CN104211122B - With the decomposition precipitation circulation technology of preparing manganous-manganic oxide by manganese sulphate solution - Google Patents
With the decomposition precipitation circulation technology of preparing manganous-manganic oxide by manganese sulphate solution Download PDFInfo
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- CN104211122B CN104211122B CN201410401285.XA CN201410401285A CN104211122B CN 104211122 B CN104211122 B CN 104211122B CN 201410401285 A CN201410401285 A CN 201410401285A CN 104211122 B CN104211122 B CN 104211122B
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Abstract
The invention discloses the decomposition precipitation circulation technology that a kind of manganous sulfate prepares trimanganese tetroxide, prepare in accordance with the following steps: (1), in precipitin reaction still, add manganese sulfate solution and bicarbonate of ammonia, manganese in manganese sulfate solution fully precipitated, then filters, wash and obtain manganous carbonate; (2), trimanganese tetroxide is obtained by carrying out decomposition in manganous carbonate feeding suspension decomposition kiln; (3) in absorption tower, pass into manganese sulfate solution and ammoniacal liquor or liquefied ammonia, and the tail gas decomposed from suspending in kiln is out passed in absorption tower simultaneously and react, the amount passing into ammoniacal liquor and liquefied ammonia should make the pH of reaction solution control about 6.5, after having reacted, carry out precipitation in reaction solution inflow precipitin reaction still and obtain manganous carbonate; (4), by manganous carbonate sending into the decomposition kiln that suspends again to decompose, repeating step (3).The carbonic acid gas that the present invention utilizes manganous carbonate to decompose and ammoniacal liquor or liquefied ammonia go to precipitate manganous carbonate, and environmental protection, energy consumption are low, and cost is low.
Description
Technical field
The present invention relates to a kind of decomposition precipitation circulation technology of preparing manganous-manganic oxide by manganese sulphate solution.
Background technology
When adopting coprecipitated explained hereafter trimanganese tetroxide, traditional method is, with bicarbonate of ammonia, manganous sulfate is carried out precipitin reaction, obtain manganous carbonate, then manganous carbonate is carried out decomposition and make trimanganese tetroxide, in process of production, a large amount of bicarbonate of ammonia need be consumed, produce again a large amount of carbonic acid gas simultaneously, carbonic acid gas directly discharges in atmosphere, cause Greenhouse effect, not environmentally, cost is high.
Summary of the invention
Because the above-mentioned defect of prior art, technical problem to be solved by this invention is to provide the decomposition precipitation circulation technology that a kind of manganous sulfate prepares trimanganese tetroxide.
For achieving the above object, the invention provides the decomposition precipitation circulation technology that a kind of manganous sulfate prepares trimanganese tetroxide, prepare in accordance with the following steps:
(1), in precipitin reaction still add manganese sulfate solution and bicarbonate of ammonia, the manganese in manganese sulfate solution is fully precipitated, then filters, wash and obtain manganous carbonate;
(2), trimanganese tetroxide is obtained by carrying out decomposition in manganous carbonate feeding suspension decomposition kiln;
(3) in absorption tower, pass into manganese sulfate solution and ammoniacal liquor or liquefied ammonia, and the tail gas decomposed from suspending in kiln is out passed in absorption tower simultaneously and react, the amount passing into ammoniacal liquor and liquefied ammonia should make the pH of reaction solution control about 6.5, after having reacted, carry out precipitation in reaction solution inflow precipitin reaction still and obtain manganous carbonate;
(4), by manganous carbonate sending into the decomposition kiln that suspends again to decompose, repeating step (3).
Adopt technique scheme, the carbonic acid gas produced all passed in absorption tower in manganous carbonate decomposition course, in absorption tower, pass into manganese sulfate solution and ammoniacal liquor or liquefied ammonia, make manganous sulfate be precipitated as manganous carbonate, reaction equation is simultaneously:
MnSO
4+CO2+2NH
3+H
2O＝MnCO
3↓+(NH
4)
2SO
4
Carbonic acid gas can be avoided like this to enter in air, reduce the pollution to air, reach the effect of environmental protection.
Secondly, we can greatly reduce the use of bicarbonate of ammonia, greatly reduce production cost.
Moreover from suspending, the temperature of decomposing kiln tail gas is out about 110 DEG C, and the waste heat in tail gas utilizes by this technique in the lump, improves speed of reaction, reaches energy-conservation object.
In technique scheme: in step (2), in step (2), the charging molar weight of manganous carbonate is the 90%-110% of the charging molar weight of manganous sulfate in step (3).Carbonic acid gas in tail gas derives from the burning of the decomposition of manganous carbonate and Sweet natural gas, and (amount of the carbonic acid gas that combustion of natural gas produces accounts for greatly 10% of the amount of carbonic acid gas in tail gas.) control manganous carbonate the manganous sulfate charging molar weight of charging molar weight in step (3) 10% scope in fluctuate, can ensure there is the amount of enough carbonic acid gas in tail gas for the reaction in next step absorption tower.
In technique scheme: in step (3), the concentration of described ammoniacal liquor is 10-17%, and in manganese sulfate solution, Fe content is 45-60g/L.By the control of the inlet amount of manganous sulfate and the inlet amount of ammoniacal liquor, thus make manganous sulfate fully be precipitated as manganous carbonate, in the solution of the discharge port on absorption tower, Fe content only has 1-3g/L.
In technique scheme: in described step (3), tail gas gas blower blasts in absorption tower.Ensure that tail gas all enters in absorption tower.
The invention has the beneficial effects as follows: the carbon dioxide recovery that manganous carbonate decomposes is used for again precipitating manganous carbonate by the present invention, do not need to re-use bicarbonate of ammonia after first time drops into bicarbonate of ammonia, the carbonic acid gas utilizing manganous carbonate to decompose and ammoniacal liquor or liquefied ammonia go to precipitate manganous carbonate, iterative cycles like this runs, both the object utilizing carbonic acid gas in tail gas had been reached, also utilize the waste heat of tail gas simultaneously, energy consumption significantly reduces, precipitation agent is done with ammoniacal liquor or liquefied ammonia, do not need Manual material feeding, and the totally-enclosed operation of system, non-environmental-pollution, level of automation is high.
Accompanying drawing explanation
Fig. 1 is schema of the present invention.
Embodiment
Below in conjunction with drawings and Examples, the invention will be further described:
Embodiment 1:
65*10 is injected in coprecipitated reactor
3l manganese sulfate solution (concentration of manganese is 45g/l), add 5500kg bicarbonate of ammonia, control temperature is 30 DEG C, reacts 2 hours, then with pump delivery to band filter being carried out filter, washing, filter, then sends into decompose in kiln and decomposes.During decomposition, control manganous carbonate enters kiln amount is 1286 ± 128kg/ hour (8.94 ± 0.89mol) (moisture 20%), decomposition temperature 800 DEG C, exhaust temperature 110 DEG C, tail gas gas blower all blasts in absorption tower, and the feed rate simultaneously passing into manganese sulfate solution (concentration of manganese is 45g/l) manganous sulfate in absorption tower is 11*10
3mass concentration is that the ammoniacal liquor of 10% is by inlet amount 1.46*10 by L/h simultaneously
3l/h pumps into absorption tower, and ensure that the pH of reaction solution is about 6.5, reacted slip overflows to coprecipitated reactor from discharge port, with pump delivery to band filter being carried out filter, washing, filter, then sends into decompose in kiln and decomposes.Circulation like this is carried out.The trimanganese tetroxide of calcining is discharged to endlessly through washing post-drying in rinse bath from kiln cyclone, and product meets trimanganese tetroxide requirement.
Embodiment 2:
65*10 is injected in coprecipitated reactor
3l manganese sulfate solution (content of manganese is 45g/l), add 5500kg bicarbonate of ammonia, control temperature is 30 DEG C, reacts 2 hours, then with pump delivery to band filter being carried out filter, washing, filter, then sends into decompose in kiln and decomposes.It is 1286 ± 120kg/ hour (moisture 20%) that control manganous carbonate enters kiln amount, decomposition temperature 800 DEG C, exhaust temperature 110 DEG C, tail gas all blasts absorption tower with gas blower, in absorption tower, pass into manganese sulfate solution (content of manganese is 60g/l), be 8.25*10 by inlet amount simultaneously
3l/h pumps in absorption tower, is injected in absorption tower by liquefied ammonia water by inlet amount 146kg/h simultaneously.Ensure that the pH of reaction solution is about 6.5, reacted slip overflows in coprecipitated reactor, with pump delivery to band filter being carried out filter, washing, filter, then sends into decompose in kiln and decomposes.Circulation like this is carried out.The trimanganese tetroxide of calcining is discharged to endlessly through washing post-drying in rinse bath from kiln cyclone, and product meets trimanganese tetroxide requirement.
More than describe preferred embodiment of the present invention in detail.Should be appreciated that those of ordinary skill in the art just design according to the present invention can make many modifications and variations without the need to creative work.Therefore, all technician in the art, all should by the determined protection domain of claims under this invention's idea on the basis of existing technology by the available technical scheme of logical analysis, reasoning, or a limited experiment.
Claims (4)
1. prepare a decomposition precipitation circulation technology for trimanganese tetroxide with manganous sulfate, prepare in accordance with the following steps:
(1), in precipitin reaction still add manganese sulfate solution and bicarbonate of ammonia, the manganese in manganese sulfate solution is fully precipitated, then filters, wash and obtain manganous carbonate;
(2), trimanganese tetroxide is obtained by carrying out decomposition in manganous carbonate feeding suspension decomposition kiln;
(3) in absorption tower, pass into manganese sulfate solution and ammoniacal liquor or liquefied ammonia, and the tail gas decomposed from suspending in kiln is out passed in absorption tower simultaneously and react, the amount passing into ammoniacal liquor and liquefied ammonia should make the pH of reaction solution control 6.5, after having reacted, carry out precipitation in reaction solution inflow precipitin reaction still and obtain manganous carbonate;
(4), by the manganous carbonate pump delivery in precipitin reaction still carry out filtering to band filter, wash, filter, then send into suspend to decompose in kiln and decompose, repeating step (3).
2. prepare the decomposition precipitation circulation technology of trimanganese tetroxide according to claim 1 with manganous sulfate, it is characterized in that: in step (2), the charging molar weight of manganous carbonate is the 90%-110% of the charging molar weight of manganous sulfate in step (3).
3. prepare the decomposition precipitation circulation technology of trimanganese tetroxide according to claim 2 with manganous sulfate, it is characterized in that: in step (3), the concentration of described ammoniacal liquor is 10%-17%, and in manganese sulfate solution, Fe content is 45-60g/L.
4. prepare the decomposition precipitation circulation technology of trimanganese tetroxide according to claim 1 with manganous sulfate, it is characterized in that: in described step (3), tail gas gas blower blasts in absorption tower.
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| CN113087516B (en) * | 2021-03-31 | 2022-07-22 | 重庆上甲电子股份有限公司 | Low-temperature sintering method for preparing manganese-zinc ferrite by using industrial wastes |
| CN115286041A (en) * | 2022-08-09 | 2022-11-04 | 贵州金瑞新材料有限责任公司 | Roasting manufacturing method of high-purity trimanganese tetroxide |
Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1295978A (en) * | 2000-12-25 | 2001-05-23 | 化学工业部天津化工研究设计院 | Process for preparing manganor manganic oxide used for soft magnetic ferrite |
| CN101531503A (en) * | 2009-02-10 | 2009-09-16 | 重庆上甲电子股份有限公司 | Method for preparing mixture of soft magnetic manganese zinc iron |
| CN101898797A (en) * | 2010-08-04 | 2010-12-01 | 湖南汇通科技有限责任公司 | High-purity trimanganese tetroxide and preparation method thereof |
| CN102060332A (en) * | 2010-11-10 | 2011-05-18 | 湘西自治州兴湘科技开发有限责任公司 | Method for circularly producing mangano-manganic oxide by manganous sulfate |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP4305629B2 (en) * | 2003-03-27 | 2009-07-29 | 戸田工業株式会社 | Trimanganese tetroxide powder and production method thereof, positive electrode active material for nonaqueous electrolyte secondary battery and production method thereof, and nonaqueous electrolyte secondary battery |
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Patent Citations (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1295978A (en) * | 2000-12-25 | 2001-05-23 | 化学工业部天津化工研究设计院 | Process for preparing manganor manganic oxide used for soft magnetic ferrite |
| CN101531503A (en) * | 2009-02-10 | 2009-09-16 | 重庆上甲电子股份有限公司 | Method for preparing mixture of soft magnetic manganese zinc iron |
| CN101898797A (en) * | 2010-08-04 | 2010-12-01 | 湖南汇通科技有限责任公司 | High-purity trimanganese tetroxide and preparation method thereof |
| CN102060332A (en) * | 2010-11-10 | 2011-05-18 | 湘西自治州兴湘科技开发有限责任公司 | Method for circularly producing mangano-manganic oxide by manganous sulfate |
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