CN112661189A - Manganese carbonate nano material and preparation method thereof - Google Patents
Manganese carbonate nano material and preparation method thereof Download PDFInfo
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- CN112661189A CN112661189A CN202011566104.0A CN202011566104A CN112661189A CN 112661189 A CN112661189 A CN 112661189A CN 202011566104 A CN202011566104 A CN 202011566104A CN 112661189 A CN112661189 A CN 112661189A
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- manganese carbonate
- permanganate
- precipitate
- nano material
- precursor solution
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- 229940093474 manganese carbonate Drugs 0.000 title claims abstract description 40
- 235000006748 manganese carbonate Nutrition 0.000 title claims abstract description 40
- 239000011656 manganese carbonate Substances 0.000 title claims abstract description 40
- 229910000016 manganese(II) carbonate Inorganic materials 0.000 title claims abstract description 40
- XMWCXZJXESXBBY-UHFFFAOYSA-L manganese(ii) carbonate Chemical compound [Mn+2].[O-]C([O-])=O XMWCXZJXESXBBY-UHFFFAOYSA-L 0.000 title claims abstract description 40
- 239000002086 nanomaterial Substances 0.000 title claims abstract description 30
- 238000002360 preparation method Methods 0.000 title abstract description 14
- 239000002243 precursor Substances 0.000 claims abstract description 27
- 239000002244 precipitate Substances 0.000 claims abstract description 26
- 238000001035 drying Methods 0.000 claims abstract description 25
- 238000004140 cleaning Methods 0.000 claims abstract description 21
- 229920002472 Starch Polymers 0.000 claims abstract description 20
- 235000019698 starch Nutrition 0.000 claims abstract description 20
- 239000008107 starch Substances 0.000 claims abstract description 20
- 239000008367 deionised water Substances 0.000 claims abstract description 12
- 229910021641 deionized water Inorganic materials 0.000 claims abstract description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Chemical compound O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000002105 nanoparticle Substances 0.000 claims abstract description 9
- 238000000034 method Methods 0.000 claims description 15
- 239000012286 potassium permanganate Substances 0.000 claims description 13
- 238000012545 processing Methods 0.000 claims description 11
- JYLNVJYYQQXNEK-UHFFFAOYSA-N 3-amino-2-(4-chlorophenyl)-1-propanesulfonic acid Chemical compound OS(=O)(=O)CC(CN)C1=CC=C(Cl)C=C1 JYLNVJYYQQXNEK-UHFFFAOYSA-N 0.000 claims description 4
- QGZKDVFQNNGYKY-UHFFFAOYSA-O Ammonium Chemical compound [NH4+] QGZKDVFQNNGYKY-UHFFFAOYSA-O 0.000 claims description 4
- 150000003839 salts Chemical class 0.000 claims 1
- 238000005406 washing Methods 0.000 claims 1
- 239000000463 material Substances 0.000 abstract description 7
- 239000002245 particle Substances 0.000 abstract description 6
- 150000002500 ions Chemical class 0.000 abstract description 3
- 239000010406 cathode material Substances 0.000 abstract description 2
- 238000003756 stirring Methods 0.000 description 10
- 238000005303 weighing Methods 0.000 description 7
- 230000009286 beneficial effect Effects 0.000 description 4
- BVKZGUZCCUSVTD-UHFFFAOYSA-L Carbonate Chemical compound [O-]C([O-])=O BVKZGUZCCUSVTD-UHFFFAOYSA-L 0.000 description 3
- 239000003792 electrolyte Substances 0.000 description 3
- 229910001437 manganese ion Inorganic materials 0.000 description 3
- 150000004649 carbonic acid derivatives Chemical class 0.000 description 2
- 238000009826 distribution Methods 0.000 description 2
- 229910052751 metal Inorganic materials 0.000 description 2
- 239000002184 metal Substances 0.000 description 2
- 239000000047 product Substances 0.000 description 2
- HBBGRARXTFLTSG-UHFFFAOYSA-N Lithium ion Chemical compound [Li+] HBBGRARXTFLTSG-UHFFFAOYSA-N 0.000 description 1
- 238000002441 X-ray diffraction Methods 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 239000010405 anode material Substances 0.000 description 1
- BVKZGUZCCUSVTD-UHFFFAOYSA-N carbonic acid Chemical compound OC(O)=O BVKZGUZCCUSVTD-UHFFFAOYSA-N 0.000 description 1
- 239000007795 chemical reaction product Substances 0.000 description 1
- 230000007547 defect Effects 0.000 description 1
- 238000013461 design Methods 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000007599 discharging Methods 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000012467 final product Substances 0.000 description 1
- 238000001027 hydrothermal synthesis Methods 0.000 description 1
- 238000011031 large-scale manufacturing process Methods 0.000 description 1
- 229910001416 lithium ion Inorganic materials 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 238000012986 modification Methods 0.000 description 1
- 230000004048 modification Effects 0.000 description 1
- 150000005837 radical ions Chemical class 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000001878 scanning electron micrograph Methods 0.000 description 1
- 239000000126 substance Substances 0.000 description 1
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Abstract
The invention discloses a manganese carbonate nano material and a preparation method thereof, wherein permanganate and starch are dissolved in deionized water and stirred to obtain a precursor solution; transferring the precursor solution into a reaction kettle, and obtaining a precipitate after reaction treatment; and centrifugally cleaning and drying the precipitate to obtain the manganese carbonate nano material. The preparation method is simple and convenient in preparation process, the material particles are uniformly distributed, the basic composition unit is the nano particles, and the nano particles have certain advantages when being used as the cathode of the ion battery. Can be applied to the work of preparing the rugby-shaped manganese carbonate cathode material.
Description
Technical Field
The invention belongs to the technical field of chemistry, and particularly relates to a manganese carbonate nano material and a preparation method thereof.
Background
Metal carbonates have become a research hotspot in recent years as high-specific-energy negative electrodes with high capacity and low cost. Manganese carbonate, a family of metal carbonates, has been reported to be used in lithium ion battery cathodes and has certain electrochemical properties. However, the regulation of the manganese carbonate micro-nano structure is not widely reported in the aspect of secondary batteries.
Disclosure of Invention
The invention aims to solve the technical problem of providing a manganese carbonate nano material and a preparation method thereof aiming at the defects in the prior art, wherein the manganese carbonate nano material is in an olivary shape, the whole of the olivary manganese carbonate is assembled by nano particles, the manganese carbonate nano material has high specific surface area, can be fully contacted with electrolyte, improves the battery capacity, and the micron-sized olivary structure can ensure the stability of the material in the charging and discharging cycle process.
The invention adopts the following technical scheme:
a manganese carbonate nano material is of an olive-ball structure and is formed by assembling nanoparticles with the size of 1-100 nm.
Specifically, the rugby ball-shaped structure has a dimension in the major axis direction of 1 to 5 μm and a dimension in the minor axis direction of 0.1 to 2 μm.
The other technical scheme of the invention is that the method for preparing the manganese carbonate nano material comprises the steps of dissolving permanganate and starch in deionized water, and stirring to obtain a precursor solution; transferring the precursor solution into a reaction kettle, and obtaining a precipitate after reaction treatment; and centrifugally cleaning and drying the precipitate to obtain the manganese carbonate nano material.
Specifically, the mass ratio of the permanganate to the starch is (1-5): 10.
specifically, the concentration of the starch solution is 1-10 g/L; the concentration of the permanganate is 0.1-1 g/L.
Specifically, the permanganate is any one of potassium permanganate, sodium permanganate, and ammonium permanganate.
Specifically, the precursor solution is transferred into a reaction kettle and reacts for 0.5-24 hours at the temperature of 120-180 ℃ to obtain a precipitate.
Specifically, the centrifugal processing speed is 3000-10000 rpm.
Specifically, the number of cleaning times is 1-3.
Specifically, the drying temperature is 60-100 ℃, and the drying time is 12-24 hours.
Compared with the prior art, the invention has at least the following beneficial effects:
the nanometer manganese carbonate material has nanometer level particle with relatively great specific surface area capable of contacting electrolyte and micron level particle favorable to maintaining stable structure in the circulation process.
Furthermore, the football-shaped structure is not only beneficial to improving the battery capacity, but also beneficial to the stability of the material structure in the circulating process.
A method for preparing manganese carbonate nano material, dissolving permanganate and starch in deionized water, stirring to obtain precursor solution; transferring the precursor solution into a reaction kettle, and obtaining a precipitate after reaction treatment; the precipitate is centrifugally cleaned and dried to obtain the manganese carbonate nano material, the preparation process is simple and convenient, and the particle size distribution of the material is uniform. .
Further, the ratio of potassium permanganate and starch is used for providing a reaction environment containing carbonate ions and manganese ions, and finally the product of manganese carbonate is formed.
Further, the concentration ranges of potassium permanganate and starch are used to provide a reaction environment containing appropriate concentrations of carbonate ions and manganese ions, ultimately forming the product manganese carbonate.
Further, the permanganate is any one of potassium permanganate, sodium permanganate and ammonium permanganate, and can conveniently provide permanganate acid radical ions.
Furthermore, the hydrothermal reaction time and temperature can be set so that substances with poor solubility at normal temperature and normal pressure can be dissolved and recrystallized to synthesize the rugby-shaped manganese carbonate precursor.
Furthermore, the centrifugal processing speed is 3000-10000 rpm, which is beneficial to collecting reaction products.
And further, removing residual carbonate ions and manganese ions by cleaning for 1-3 times.
Further, the drying temperature is 60-100 ℃, and the drying time is 12-24 hours, so that the final product manganese carbonate is obtained.
In conclusion, the preparation process is simple and convenient, the particle size distribution of the material is uniform, the basic composition unit is the nano particles, and the preparation method has certain advantages when being used as the cathode of the ion battery. Can be applied to the work of preparing the rugby-shaped manganese carbonate cathode material.
The technical solution of the present invention is further described in detail by the accompanying drawings and embodiments.
Drawings
FIG. 1 is an XRD pattern of a sample prepared in the present invention;
FIG. 2 is an SEM image of a sample prepared in the present invention;
FIG. 3 is a schematic diagram of the preparation process of the material of the present invention.
Detailed Description
It will be understood that the terms "comprises" and/or "comprising," when used in this specification and the appended claims, specify the presence of stated features, integers, steps, operations, elements, and/or components, but do not preclude the presence or addition of one or more other features, integers, steps, operations, elements, components, and/or groups thereof.
It is also to be understood that the terminology used in the description of the invention herein is for the purpose of describing particular embodiments only and is not intended to be limiting of the invention. As used in the specification of the present invention and the appended claims, the singular forms "a," "an," and "the" are intended to include the plural forms as well, unless the context clearly indicates otherwise.
It should be further understood that the term "and/or" as used in this specification and the appended claims refers to and includes any and all possible combinations of one or more of the associated listed items.
Various structural schematics according to the disclosed embodiments of the invention are shown in the drawings. The figures are not drawn to scale, wherein certain details are exaggerated and possibly omitted for clarity of presentation. The shapes of various regions, layers and their relative sizes and positional relationships shown in the drawings are merely exemplary, and deviations may occur in practice due to manufacturing tolerances or technical limitations, and a person skilled in the art may additionally design regions/layers having different shapes, sizes, relative positions, according to actual needs.
Referring to fig. 1 and 2, the present invention provides a manganese carbonate nanomaterial, wherein the manganese carbonate nanomaterial is in the form of rugby, the dimension in the major axis direction is 1-5 μm, the dimension in the minor axis direction is 0.1-2 μm, and the rugby manganese carbonate is integrally assembled from nanoparticles, and the size of the nanoparticles is 1-100 nm.
Referring to fig. 3, the method for preparing a manganese carbonate nanomaterial of the present invention includes the following steps:
s1, dissolving a certain amount of permanganate and starch in deionized water, and uniformly stirring to obtain a precursor solution;
the concentration of the starch solution is 1-10 g/L; the concentration of the permanganate is 0.1-1 g/L; the mass ratio of the permanganate to the starch is (1-5): 10.
the permanganate is any one of potassium permanganate, sodium permanganate and ammonium permanganate.
S2, transferring the precursor solution into a reaction kettle, and reacting at the temperature of 120-180 ℃ for 0.5-24 h to obtain a precipitate;
and S3, centrifugally cleaning and drying the precipitate obtained in the step S2 to obtain the manganese carbonate nano material.
The centrifugal processing speed is 3000-10000 rpm, the cleaning times are 1-3 times, the drying temperature is 60-100 ℃, and the time is 12-24 hours.
In order to make the objects, technical solutions and advantages of the embodiments of the present invention clearer, the technical solutions in the embodiments of the present invention will be clearly and completely described below with reference to the drawings in the embodiments of the present invention, and it is obvious that the described embodiments are some, but not all, embodiments of the present invention. The components of the embodiments of the present invention generally described and illustrated in the figures herein may be arranged and designed in a wide variety of different configurations. Thus, the following detailed description of the embodiments of the present invention, presented in the figures, is not intended to limit the scope of the invention, as claimed, but is merely representative of selected embodiments of the invention. All other embodiments, which can be derived by a person skilled in the art from the embodiments given herein without making any creative effort, shall fall within the protection scope of the present invention.
Example 1
Weighing 0.2g of potassium permanganate and 1g of starch, dissolving in 200ml of deionized water, and uniformly stirring to obtain a precursor solution;
transferring the precursor solution into a reaction kettle, and reacting at 160 ℃ for 12h to obtain a precipitate;
and centrifugally cleaning and drying the precipitate to obtain the manganese carbonate nano material, wherein the centrifugal processing speed is 3000rpm, the cleaning times are 1 time, the drying temperature is 60 ℃, and the time is 12 hours.
Example 2
Weighing 0.2g of potassium permanganate and 1g of starch, dissolving in 200ml of deionized water, and uniformly stirring to obtain a precursor solution;
transferring the precursor solution into a reaction kettle, and reacting at 160 ℃ for 6 hours to obtain a precipitate;
and centrifugally cleaning and drying the precipitate to obtain the manganese carbonate nano material, wherein the centrifugal processing speed is 5000rpm, the cleaning times are 1 time, the drying temperature is 60 ℃, and the time is 14 hours.
Example 3
Weighing 0.2g of potassium permanganate and 1g of starch, dissolving in 200ml of deionized water, and uniformly stirring to obtain a precursor solution;
transferring the precursor solution into a reaction kettle, and reacting at 180 ℃ for 12h to obtain a precipitate;
and (3) centrifugally cleaning and drying the precipitate to obtain the manganese carbonate nano material, wherein the centrifugal processing speed is 6000rpm, the cleaning times are 2 times, the drying temperature is 70 ℃, and the time is 16 hours.
Example 4
Weighing 0.2g of potassium permanganate and 1g of starch, dissolving in 200ml of deionized water, and uniformly stirring to obtain a precursor solution;
transferring the precursor solution into a reaction kettle, and reacting at 180 ℃ for 6 hours to obtain a precipitate;
and (3) centrifugally cleaning and drying the precipitate to obtain the manganese carbonate nano material, wherein the centrifugal processing speed is 6000rpm, the cleaning times are 2 times, the drying temperature is 70 ℃, and the time is 18 hours.
Example 5
Weighing 0.1g of potassium permanganate and 1g of starch, dissolving in 200ml of deionized water, and uniformly stirring to obtain a precursor solution;
transferring the precursor solution into a reaction kettle, and reacting at 180 ℃ for 6 hours to obtain a precipitate;
and centrifugally cleaning and drying the precipitate to obtain the manganese carbonate nano material, wherein the centrifugal processing speed is 8000rpm, the cleaning times are 2 times, the drying temperature is 80 ℃, and the time is 20 hours.
Example 6
Weighing 0.1g of potassium permanganate and 1g of starch, dissolving in 200ml of deionized water, and uniformly stirring to obtain a precursor solution;
transferring the precursor solution into a reaction kettle, and reacting at 160 ℃ for 6 hours to obtain a precipitate;
and centrifugally cleaning and drying the precipitate to obtain the manganese carbonate nano material, wherein the centrifugal processing speed is 9000rpm, the cleaning times are 3 times, the drying temperature is 90 ℃, and the time is 22 hours.
Example 7
Weighing 0.1g of potassium permanganate and 1g of starch, dissolving in 200ml of deionized water, and uniformly stirring to obtain a precursor solution;
transferring the precursor solution into a reaction kettle, and reacting at 160 ℃ for 12h to obtain a precipitate;
and centrifugally cleaning and drying the precipitate to obtain the manganese carbonate nano material, wherein the centrifugal processing speed is 10000rpm, the cleaning times are 3 times, the drying temperature is 100 ℃, and the time is 24 hours.
In conclusion, the manganese carbonate nano material and the preparation method thereof have the advantages of simple preparation process and mild preparation conditions, are suitable for large-scale production, and are suitable for being used as the anode material of the ion battery, the micron-sized rugby-shaped carbonic acid assembled by the nano-sized particles can fully contact electrolyte to exert high-efficiency specific capacity, and meanwhile, the micron-sized structure can ensure the stability in the circulation process.
The above-mentioned contents are only for illustrating the technical idea of the present invention, and the protection scope of the present invention is not limited thereby, and any modification made on the basis of the technical idea of the present invention falls within the protection scope of the claims of the present invention.
Claims (10)
1. The manganese carbonate nano material is characterized by being of an olive-shaped structure and assembled by nano particles with the size of 1-100 nm.
2. The manganese carbonate nanomaterial according to claim 1, wherein the rugby-ball structure has a major axis dimension of 1 to 5 μm and a minor axis dimension of 0.1 to 2 μm.
3. The method for preparing the manganese carbonate nano material of claim 1 is characterized in that permanganate and starch are dissolved in deionized water and stirred to obtain a precursor solution; transferring the precursor solution into a reaction kettle, and obtaining a precipitate after reaction treatment; and centrifugally cleaning and drying the precipitate to obtain the manganese carbonate nano material.
4. The method according to claim 3, wherein the mass ratio of the permanganate to the starch is (1-5): 10.
5. the method according to claim 3, wherein the concentration of the starch solution is 1-10 g/L; the concentration of the permanganate is 0.1-1 g/L.
6. The method of claim 3, wherein the permanganate salt is any one of potassium permanganate, sodium permanganate, and ammonium permanganate.
7. The method as claimed in claim 3, wherein the precursor solution is transferred into a reaction kettle and reacts at 120-180 ℃ for 0.5-24 h to obtain a precipitate.
8. The method according to claim 3, wherein the centrifugal processing speed is 3000 to 10000 rpm.
9. The method according to claim 3, wherein the number of washing is 1 to 3.
10. The method according to claim 3, wherein the drying temperature is 60-100 ℃ and the drying time is 12-24 h.
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN113725423A (en) * | 2021-09-17 | 2021-11-30 | 陕西科技大学 | MnCO3/MoS2Heterojunction composite material and preparation method and application thereof |
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