope and N to obtain a product2The adsorption-desorption isotherm diagram, the scanning electron microscope and the transmission electron microscope are characterized, and the results are shown in the figures 1-7;
as can be seen from the X-ray diffraction pattern of fig. 1, the obtained product is trimanganese tetroxide, the peak type sharp intensity is high, no diffraction peak of impurities such as other oxides or hydroxides is detected, and the product is proved to have high purity, no other impurity phase exists, and the product is high-purity trimanganese tetroxide with excellent crystallinity;
the X-ray photoelectron spectra of fig. 2 and 3 further show that the prepared material is trimanganese tetroxide;
n of FIG. 42The adsorption-desorption isotherm diagram shows that the prepared manganomanganic oxide has high specific surface area which is 190m2/g;
The scanning electron micrographs of fig. 5 and 6 show that the obtained manganomanganic oxide material has a small size, a three-dimensional porous structure with self-accumulated nanoparticles and good dispersibility;
as can be seen from the transmission electron micrograph of FIG. 7, the obtained trimanganese tetroxide nanoparticles have small size, nonuniform particle size and obvious porous structure. In conclusion, the material prepared by the one-step method is a porous trimanganese tetroxide nano material with a large specific surface area.
Example 2
Preparing a porous manganous-manganic oxide nano material with a large specific surface area:
manganese acetate tetrahydrate is used as a manganese source in an air atmosphere, the manganese acetate tetrahydrate is directly calcined at 400 ℃ for 6 hours at the heating rate of 5 ℃/min, trimanganese tetroxide nanoparticles are also prepared, and the scanning electron microscope photo of the product is shown in figure 8.
Example 3
Preparing a porous manganous-manganic oxide nano material with a large specific surface area:
manganese acetate tetrahydrate is used as a manganese source in an air atmosphere, the manganese acetate tetrahydrate is directly calcined at the temperature rise rate of 5 ℃/min for 1 hour at the temperature of 500 ℃, manganomanganic oxide nano particles are also prepared, and a scanning electron microscope photo of the product is shown in figure 9.
Comparative example 1
The other steps are the same as example 1, except that the material is not calcined, and scanning electron micrographs of the material are respectively shown in fig. 10 and 11, which shows that the raw material manganese acetate tetrahydrate has a large lamellar structure.
Comparative example 2
The other steps were the same as in example 1 except that calcination was carried out at 300 ℃ for 2 hours; the scanning electron micrograph of the product is shown in fig. 12, and has a large bulk structure.
Comparative example 3
The other steps were the same as in example 1 except that calcination was carried out at 300 ℃ for 6 hours; the scanning electron micrograph of the product is shown in fig. 13, and the product has a loose porous structure assembled by nano particles and smaller particle size; x-ray diffraction analysis is carried out on the product, as can be seen from figure 14, the main crystal phase of the product is manganous-manganic oxide, a small amount of manganous oxide phase exists, and the prepared manganous-manganic oxide nano material has low purity and exists in a mixed phase.
Claims (4)
1. The method for rapidly preparing the porous trimanganese tetroxide nano-material with large specific surface area in one step is characterized by comprising the following steps: in the air atmosphere, manganese acetate tetrahydrate is used as a manganese source, and the manganese acetate tetrahydrate is calcined for a period of time to obtain the porous mangano-manganic oxide nano material with large specific surface area.
2. The method for rapidly preparing the porous trimanganese tetroxide nanomaterial with large specific surface area in one step according to claim 1, wherein the calcination temperature is 400-500 ℃.
3. The method for rapidly preparing the porous trimanganese tetroxide nanomaterial with large specific surface area in one step according to claim 1, wherein the calcination time is 1-6 h.
4. The method for rapidly preparing the porous trimanganese tetroxide nanomaterial with large specific surface area in one step according to claim 1, wherein the temperature rise rate during the calcination is 5 ℃/min.
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