CN104512932A - Preparation method of mesoporous manganic manganous oxide - Google Patents
Preparation method of mesoporous manganic manganous oxide Download PDFInfo
- Publication number
- CN104512932A CN104512932A CN201310446901.9A CN201310446901A CN104512932A CN 104512932 A CN104512932 A CN 104512932A CN 201310446901 A CN201310446901 A CN 201310446901A CN 104512932 A CN104512932 A CN 104512932A
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- CN
- China
- Prior art keywords
- mesoporous
- preparation
- ctab
- trimanganese tetroxide
- manganous oxide
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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
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2002/00—Crystal-structural characteristics
- C01P2002/70—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data
- C01P2002/72—Crystal-structural characteristics defined by measured X-ray, neutron or electron diffraction data by d-values or two theta-values, e.g. as X-ray diagram
-
- 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
-
- 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
- C01P2006/16—Pore diameter
Abstract
The invention provides a preparation method of mesoporous manganic manganous oxide. The preparation method comprises the following steps: weighing a certain amount of CTAB, dissolving CTAB into distilled water, stirring to disperse CTAB, adding a Mn(NO3)2 solution with a concentration of 50 wt% under stirring, keeping on stirring, adjusting the pH value by a NaOH solution, performing aging for 3 hours at a temperature of 90 DEG C, washing the product by hot water, subjecting the product to suction filtration, drying the product at a temperature of 90 DEG C for 6 hours, and burning the product at a temperature of 400-600 DEG C so as to obtain the mesoporous manganic manganous oxide. Through a great number of experiments, a cationic surfactant CTAB is taken as the template to prepare manganic manganous oxide with a mesoporous structure, and the mesoporous manganic manganous oxide is suitable for being taken as a high activity catalyst. The prepared material has a mesoporous structure and a large specific surface area, and the mesoporous manganic manganous oxide has a high catalytic oxidizing activity on propane. The preparation method has the advantages of simple preparation technology and equipment, convenient operation, low cost, low energy consumption, and no pollution, and thus has a very good industrialization prospect.
Description
Technical field
The present invention relates to pharmaceutical field, especially relate to a kind of preparation method of mesoporous trimanganese tetroxide.
Background technology
Trimanganese tetroxide is a kind of important chemical materials, be widely used in electrode materials, volatile organic compounds redox reaction and prepare soft magnetic manganese-zinc ferrite.
At present, the preparation method of trimanganese tetroxide mainly contains roasting method, spray pyrolysis, combustion method, manganese salt (or Mn2+) method, manganese metal (powder, grain, sheet) method etc.All there is different defects in aforesaid method: as energy consumption is large, production cost is high; Production process produces waste, secondary treatment difficulty; Containing partial impurities in product; Specific surface area is relatively little.Chinese patent ZL200710179579.2 discloses a kind of preparation method of trimanganese tetroxide, they adopt the scavenging solution-manganese sulfate solution of manganese ore leach liquor to be raw material, precipitation agent is made with carbonate or supercarbonate, the mn ion of the solution in manganous sulfate is precipitated as manganous carbonate throw out, with air or oxygen as oxygenant, under 120 DEG C-800 DEG C and thermal decomposition time are the condition of 0.1-30 hour, obtained the mixture of manganese by oxidation.The mixture of manganese roasting 0.01-10 hour at 800 DEG C-1200 DEG C is obtained trimanganese tetroxide.We adopt a kind of condition more gentle, the more simple method of processing unit, with cationic surfactant cetyl trimethylammonium bromide (CTAB) for template, the manganic compound adopting relative low price is presoma, prepared trimanganese tetroxide, it has reacted good katalysis to oxidation of propane.
Summary of the invention
The invention provides a kind of preparation method of mesoporous trimanganese tetroxide.
For realizing above-mentioned goal of the invention, the embodiment that the present invention takes is as follows:
A kind of mesoporous trimanganese tetroxide, the aperture of described mesoporous trimanganese tetroxide is 12.6nm, and specific surface area is 37m
2/ g.
A preparation method for mesoporous trimanganese tetroxide, concrete preparation process is as follows: under normal temperature, takes a certain amount of CTAB and is dissolved in distilled water, and vigorous stirring is to disperseing completely; 50wt%Mn (NO is added under continuing stirring
3)
2solution, continues to stir 30min, obtains suspension liquid, 90 DEG C of aging 3h, hot wash, suction filtration, 90 DEG C of dry 6h, roasting for some time at temperature 400 DEG C-600 DEG C, prepare mesoporous trimanganese tetroxide by NaOH solution after regulating pH.
Described CTAB and Mn (NO
3)
2mol ratio be 3:5.
The concentration of NaOH solution is 0.2mol/L, regulates pH=9.
Maturing temperature is 400 DEG C, and roasting time is 4h.
The invention has the beneficial effects as follows: the present invention, by lot of experiments, adopts cationic surfactant CTAB to be template, prepares the trimanganese tetroxide with meso-hole structure, be applicable to be used as high activated catalyst.Prepared material all has meso-hole structure and higher specific surface area, and mesoporous trimanganese tetroxide has high catalytic oxidation activity to propane.The method preparation technology and equipment are simple, and easy to operate, cost is low, less energy-consumption, pollution-free, have good industrial prospect.
Accompanying drawing explanation
Fig. 1 is XRD spectra and the Mn of the mesoporous trimanganese tetroxide prepared in embodiment
3o
4standard diffraction spectrogram.
Embodiment
Below in conjunction with embodiment, to according to embodiment provided by the invention, details are as follows:
Embodiment
Under normal temperature, the CTAB taking 6mmol is dissolved in 200ml distilled water, and vigorous stirring is to disperseing completely; 3.6ml50wt%Mn (NO is added under continuing stirring
3)
2solution, continue to stir 30min, suspension liquid is obtained after regulating pH=9 with 0.2mol/LNaOH solution, 90 DEG C of aging 3h, hot wash, suction filtration, 90 DEG C of dry 6h, at temperature 400 DEG C, roasting 4h roasting process temperature rise rate is 2 DEG C/min, prepares mesoporous trimanganese tetroxide, the XRD spectra of the mesoporous trimanganese tetroxide of preparation and Mn
3o
4standard diffraction spectrogram as shown in Figure 1.
Above one embodiment of the present of invention have been described in detail, but described content being only preferred embodiment of the present invention, can not being considered to for limiting practical range of the present invention.All equalizations done according to the present patent application scope change and improve, and all should still belong within patent covering scope of the present invention.
Claims (5)
1. a mesoporous trimanganese tetroxide, is characterized in that: the aperture of described mesoporous trimanganese tetroxide is 12.6nm, and specific surface area is 37m
2/ g.
2. a preparation method for mesoporous trimanganese tetroxide, is characterized in that: concrete preparation process is as follows: under normal temperature, take a certain amount of CTAB and be dissolved in distilled water, and vigorous stirring is to disperseing completely; 50wt%Mn (NO is added under continuing stirring
3)
2solution, continues to stir 30min, obtains suspension liquid, 90 DEG C of aging 3h, hot wash, suction filtration, 90 DEG C of dry 6h, roasting for some time at temperature 400 DEG C-600 DEG C, prepare mesoporous trimanganese tetroxide by NaOH solution after regulating pH.
3. the preparation method of a kind of mesoporous trimanganese tetroxide according to claim 2, is characterized in that: described CTAB and Mn (NO
3)
2mol ratio be 3:5.
4. the preparation method of a kind of mesoporous trimanganese tetroxide according to claim 2, is characterized in that: the concentration of NaOH solution is 0.2mol/L, regulates pH=9.
5. the preparation method of a kind of mesoporous trimanganese tetroxide according to claim 2, it is characterized in that: maturing temperature is 400 DEG C, roasting time is 4h.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310446901.9A CN104512932A (en) | 2013-09-26 | 2013-09-26 | Preparation method of mesoporous manganic manganous oxide |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310446901.9A CN104512932A (en) | 2013-09-26 | 2013-09-26 | Preparation method of mesoporous manganic manganous oxide |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN104512932A true CN104512932A (en) | 2015-04-15 |
Family
ID=52788853
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201310446901.9A Pending CN104512932A (en) | 2013-09-26 | 2013-09-26 | Preparation method of mesoporous manganic manganous oxide |
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| CN (1) | CN104512932A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111215049A (en) * | 2020-03-04 | 2020-06-02 | 辽宁大学 | Mn doped with Cr ions3O4Thermal catalytic material and preparation method and application thereof |
| CN112573577A (en) * | 2020-12-25 | 2021-03-30 | 中钢天源股份有限公司 | High-quality manganous-manganic oxide and preparation method thereof |
| CN114515579A (en) * | 2022-03-11 | 2022-05-20 | 黑龙江大学 | Preparation method of catalyst for low-temperature catalytic oxidation of volatile organic compounds |
-
2013
- 2013-09-26 CN CN201310446901.9A patent/CN104512932A/en active Pending
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111215049A (en) * | 2020-03-04 | 2020-06-02 | 辽宁大学 | Mn doped with Cr ions3O4Thermal catalytic material and preparation method and application thereof |
| CN111215049B (en) * | 2020-03-04 | 2022-07-19 | 辽宁大学 | Mn doped with Cr ions3O4Thermocatalytic material and preparation method and application thereof |
| CN112573577A (en) * | 2020-12-25 | 2021-03-30 | 中钢天源股份有限公司 | High-quality manganous-manganic oxide and preparation method thereof |
| CN112573577B (en) * | 2020-12-25 | 2022-08-26 | 中钢天源股份有限公司 | High-quality manganous-manganic oxide and preparation method thereof |
| CN114515579A (en) * | 2022-03-11 | 2022-05-20 | 黑龙江大学 | Preparation method of catalyst for low-temperature catalytic oxidation of volatile organic compounds |
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Legal Events
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| PB01 | Publication | ||
| WD01 | Invention patent application deemed withdrawn after publication |
Application publication date: 20150415 |
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| WD01 | Invention patent application deemed withdrawn after publication |