CN106367589B - A kind of low consumed high purity manganese sulfate solution manufacturing method of short route - Google Patents
A kind of low consumed high purity manganese sulfate solution manufacturing method of short route Download PDFInfo
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- CN106367589B CN106367589B CN201610832433.2A CN201610832433A CN106367589B CN 106367589 B CN106367589 B CN 106367589B CN 201610832433 A CN201610832433 A CN 201610832433A CN 106367589 B CN106367589 B CN 106367589B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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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
- C01G45/10—Sulfates
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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Abstract
The present invention relates to a kind of method of the sulfuric acid to leach liquid direct preparation of high-purity manganese sulfate solution from low grade rhodochrosite, the ascending changing rule of system pH value is implemented, and played efficient chemical coupling mechanism.The method of the present invention continues to dissolve manganese mineral powder first into the sulfuric acid to leach liquid of low-grade manganese, connects, and adds barium fluoride after reaching 3 ~ 4 with the pH value of barium hydroxide regulation leaching liquid successively, filters；Adjusted again with barium hydroxide between filtrate pH value reaches 5 ~ 6 and add barium sulphide afterwards, filtering, obtain new filtrate；The PH to 8 of new filtrate is finally adjusted with barium hydroxide, high-purity sulphuric acid manganese solution is obtained after filtering.Medicament caused by present invention operation that is simple to operate, avoiding repeatedly overlapping regulation system pH value wastes, manganese content >=80g/L in the high-purity sulphuric acid manganese solution of preparation, major impurity content≤10ppm, content of beary metal≤1ppm, there is provided the free of contamination high purity manganese sulfate solution manufacturing method of short route low consumption.
Description
Technical field
It is more particularly to a kind of directly to be prepared from the sulfuric acid to leach liquid of low grade rhodochrosite the invention belongs to chemical production field
The method of high-purity sulphuric acid manganese solution.
Background technology
At present, the demand of high purity manganese sulfate gradually increases, but the production of high purity manganese sulfate receives larger technology limit
System.At home and abroad generally using electrolytic manganese metal production high purity manganese sulfate, i.e., with electrolytic manganese metal processing powdering, sulfuric acid is molten again
Solution produces, because the production of these high purity manganese sulfates experienced ions of manganese (manganese ore)-manganese metal (electrolysis)-ions of manganese (oxidation)
Production cycle, thus the physical index such as product price is expensive, granularity pattern be difficult to regulation and control the problem of.Moreover, current electrolysis manganese industry
95% raw material is low grade rhodochrosite, and full manganese comprehensive utilization ratio is only 70% or so, while direct current in electrolytic manganese production process
Current efficiency is hovered 75% or so always, and energy efficiency is relatively low, and the electrolysis production waste water containing chromium, selenium, manganese and ammonia nitrogen and
Manganese slag had once triggered startling ecological environment problem.Therefore sulphur is prepared from industrial manganic sulfate or directly from manganese spar removal of impurities
The technology of sour manganese solution is by extensive concern.
The technological process length of manganese sulfate solution is directly prepared from manganese spar removal of impurities, and key issue is its impurity depth
The technical difficulty of removal is high, it is contemplated that the poor feasibility of technology the problems such as cost accounting and environmental protection.Especially for current
The present situation of China's manganese spar average grade≤14%, from the sulfuric acid to leach liquid removal of impurities direct preparation of high-purity manganese sulfate solution of manganese spar
Face very big challenge：(1) because soluble impurity species is complicated, content is more and is difficult to remove in low-grade manganese.(2) lead to
Frequently with go removing calcium and magnesium contamination precipitation agent mainly to have ammonium fluoride, manganous fluoride etc., but due to precipitated product magnesium fluoride, calcirm-fluoride
Particle it is smaller, it is more difficult to sedimentation and filtering, cause the calcium and magnesium impurity in manganese sulfate solution to be not easy depth removal, and precipitated product
Because high ratio surface can adsorb more manganese ion, with the loss of manganese while causing removing calcium and magnesium impurity.(3) tradition system
In standby technique, to coordinate dedoping step to need repeatedly the pH value of regulation system, the serious waste and technological operation for causing medicament are answered
Miscellaneous, synthesis cycle length.
The content of the invention
For China's manganese spar average grade it is low≤14% current resources situation, it is a kind of from low product present invention aims at providing
The method of the sulfuric acid to leach liquid direct preparation of high-purity manganese sulfate solution of position manganese spar, using ion ionization and dissolution equilibrium theory as base
Plinth, the ascending changing rule of the pH value of system is implemented, has played efficient chemical coupling mechanism, being that a kind of short route is low disappears
The method for preparing high-purity sulphuric acid manganese solution of consumption.
The low consumed high purity manganese sulfate solution manufacturing method of short route of the present invention, is comprised the following steps that：
(1) it is the manganese spar of grade≤14% is levigate, 100~200 mesh sieves are crossed, obtain manganese mineral powder；Manganese mineral powder is added to
Concentration is in 1.5~2mol/L sulfuric acid solution, and the mass ratio of sulfuric acid solution and manganese mineral powder is 3:1~5:1, in the condition of stirring
Under be heated to 80~90 DEG C and keep 2~4h, be filtrated to get leaching manganese ore liquid 1；
(2) manganese mineral powder mentioned in step (1) is continuously added into leaching manganese ore liquid 1, leaching manganese ore liquid 1 and manganese mineral powder
Mass ratio is 3:1~5:1,80~90 DEG C are heated under agitation and keeps 2~4h, are filtrated to get leaching manganese ore liquid 2；
(3) barium hydroxide is added in the leaching manganese ore liquid 2 obtained into step (2), regulation pH value reaches 3~4, added
Barium fluoride, until being produced without new precipitation, then filter, obtain filtrate 1；
(4) barium hydroxide is added in the filtrate 1 obtained into step (3), regulation pH value reaches 5~6, adds vulcanization
Barium, until being produced without new precipitation, then filter, obtain filtrate 2；
(5) barium hydroxide is added in the filtrate 2 obtained into step (4), the PH to 7~8 of regulation, after filtering, is obtained
Filtrate is high-purity sulphuric acid manganese solution.
Content >=80g/L of manganese, K, Ca, Na, Mg, Fe, Al, Si impurity in high-purity sulphuric acid manganese solution prepared by the above method
Content≤10ppm, and beavy metal impurity content≤1ppm, wherein beavy metal impurity include Cu, Ni, Zn, Co, Cr, Pb wherein
One or more.
Step (3), (4), barium hydroxide is content >=98% described in (5), and cross the barium hydroxide octahydrate of 100 mesh sieves
Solid powder；
Barium fluoride described in step (3) is content >=99%, and crosses the barium fluoride solid powder of 100 mesh sieves；
Barium sulphide described in step (4) is content >=99%, and crosses the barium sulphide solid powder of 100 mesh sieves.
The present invention outstanding feature and have technical effect that：(1) based on system ionic ionization and dissolution equilibrium theory,
Proposing includes barium hydroxide, barium fluoride, barium sulphide using containing barium compound and follows the small of solution system pH value and arrive big tune
Section order, the method for going iron removaling aluminium, calcium and magnesium, heavy metal and iron tramp to obtain high-purity sulphuric acid manganese solution successively are simple to operate, pair set
It is standby require low, process is pollution-free.(2) operation for adjusting solution ph repeatedly is avoided in dedoping step, saves medicament, is dropped
Low production cost, technological process is shortened, improve production efficiency；(3) compound that baric is introduced in preparation process is entered
Row system acid-base value adjusts and removing impurity by means of precipitation, due to barium ions combined with sulfate ion the barium sulfate precipitate particle generated compared with
Greatly, therefore barium ions is easily settled and filtered in the sulfuric acid to leach liquid of manganese spar, so as to which depth goes the removal of impurity, will not cause manganese
Loss；(4) manganese content is high in the high-purity sulphuric acid manganese solution prepared, comprising K, Ca, Na, Mg, Fe, Al, Si, Cu, Ni, Zn, Co,
Impurity content including Cr, Pb is low, purity is higher than current like product.
Brief description of the drawings
Fig. 1 is the composition of high-purity sulphuric acid manganese solution and the chemical pure manganese sulfate solution of in the market purchase that embodiment 3 synthesizes
Analysis contrast column diagram.
Embodiment
In order to make the purpose , technical scheme and advantage of the present invention be clearer, it is right below in conjunction with drawings and Examples
The present invention is explained in further detail.It should be appreciated that specific embodiment described herein is used only for explaining the present invention, and
It is not used in the restriction present invention.
Embodiment 1
(1) it is the manganese spar of grade 12% is levigate, 200 mesh sieves are crossed, obtain manganese mineral powder；Manganese mineral powder is added to 2mol/L's
In sulfuric acid solution, the mass ratio of sulfuric acid solution and manganese mineral powder is 3:1, continue to react after 90 DEG C are heated under conditions of stirring
4h, leaching manganese ore liquid 1 is filtrated to get, using its impurity content of icp analysis；
(2) manganese mineral powder is added into leaching manganese ore liquid 1, the mass ratio of leaching manganese ore liquid 1 and manganese mineral powder is 3:1, stirring
Under the conditions of be heated to 90 DEG C after continue react 4h, be filtrated to get leaching manganese ore liquid 2；
(3) PH to 4 of leaching manganese ore liquid 2 is adjusted with barium hydroxide, adds barium fluoride, until being produced without new precipitation, so
After filter, obtain filtrate 1, wherein barium hydroxide is the barium hydroxide octahydrate solid powder that content 98% crosses 100 mesh sieves, fluorination
Barium is content 99% and crosses the barium fluoride solid powder of 100 mesh sieves；
(4) PH to 6 of filtrate 1 is adjusted with barium hydroxide, adds barium sulphide, until being produced without new precipitation, is then filtered,
Obtain filtrate 2, wherein barium hydroxide is the barium hydroxide octahydrate solid powder that content 98% crosses 100 mesh sieves, barium sulphide be containing
Amount 99% and the barium sulphide solid powder for crossing 100 mesh sieves；
(5) PH to 8 of filtrate 2 is adjusted with barium hydroxide, barium hydroxide is eight hydrated hydroxides that content 98% crosses 100 mesh sieves
Change barium solid powder, the filtrate being filtrated to get is high-purity sulphuric acid manganese solution.
Manganese content 83g/L in the manganese sulfate solution that embodiment 1 synthesizes.Table 1 is high-purity sulphuric acid manganese solution prepared by embodiment 1
Icp analysis result, and be that impurity in embodiment in leaching manganese ore liquid 1 is carried out pair with the manganese spar sulfuric acid to leach liquid of grade 12%
Than.As can be seen from the table, grade for 12% manganese spar dopant species are more, content height, but be prepared by the method for the present invention
In manganese sulfate solution Potassium, calcium, sodium, magnesium, iron, aluminium, silicone content≤heavy metal such as 10ppm, nickel, zinc, cobalt, chromium, copper, lead is miscellaneous
Matter content≤1ppm, it was confirmed that be directly prepared for high-purity sulphuric acid manganese solution from the sulfuric acid to leach liquid of low grade rhodochrosite.
The impurity icp analysis of high-purity sulphuric acid manganese solution prepared by the embodiment 1 of table 1 and the manganese spar sulfuric acid to leach liquid of grade 12%
As a result
Embodiment 2
(1) it is the manganese spar of grade 14% is levigate, 150 mesh sieves are crossed, obtain manganese mineral powder；Manganese mineral powder is added to 1.8mol/L
Sulfuric acid solution in, the mass ratio of sulfuric acid solution and manganese mineral powder is 4:1, continue to react after 85 DEG C are heated under conditions of stirring
3h, leaching manganese ore liquid 1 is filtrated to get, using its impurity content of icp analysis；
(2) manganese mineral powder is added into leaching manganese ore liquid 1, the mass ratio of leaching manganese ore liquid 1 and manganese mineral powder is 5:1 in stirring bar
Continue to react 3h after being heated to 80 DEG C under part, be filtrated to get leaching manganese ore liquid 2；
(3) PH to 3 of leaching manganese ore liquid 2 is adjusted with barium hydroxide, adds barium fluoride, until being produced without new precipitation, so
After filter, obtain filtrate 1, wherein barium hydroxide is the barium hydroxide octahydrate solid powder that content 98% crosses 100 mesh sieves, fluorination
Barium is content 99% and crosses the barium fluoride solid powder of 100 mesh sieves；
(4) PH to 5 of filtrate 1 is adjusted with barium hydroxide, adds barium sulphide, until being produced without new precipitation, is then filtered,
Obtain filtrate 2, wherein barium hydroxide is the barium hydroxide octahydrate solid powder that content 98% crosses 100 mesh sieves, barium sulphide be containing
Amount 99% and the barium sulphide solid powder for crossing 100 mesh sieves；
(5) PH to 7 of filtrate 2 is adjusted with barium hydroxide, barium hydroxide is eight hydrated hydroxides that content 98% crosses 100 mesh sieves
Change barium solid powder, the filtrate being filtrated to get is high-purity sulphuric acid manganese solution.
Embodiment it is 2-in-1 into manganese sulfate solution in manganese content 80g/L.The table 1 of table 2 is high purity manganese sulfate prepared by embodiment 2
Solution I CP analysis results.As can be seen from the table, Potassium in the manganese sulfate solution being prepared by the method for the present invention, calcium, sodium,
Magnesium, iron, aluminium, silicone content≤beavy metal impurity such as 10ppm, nickel, zinc, cobalt, chromium, copper, lead content≤1ppm, it was confirmed that from low
The sulfuric acid to leach liquid of grade manganese spar is directly prepared for high-purity sulphuric acid manganese solution.
The impurity icp analysis result of high-purity sulphuric acid manganese solution prepared by the embodiment 2 of table 2
| Impurity element/ppm | Fe | Al | Si | Ca | Mg | K | Na | Cu | Ni | Zn | Cr |
| High-purity sulphuric acid manganese solution | 9.3 | 2.1 | 1.6 | 3.2 | 8.1 | 1.1 | 1.8 | 0.1 | ＜ 0.1 | 0.4 | ＜ 0.1 |
Embodiment 3
(1) it is the manganese spar of grade 11% is levigate, 100 mesh sieves are crossed, obtain manganese mineral powder；Manganese mineral powder is added to 1.5mol/L
Sulfuric acid solution in, the mass ratio of sulfuric acid solution and manganese mineral powder is 5:1, continue to react after 80 DEG C are heated under conditions of stirring
2h, it is filtrated to get leaching manganese ore liquid 1；
(2) manganese mineral powder is added into leaching manganese ore liquid 1, the mass ratio of leaching manganese ore liquid 1 and manganese mineral powder is 4:1；Stirring
Under the conditions of be heated to 85 DEG C after continue react 2h, be filtrated to get leaching manganese ore liquid 2；
(3) PH to 3 of leaching manganese ore liquid 2 is adjusted with barium hydroxide, adds barium fluoride, until being produced without new precipitation, so
After filter, obtain filtrate 1, wherein barium hydroxide is the barium hydroxide octahydrate solid powder that content 98% crosses 100 mesh sieves, fluorination
Barium is content 99% and crosses the barium fluoride solid powder of 100 mesh sieves；
(4) PH to 6 of filtrate 1 is adjusted with barium hydroxide, adds barium sulphide, until being produced without new precipitation, is then filtered,
Obtain filtrate 2, wherein barium hydroxide is the barium hydroxide octahydrate solid powder that content 98% crosses 100 mesh sieves, barium sulphide be containing
Amount 99% and the barium sulphide solid powder for crossing 100 mesh sieves；
(5) PH to 8 of filtrate 2 is adjusted with barium hydroxide, barium hydroxide is eight hydrated hydroxides that content 98% crosses 100 mesh sieves
Change barium solid powder, the filtrate being filtrated to get is high-purity sulphuric acid manganese solution.
Manganese content 82g/L in the manganese sulfate solution that embodiment 3 synthesizes.Fig. 1 is the high-purity sulphuric acid manganese solution that embodiment 3 synthesizes
Constituent analysis with the chemical pure manganese sulfate solution of in the market purchase contrasts block diagram.Comparative analysis can be found, pass through the present invention
Method prepare manganese sulfate solution in impurity content≤10ppm, beavy metal impurity content≤1ppm, it was confirmed that synthesized high-purity
Manganese sulfate solution, technological process that the present invention is directly prepared from the sulfuric acid to leach liquid of low grade rhodochrosite is short, consumption is low, has
There is obvious advantage.
Claims (6)
1. a kind of low consumed high purity manganese sulfate solution manufacturing method of short route, it is characterised in that comprise the following steps that：
（1）The manganese spar of grade≤14% is levigate, 100 ~ 200 mesh sieves are crossed, obtain manganese mineral powder；Manganese mineral powder is added into concentration is
In 1.5 ~ 2mol/L sulfuric acid solution, the mass ratio of sulfuric acid solution and manganese mineral powder is 3:1~5:1, it is heated under conditions of stirring
80 ~ 90 DEG C and 2 ~ 4h of holding, it is filtrated to get leaching manganese ore liquid 1；
（2）Step is continuously added into leaching manganese ore liquid 1（1）In the manganese mineral powder mentioned, the quality of leaching manganese ore liquid 1 and manganese mineral powder
Than for 3:1~5:1,80 ~ 90 DEG C are heated under agitation and keeps 2 ~ 4h, are filtrated to get leaching manganese ore liquid 2；
（3）To step（2）In add barium hydroxide in obtained leaching manganese ore liquid 2, regulation pH value reaches 3 ~ 4, adds fluorination
Barium, until being produced without new precipitation, then filter, obtain filtrate 1；
（4）To step（3）In add barium hydroxide in obtained filtrate 1, regulation pH value reaches 5 ~ 6, adds barium sulphide, until
Produced without new precipitation, then filter, obtain filtrate 2；
（5）To step（4）In add barium hydroxide in obtained filtrate 2, the PH to 7 ~ 8 of regulation, after filtering, obtained filtrate is
High-purity sulphuric acid manganese solution.
2. the low consumed high purity manganese sulfate solution manufacturing method of short route according to claim 1, it is characterised in that described
Barium hydroxide is content >=98%, and crosses the barium hydroxide octahydrate solid powder of 100 mesh sieves.
3. the low consumed high purity manganese sulfate solution manufacturing method of short route according to claim 1, it is characterised in that described
Barium fluoride is content >=99%, and crosses the barium fluoride solid powder of 100 mesh sieves.
4. the low consumed high purity manganese sulfate solution manufacturing method of short route according to claim 1, it is characterised in that described
Barium sulphide is content >=99%, and crosses the barium sulphide solid powder of 100 mesh sieves.
A kind of 5. low consumed high purity manganese sulfate solution manufacturing method of short route according to claim 1, it is characterised in that
Content >=80g/L of manganese in the high-purity sulphuric acid manganese solution, K, Ca, Na, Mg, Fe, Al, Si impurity content≤10ppm, and again
Metals content impurity≤1ppm.
A kind of 6. low consumed high purity manganese sulfate solution manufacturing method of short route according to claim 5, it is characterised in that
Beavy metal impurity in high-purity sulphuric acid manganese solution includes Cu, Ni, Zn, Co, Cr, Pb one or more therein.
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| CN107055501B (en) * | 2017-04-28 | 2019-05-03 | 北京科技大学 | A method of hureaulite type manganese phosphate is prepared from low grade rhodochrosite leachate |
| CN107651709B (en) * | 2017-10-19 | 2019-05-17 | 北京科技大学 | A kind of short flow process of high purity manganese sulfate monohydrate powder of the free-floride without sulphur |
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| CN101698513A (en) * | 2009-11-03 | 2010-04-28 | 鄢冬子 | Method for preparing high-purity trimanganese tetroxide |
| CN102134101B (en) * | 2011-04-29 | 2012-08-29 | 金瑞新材料科技股份有限公司 | Method for preparing trimanganese tetroxide by using rhodochrosite |
| CN103342390B (en) * | 2013-07-18 | 2015-04-08 | 广西南宁晟瑞冶化技术有限公司 | Method for high-purity manganese sulfate monohydrate |
| CN104294038A (en) * | 2013-07-19 | 2015-01-21 | 无锡永发电镀有限公司 | Technology for preparing manganese carbonate from silver-manganese ores |
| CN104060294B (en) * | 2013-12-24 | 2017-01-04 | 中信大锰矿业有限责任公司大新锰矿分公司 | A kind of manganese sulphate solution degree of depth filter pressing purification method |
| CN104404568B (en) * | 2014-12-15 | 2017-09-26 | 中信大锰矿业有限责任公司大新锰矿分公司 | Utilize the method for manganese carbonate ore and manganese oxide ore baked for producing electrolytic manganese metal |
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