CN106745288A - A kind of production method of high-purity manganese sulphate - Google Patents
A kind of production method of high-purity manganese sulphate Download PDFInfo
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- CN106745288A CN106745288A CN201611150554.5A CN201611150554A CN106745288A CN 106745288 A CN106745288 A CN 106745288A CN 201611150554 A CN201611150554 A CN 201611150554A CN 106745288 A CN106745288 A CN 106745288A
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- manganese
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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
- C01—INORGANIC CHEMISTRY
- C01P—INDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
- C01P2006/00—Physical properties of inorganic compounds
- C01P2006/80—Compositional purity
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Abstract
The invention discloses a kind of production method of high-purity manganese sulphate, comprise the following steps：(1) electrolytic manganese dioxide crushing and water washing is dried and is milled, sulphur milling；(2) electrolytic manganese dioxide powder and Cosan are well mixed to be put into porcelain dish and be put into by 1: 0.3~1: 0.5 and are had warmed up to 630 DEG C of Muffle kiln roastings, produce manganese monoxide；(3) manganese monoxide is poured into while hot after being stirred in the beaker equipped with pure water and is filtered, obtain filter cake；(4) separately take in beaker addition pure water and analytical pure sulfuric acid, adjust pH value to stopping after 5.2 with filter cake under stirring and add, obtain the manganese sulfate solution for having leached；(5) manganese sulfate solution for having leached condensing crystallizing in 100 DEG C, when filtrate is evaporated soon, is filtrated to get manganese sulfate monohydrate crystal while hot.A kind of production method of high-purity manganese sulphate that the present invention is provided, can simplify the purification problem of solution in preparation process, solution quality is guaranteed, and reduce production cost.
Description
Technical field
The invention belongs to production of manganese sulfate as field, especially a kind of production method of high-purity manganese sulphate.
Background technology
In all manganese products that the whole world is used, the manganese product produced using manganese sulfate just occupies 80% ratio,
This is also the main aspect of manganese sulfate consumption, and it is widely used in the industries such as industry, electronics, light industry, animal husbandry and agricultural.
Manganese sulfate is at home a kind of commercial industry product, is divided into technical grade sulfuric acid manganese and feed grade manganese sulfate.Industrial manganic sulfate master
If the raw material of the synthesis material of ink, paint, terebine, the catalyst of synthetic fatty acid and other manganese salts, and
For industrial departments such as electronics, metallurgical and national defence.Feed grade manganese sulfate is mainly used in feed industry, is added as formula feed
The raw material of agent.With the fast development of battery industry, problem in the urgent need to address is to produce high performance anode
Material.Thus propose the quality requirement to high-purity manganese sulphate.The main purposes of LITHIUM BATTERY high purity manganese sulfate is to be applied to nickel
The synthesis of cobalt manganic acid lithium tertiary cathode material and manganate cathode material for lithium.
Country's production of manganese sulfate as at present, mainly with pyrolusite as raw material, point roasting reduction (carbon reduction, sulphur reduction) and
Wet reducing (reducing agent such as troilite, ferrous sulfate or titanium white waste acid) two kinds of reducing leaching technologies of acidleach, then simply
Oxidation neutralize except iron, vulcanization removing heavy metals, filter, staticly settle, solution crystallization, centrifugal dehydration drying, obtain technical grade, raise
Material level and fine work three kinds of ranks of level.The production of the domestic high purity manganese sulfate of restriction is mainly in purification calcium and magnesium and potassium sodium technology.
Having corresponding technical finesse these impurity makes product reach requirement, but needs strict controlling reaction temperature and pH value, and consumption is a large amount of
The removal of impurities medicament of high-purity, is unfavorable for reducing production cost.
The content of the invention
In view of this, it is an object of the invention to provide a kind of production method of high-purity manganese sulphate, can simplify and prepare
The purification problem of solution, makes solution quality be guaranteed, and reduce production cost in journey.
The technical scheme is that：A kind of production method of high-purity manganese sulphate, comprises the following steps：
(1) by electrolytic manganese dioxide (more than 90%) is broken, washing, be milled after drying, sulphur milling；
(2) the electrolytic manganese dioxide powder and Cosan for obtaining step (1) are by 1：0.3~1：0.5 well mixed is put into porcelain
In ware, porcelain dish is put into and is had warmed up to 630 DEG C of Muffle kiln roasting certain hours, produce manganese monoxide；
(3) manganese monoxide that step (2) is obtained is poured into the beaker equipped with pure water from porcelain dish while hot, is stirred
Filtered after certain hour, obtain manganese monoxide filter cake；
(4) the another beaker that takes adds pure water and analytical pure sulfuric acid, and stirring is lower slowly repeatedly to add the regulation of manganese monoxide filter cake
PH value to stopping after 5.2 is added, and obtains the manganese sulfate solution for having leached；
(5) by the manganese sulfate solution filtering of having leached of obtaining of step (4), take filtrate by it condensing crystallizing in 100 DEG C,
When filtrate is evaporated soon, manganese sulfate monohydrate crystal is filtrated to get while hot, mother liquor returns to next condensing crystallizing again.
Preferably, electrolytic manganese dioxide is 100g in the step (1).
Preferably, electrolytic manganese dioxide is milled to 200 mesh, sulphur and is milled to 100 mesh in the step (1).
Preferably, roasting time is 25min in the step (2).
Preferably, pure water is 200ml in the step (3).
Preferably, mixing time is 30min in the step (3).
Preferably, pure water and analytical pure sulfuric acid are respectively 200ml and 60g in the step (4).
Compared with prior art, the present invention has the advantages that：
1. the advantage of the invention is that using electrolytic manganese dioxide as raw material, eliminate calcium and magnesium potassium sodium iron in raw material and
Heavy metal ion, simplifies the purification problem of solution in high purity manganese sulfate preparation process, and solution quality is guaranteed, final products
Purity reaches more than 99.5%, and potassium sodium calcium and magnesium impurity is respectively less than 50ppm；
2. the present invention will not bring new impurity into using sulphur reduction, and the sulfur dioxide gas of generation can produce sulfuric acid
Return to during electrolytic manganese dioxide preamble prepares manganese sulfate solution operation, or production analytical pure sulfuric acid is used for leaching manganese monoxide
Prepare high purity manganese sulfate；
3. the manganese monoxide that the present invention is produced has been calcined and be added to immediately stirring reaction in pure water, has completely cut off air by an oxygen
Change manganese and be oxidized to manganese dioxide, while washing can further remove the calcium and magnesium being mingled with electrolytic manganese dioxide.
Specific embodiment
With reference to specific embodiment, the present invention will be further described.
Embodiment 1
A kind of production method of high-purity manganese sulphate, comprises the following steps：
(1) by 100g electrolytic manganese dioxides (more than 90%) are broken, washing, be milled to 200 mesh, 40g sulphur mill after drying
Powder is to 100 mesh.
(2) electrolytic manganese dioxide powder and Cosan are well mixed by 1: 0.4 and are put into porcelain dish, porcelain dish is put into and is had warmed up
To 630 DEG C of Muffle kiln roasting 25min, manganese monoxide is produced.
(3) manganese monoxide is poured into the beaker equipped with 200ml pure water from porcelain dish while hot, stir 30min when
Between after filtering, obtain manganese monoxide filter cake.
(4) the another beaker that takes adds 200ml pure water and 60g analytical pure sulfuric acids, and stirring is lower slowly repeatedly to add manganese monoxide
Filter cake adjusts pH value to stopping after 5.2 and adds, and obtains the manganese sulfate solution for having leached.
(5) will leach manganese sulfate solution filtering, take filtrate by it condensing crystallizing in 100 DEG C, treat that filtrate is evaporated soon
When, manganese sulfate monohydrate crystal is filtrated to get while hot, mother liquor returns to next condensing crystallizing again.
Embodiment 2
High-purity manganese sulphate is obtained according to the preparation method described in embodiment 1, as different from Example 1, in step (1)
The ratio for taking electrolytic manganese dioxide 100g, sulphur 30g and electrolytic manganese dioxide powder and Cosan is 1: 0.3.
Embodiment 3
High-purity manganese sulphate is obtained according to the preparation method described in embodiment 1, as different from Example 1, in step (1)
The ratio for taking electrolytic manganese dioxide 100g, sulphur 50g and electrolytic manganese dioxide powder and Cosan is 1: 0.5.
The above embodiments are only the preferred embodiments of the present invention, it is impossible to interest field of the invention is limited with this, because
This, modification, equivalent variations, improvement for being made according to scope of the present invention patent etc. still belong to the scope that the present invention is covered.
Claims (7)
1. a kind of production method of high-purity manganese sulphate, it is characterised in that comprise the following steps：
(1) by electrolytic manganese dioxide (more than 90%) is broken, washing, be milled after drying, sulphur milling；
(2) the electrolytic manganese dioxide powder and Cosan for obtaining step (1) are well mixed by 1: 0.3~1: 0.5 and are put into porcelain dish,
Porcelain dish is put into and is had warmed up to 630 DEG C of Muffle kiln roasting certain hours, produce manganese monoxide；
(3) manganese monoxide that step (2) is obtained is poured into the beaker equipped with pure water from porcelain dish while hot, is stirred certain
Filtered after time, obtain manganese monoxide filter cake；
(4) the another beaker that takes adds pure water and analytical pure sulfuric acid, and stirring is lower slowly repeatedly to add manganese monoxide filter cake regulation pH value
Stop adding after to 5.2, and obtain the manganese sulfate solution for having leached；
(5) by the manganese sulfate solution filtering of having leached of obtaining of step (4), take filtrate by it condensing crystallizing in 100 DEG C, it is to be filtered
When liquid is evaporated soon, manganese sulfate monohydrate crystal is filtrated to get while hot, mother liquor returns to next condensing crystallizing again.
2. the production method of a kind of high-purity manganese sulphate according to claim 1, it is characterised in that in the step (1)
Electrolytic manganese dioxide is 100g.
3. the production method of a kind of high-purity manganese sulphate according to claim 1, it is characterised in that in the step (1)
Electrolytic manganese dioxide is milled to 200 mesh, sulphur and is milled to 100 mesh.
4. the production method of a kind of high-purity manganese sulphate according to claim 1, it is characterised in that in the step (2)
Roasting time is 25min.
5. the production method of a kind of high-purity manganese sulphate according to claim 1, it is characterised in that in the step (3)
Pure water is 200ml.
6. the production method of a kind of high-purity manganese sulphate according to claim 1, it is characterised in that in the step (3)
Mixing time is 30min.
7. the production method of a kind of high-purity manganese sulphate according to claim 1, it is characterised in that in the step (4)
Pure water and analytical pure sulfuric acid are respectively 200ml and 60g.
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| CN201611150554.5A CN106745288A (en) | 2016-12-14 | 2016-12-14 | A kind of production method of high-purity manganese sulphate |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107963669A (en) * | 2018-01-08 | 2018-04-27 | 中南大学 | A kind of calcium removal methods of technical grade sulfuric acid manganese |
| CN116375094A (en) * | 2023-05-10 | 2023-07-04 | 四川大学 | Method for preparing high-purity manganese sulfate by using manganese dioxide and sulfur |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320665A (en) * | 2011-07-27 | 2012-01-18 | 姚茂君 | Application of secondary air to process for reducing pyrolusite and producing sulfuric acid in fluidized bed furnace |
| CN102424365A (en) * | 2011-07-27 | 2012-04-25 | 刘集贵 | Recycling method of tail gas from pyrolusite reduction and sulfuric acid coproduction in fluidized bed furnace |
-
2016
- 2016-12-14 CN CN201611150554.5A patent/CN106745288A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102320665A (en) * | 2011-07-27 | 2012-01-18 | 姚茂君 | Application of secondary air to process for reducing pyrolusite and producing sulfuric acid in fluidized bed furnace |
| CN102424365A (en) * | 2011-07-27 | 2012-04-25 | 刘集贵 | Recycling method of tail gas from pyrolusite reduction and sulfuric acid coproduction in fluidized bed furnace |
Non-Patent Citations (1)
| Title |
|---|
| 无名: ""氧化锰法制硫酸锰"", 《无机盐工业》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107963669A (en) * | 2018-01-08 | 2018-04-27 | 中南大学 | A kind of calcium removal methods of technical grade sulfuric acid manganese |
| CN116375094A (en) * | 2023-05-10 | 2023-07-04 | 四川大学 | Method for preparing high-purity manganese sulfate by using manganese dioxide and sulfur |
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