CN103121722A - Preparation method of trimanganese tetraoxide with high activity - Google Patents
Preparation method of trimanganese tetraoxide with high activity Download PDFInfo
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- CN103121722A CN103121722A CN 201110369430 CN201110369430A CN103121722A CN 103121722 A CN103121722 A CN 103121722A CN 201110369430 CN201110369430 CN 201110369430 CN 201110369430 A CN201110369430 A CN 201110369430A CN 103121722 A CN103121722 A CN 103121722A
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- trimanganese tetroxide
- trimanganese tetraoxide
- electrolytic metal
- preparation
- ammoniacal liquor
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Abstract
The invention discloses a preparation method of trimanganese tetraoxide with high activity. The preparation method comprises the steps of: grinding an electrolytic metal manganese sheet to electrolytic metal manganese powder with grain size being 150 microns by a pair of rollers; rapidly putting the electrolytic metal manganese powder in a reaction kettle with an ultrasonic oscillator, wherein the reaction kettle has ammonia-water-containing warm water with the temperature of 20-40 DEG C, which is added in advance; carrying out stirring and introducing filtered purified air simultaneously; slowly introducing ammonia water; carrying out ultrasonic oscillation on suspension simultaneously when reacting so as to restrain the agglomeration of trimanganese tetraoxide; improving the activity of the trimanganese tetraoxide simultaneously when accelerating reaction speed; after washing trimanganese tetraoxide slurry, carrying out centrifugal spray drying or pressure spray drying with air inlet temperature of 300-400 DEG C; and then drying out water by a kiln with the temperature of 150-250 DEG C, thereby obtaining the trimanganese tetraoxide with high activity.
Description
Technical field
The present invention relates to compound of manganese and preparation method thereof, be specifically related to a kind of preparation method of high reactivity trimanganese tetroxide.
Background technology
At present, development along with electronic technology, need the high reactivity trimanganese tetroxide as raw material for producing high-performance manganese-zinc ferrite, the preparation method of present existing trimanganese tetroxide mainly contains electrolytic metal manganese powder suspension liquid catalytic oxidation, roasting method, reduction method etc.Existing production high reactivity trimanganese tetroxide production technique, be mainly select activity preferably the electrolytic metal Mn sheet do raw material, adopt lower concentration electrolytic metal manganese powder suspension liquid oxidation style in the common response still, then obtain the high reactivity trimanganese tetroxide by washing, high temperature drying.But oxidization time is long, and production cost is high.
Summary of the invention
Long reaction time for the production that overcomes existing high reactivity trimanganese tetroxide, the deficiency that cost is higher the invention provides a kind of preparation method of high reactivity trimanganese tetroxide.
The technical solution adopted for the present invention to solve the technical problems is: a kind of preparation method of high reactivity trimanganese tetroxide, be with the electrolytic metal Mn sheet with roller-crushing mill to the electrolytic metal manganese powder of-150 μ m, drop into fast in the reactor with ultrasonic oscillator, the warm water that contains ammoniacal liquor that adds in advance 20 ~ 40 ℃ in reactor, manganese slurry solid-to-liquid ratio is about 1:5 ~ 10, stirs, and passes into simultaneously through purifying air of filtering, and slowly inject ammoniacal liquor, the amount of ammoniacal liquor is along with Mn in reaction soln
2+The slow reduction of concentration and slowly adding.In the time of reaction, suspension liquid is added ultra-sonic oscillation, suppress the reunion of trimanganese tetroxide by ultra-sonic oscillation, in fast reaction speed, improve trimanganese tetroxide active.The trimanganese tetroxide slurries that reaction obtains are after washing, the employing intake air temperature is centrifugal spray drying or the pressure spray dryer of 300 ~ 400 ℃, disperseed but the trimanganese tetroxide of certain water content is arranged, then being dried moisture content by 150 ~ 250 ℃ of kilns, namely being got the high reactivity trimanganese tetroxide.
The invention has the beneficial effects as follows, greatly shortened the reaction production cycle of high reactivity trimanganese tetroxide, thereby reduced production cost.
Embodiment:
Embodiment: with 2 tons of electrolytic metal Mn sheets with the electrolytic metal manganese powder of roller-crushing mill to-150 μ m; grind and the protection of screening process employing inert gas; to keep the activity of electrolytic metal manganese powder; drop into fast in the reactor with ultrasonic oscillator, add in advance the approximately warm water that contains ammoniacal liquor of 30 ℃ in reactor, manganese slurry solid-to-liquid ratio is about 1:7.5; stir; and pass into through purifying air of filtering, and slowly implantation concentration is 10% ammoniacal liquor, ammoniacal liquor is along with Mn in reaction soln
2+The slow reduction of concentration and slowly add Mn
2+Stop adding ammoniacal liquor when change in concentration is little.In the time of reaction, the suspension liquid in reactor is added ultra-sonic oscillation, suppress the reunion of trimanganese tetroxide by ultra-sonic oscillation, in fast reaction speed, improved trimanganese tetroxide active.The trimanganese tetroxide slurries that reaction obtains are after pure water washing impurity elimination, the employing intake air temperature is the pressure spray dryer of 300 ~ 400 ℃, disperseed but the trimanganese tetroxide of certain water content is arranged, then being dried moisture content by 180 ℃ of kilns, namely being got the high reactivity trimanganese tetroxide.The performance of high reactivity trimanganese tetroxide is as follows: Mn content is that 71.2%, Si content is that 0.0045%, S content is that 0.035%, K content is that 0.001%, Ca content is that 0.0032%, Mg content is 0.0048%, and crystal formation is γ-Mn
3O
4, loose density is 0.58g/cm
3, specific surface area (BET) is 26m
2/ g.
Claims (1)
1. the preparation method of a high reactivity trimanganese tetroxide, it is characterized in that: with the electrolytic metal Mn sheet with roller-crushing mill to the electrolytic metal manganese powder of-150 μ m, drop into fast in the reactor with ultrasonic oscillator, the warm water that contains ammoniacal liquor that adds in advance 20 ~ 40 ℃ in reactor, manganese slurry solid-to-liquid ratio is about 1:5 ~ 10, stirs, and passes into simultaneously through purifying air of filtering, and slowly inject ammoniacal liquor, the amount of ammoniacal liquor is along with Mn in reaction soln
2+The slow reduction of concentration and slowly adding.In the time of reaction, suspension liquid is added ultra-sonic oscillation.The trimanganese tetroxide slurries that reaction obtains are after washing, the employing intake air temperature is centrifugal spray drying or the pressure spray dryer of 300 ~ 400 ℃, disperseed but the trimanganese tetroxide of certain water content is arranged, then being dried moisture content by 150 ~ 250 ℃ of kilns, namely being got the high reactivity trimanganese tetroxide.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110369430 CN103121722A (en) | 2011-11-21 | 2011-11-21 | Preparation method of trimanganese tetraoxide with high activity |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN 201110369430 CN103121722A (en) | 2011-11-21 | 2011-11-21 | Preparation method of trimanganese tetraoxide with high activity |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN103121722A true CN103121722A (en) | 2013-05-29 |
Family
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Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN 201110369430 Pending CN103121722A (en) | 2011-11-21 | 2011-11-21 | Preparation method of trimanganese tetraoxide with high activity |
Country Status (1)
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| CN (1) | CN103121722A (en) |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105417586A (en) * | 2015-12-29 | 2016-03-23 | 中国科学院过程工程研究所 | Preparation method for manganic manganous oxide |
| CN109052480A (en) * | 2018-09-30 | 2018-12-21 | 贵州铜仁金瑞锰业有限责任公司 | A kind of high-purity mangano-manganic oxide and preparation method thereof |
| CN110422881A (en) * | 2019-08-15 | 2019-11-08 | 湖南特种金属材料有限责任公司 | A kind of preparation method of trimanganese tetraoxide with high activity |
-
2011
- 2011-11-21 CN CN 201110369430 patent/CN103121722A/en active Pending
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105417586A (en) * | 2015-12-29 | 2016-03-23 | 中国科学院过程工程研究所 | Preparation method for manganic manganous oxide |
| CN109052480A (en) * | 2018-09-30 | 2018-12-21 | 贵州铜仁金瑞锰业有限责任公司 | A kind of high-purity mangano-manganic oxide and preparation method thereof |
| CN110422881A (en) * | 2019-08-15 | 2019-11-08 | 湖南特种金属材料有限责任公司 | A kind of preparation method of trimanganese tetraoxide with high activity |
| CN110422881B (en) * | 2019-08-15 | 2022-03-11 | 湖南特种金属材料有限责任公司 | Preparation method of high-activity trimanganese tetroxide |
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Application publication date: 20130529 |