CN108217739A - It is a kind of to prepare the method for manganese sulfate and its product obtained with troilite - Google Patents
It is a kind of to prepare the method for manganese sulfate and its product obtained with troilite Download PDFInfo
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- CN108217739A CN108217739A CN201611194408.2A CN201611194408A CN108217739A CN 108217739 A CN108217739 A CN 108217739A CN 201611194408 A CN201611194408 A CN 201611194408A CN 108217739 A CN108217739 A CN 108217739A
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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
It is a kind of with troilite prepare manganese sulfate method and its product obtained, method and step it is as follows：The first step takes raw material to add sulfuric acid leaching；Second step, removal of impurities；Third walks, using crystallization；Up to the present invention.Not only raw material is easy to get the present invention, makes simply, easy to operation, solves the separation problem of heavy metal, the content of common manganese sulfate product beavy metal impurity can be significantly reduced, particularly to going deliming, magnesium addition with obvious effects, obtains the extremely low manganese sulfate of calcium, magnesium addition content.
Description
Technical field
The present invention relates to a kind of production method of chemical products, it is especially a kind of with troilite prepare manganese sulfate method and its
Product obtained.
Background technology
Manganese sulfate is a kind of traditional manganese salt product, and purposes is very extensive.At present, domestic production of manganese sulfate as, mainly
Using pyrolusite as raw material, divide carbon fire reduction and wet reducing (reducing agents such as troilite, ferrous sulfate or titanium white waste acid) acidleach
Then two kinds of reducing leaching technologies carry out simply oxidation-hydrolysis except iron, vulcanization removing heavy metals again, filtering stands and sinks
Form sediment, solution crystallization, centrifugal dehydration drying, obtain technical grade, three kinds of ranks of feed grade or fine work grade manganese sulfate product, for changing
The fields such as fertilizer, feed, paint, pesticide.In recent years, with the development of New Energy Sources lithium manganate battery technology, with high-purity sulphuric acid
Manganese produces LiMn2O4 for raw material and is increasingly taken seriously, and technology is also more and more ripe.And foreign countries are for environmental protection, cost
The consideration of the various reasons such as consumption, the particularly developed countries such as America and Europe, Japan and Korea S, produce almost without manganese sulfate；China has become generation
Main manganese sulfate producing country and supply country in boundary, about 150,000 tons of annual output.Therefore, overseas lithium manganate battery manufacturer wishes
High-purity sulfuric acid manganese material is found by China, for the lithium battery that taps a new source of energy.
China's production of manganese sulfate as technology, either wet method or pyrogenic process, the main content of product produced is low, impurity
Content is high, is much unable to reach more than high purity manganese sulfate technical requirement.
Invention content
The purpose of the present invention is overcoming the above-mentioned deficiency of the prior art, and provide a kind of side that manganese sulfate is prepared with troilite
Method and its product obtained.
Realizing above-mentioned purpose scheme of the present invention is：It is a kind of to prepare the method for manganese sulfate and its product obtained with troilite,
Its method and step is as follows：
The first step：Using troilite as raw material, after adding sulfuric acid leaching, the manganese sulfate for being tuned into a concentration of 300g/L~600g/L is molten
Liquid is stood；
Second step：Cleaner MnF2, deliming, magnesium addition are added in, the dosage of MnF2 is the 100%- of impurity theoretical amount
200%, the pH value 6-12 of solution is maintained, is reacted 1-3 hours at a temperature of being maintained at 30 DEG C -90 DEG C；
Third walks：Add in cleaner MnS again into second step solution, except Co, Ni, Pb, Cd or Cr beavy metal impurity,
The dosage of MnS or manganese powder is the 100%-200% of impurity theoretical amount, maintains the pH value 6-12 of solution, is maintained at 30 DEG C -90
It is reacted 1-3 hours at a temperature of DEG C, the introducing of impurity can be avoided by making cleaner with MnF2 and MnS；
4th step：By the solution filtering of third step, normal pressure concentration, crystallization, dehydration, it is dry after to get product of the present invention.
Further technical solution is the present invention：
Its method and step is as follows：
The first step：Using troilite as raw material, after adding sulfuric acid leaching, the manganese sulfate solution of a concentration of 600g/L is tuned into, is stood；
Second step：Cleaner MnF2, deliming, magnesium addition are added in, the dosage of MnF2 is the 200% of impurity theoretical amount, is maintained
The pH value 12 of solution is reacted 3 hours at a temperature of being maintained at 90 DEG C；
Third walks：Add in cleaner MnS again into second step solution, except Co, Ni, Pb, Cd or Cr beavy metal impurity,
The dosage of MnS or manganese powder is the 200% of impurity theoretical amount, maintains the pH value 12 of solution, anti-at a temperature of being maintained at 90 DEG C
It answers 3 hours, the introducing of impurity can be avoided by making cleaner with MnF2 and MnS；
4th step：By the solution filtering of third step, normal pressure concentration, crystallization, dehydration, it is dry after to get product of the present invention.
Further technical solution is the present invention：
Its method and step is as follows：
The first step：Using troilite as raw material, after adding sulfuric acid leaching, the manganese sulfate solution of a concentration of 300g/L is tuned into, is stood；
Second step：Cleaner MnF2, deliming, magnesium addition are added in, the dosage of MnF2 is the 100% of impurity theoretical amount, is maintained
The pH value 6 of solution is reacted 1 hour at a temperature of being maintained at 30 DEG C；
Third walks：Add in cleaner MnS again into second step solution, except Co, Ni, Pb, Cd or Cr beavy metal impurity,
The dosage of MnS or manganese powder is the 100% of impurity theoretical amount, maintains the pH value 6 of solution, is reacted at a temperature of being maintained at 30 DEG C
1 hour, the introducing of impurity can be avoided by making cleaner with MnF2 and MnS；
4th step：By the solution filtering of third step, normal pressure concentration, crystallization, dehydration, it is dry after to get product of the present invention.
Technical solution of the invention further can also be：
Its method and step is as follows：
The first step：Using troilite as raw material, after adding sulfuric acid leaching, the manganese sulfate solution of a concentration of 450g/L is tuned into, is stood；
Second step：Cleaner MnF2, deliming, magnesium addition are added in, the dosage of MnF2 is the 150% of impurity theoretical amount, is maintained
The pH value 8 of solution is reacted 1.5 hours at a temperature of being maintained at 75 DEG C；
Third walks：Add in cleaner MnS again into second step solution, except Co, Ni, Pb, Cd or Cr beavy metal impurity,
The dosage of MnS or manganese powder is the 150% of impurity theoretical amount, maintains the pH value 8 of solution, is reacted at a temperature of being maintained at 75 DEG C
1.5 hours, the introducing of impurity can be avoided by making cleaner with MnF2 and MnS；
4th step：By the solution filtering of third step, normal pressure concentration, crystallization, dehydration, it is dry after to get product of the present invention.
The present invention has the following advantages that compared with prior art：Not only raw material is easy to get the present invention, makes simply, convenient for behaviour
Make, solve the separation problem of heavy metal, the content of common manganese sulfate product beavy metal impurity can be significantly reduced, particularly to going
Deliming, magnesium addition are with obvious effects, obtain the extremely low manganese sulfate of calcium, magnesium addition content.
The present invention is further described below in conjunction with specific embodiment.
Specific embodiment
Embodiment 1
It is a kind of with troilite prepare manganese sulfate method and its product obtained, method and step it is as follows：
The first step：Using troilite as raw material, after adding sulfuric acid leaching, the manganese sulfate solution of a concentration of 600g/L is tuned into, is stood；
Second step：Cleaner MnF2, deliming, magnesium addition are added in, the dosage of MnF2 is the 200% of impurity theoretical amount, is maintained
The pH value 12 of solution is reacted 3 hours at a temperature of being maintained at 90 DEG C；
Third walks：Add in cleaner MnS again into second step solution, except Co, Ni, Pb, Cd or Cr beavy metal impurity,
The dosage of MnS or manganese powder is the 200% of impurity theoretical amount, maintains the pH value 12 of solution, anti-at a temperature of being maintained at 90 DEG C
It answers 3 hours, the introducing of impurity can be avoided by making cleaner with MnF2 and MnS；
4th step：By the solution filtering of third step, normal pressure concentration, crystallization, dehydration, it is dry after to get product of the present invention.
Embodiment 2
It is a kind of with troilite prepare manganese sulfate method and its product obtained, method and step it is as follows：
The first step：Using troilite as raw material, after adding sulfuric acid leaching, the manganese sulfate solution of a concentration of 300g/L is tuned into, is stood；
Second step：Cleaner MnF2, deliming, magnesium addition are added in, the dosage of MnF2 is the 100% of impurity theoretical amount, is maintained
The pH value 6 of solution is reacted 1 hour at a temperature of being maintained at 30 DEG C；
Third walks：Add in cleaner MnS again into second step solution, except Co, Ni, Pb, Cd or Cr beavy metal impurity,
The dosage of MnS or manganese powder is the 100% of impurity theoretical amount, maintains the pH value 6 of solution, is reacted at a temperature of being maintained at 30 DEG C
1 hour, the introducing of impurity can be avoided by making cleaner with MnF2 and MnS；
4th step：By the solution filtering of third step, normal pressure concentration, crystallization, dehydration, it is dry after to get product of the present invention.
Embodiment 3
It is a kind of with troilite prepare manganese sulfate method and its product obtained, method and step it is as follows：
The first step：Using troilite as raw material, after adding sulfuric acid leaching, the manganese sulfate solution of a concentration of 450g/L is tuned into, is stood；
Second step：Cleaner MnF2, deliming, magnesium addition are added in, the dosage of MnF2 is the 150% of impurity theoretical amount, is maintained
The pH value 8 of solution is reacted 1.5 hours at a temperature of being maintained at 75 DEG C；
Third walks：Add in cleaner MnS again into second step solution, except Co, Ni, Pb, Cd or Cr beavy metal impurity,
The dosage of MnS or manganese powder is the 150% of impurity theoretical amount, maintains the pH value 8 of solution, is reacted at a temperature of being maintained at 75 DEG C
1.5 hours, the introducing of impurity can be avoided by making cleaner with MnF2 and MnS；
4th step：By the solution filtering of third step, normal pressure concentration, crystallization, dehydration, it is dry after to get product of the present invention.
The above only to presently preferred embodiments of the present invention, not limits the present invention,
Any person skilled in the art is changed or is modified as what is changed on an equal basis possibly also with the technology contents of the disclosure above
Equivalent embodiment, every content for not departing from the present invention program, technical spirit according to the present invention are made to the above embodiment
Any simple modification, equivalent variations and remodeling, all fall in protection scope of the present invention.
Claims (5)
1. a kind of method that manganese sulfate is prepared with troilite, it is characterized in that:
Its method and step is as follows：
The first step：Using troilite as raw material, after adding sulfuric acid leaching, the manganese sulfate solution of a concentration of 300g/L~600g/L is tuned into,
It stands；
Second step：Cleaner MnF2, deliming, magnesium addition are added in, the dosage of MnF2 is the 100%-200% of impurity theoretical amount, dimension
The pH value 6-12 of solution is held, is reacted 1-3 hours at a temperature of being maintained at 30 DEG C -90 DEG C；
Third walks：Add in cleaner MnS again into second step solution, except Co, Ni, Pb, Cd or Cr beavy metal impurity, MnS or
The dosage of manganese powder is the 100%-200% of impurity theoretical amount, maintains the pH value 6-12 of solution, is maintained at 30 DEG C -90 DEG C
At a temperature of react 1-3 hours, the introducing of impurity can be avoided by making cleaner with MnF2 and MnS；
4th step：By the solution filtering of third step, normal pressure concentration, crystallization, dehydration, it is dry after to get product of the present invention.
2. the method for manganese sulfate is prepared with troilite as described in claim 1, it is characterized in that：
Its method and step is as follows：
The first step：Using troilite as raw material, after adding sulfuric acid leaching, the manganese sulfate solution of a concentration of 600g/L is tuned into, is stood；
Second step：Cleaner MnF2, deliming, magnesium addition are added in, the dosage of MnF2 is the 200% of impurity theoretical amount, maintains solution
PH value 12, reacted 3 hours at a temperature of being maintained at 90 DEG C；
Third walks：Add in cleaner MnS again into second step solution, except Co, Ni, Pb, Cd or Cr beavy metal impurity, MnS or
The dosage of manganese powder is the 200% of impurity theoretical amount, maintains the pH value 12 of solution, and it is small that 3 are reacted at a temperature of being maintained at 90 DEG C
When, the introducing of impurity can be avoided by making cleaner with MnF2 and MnS；
4th step：By the solution filtering of third step, normal pressure concentration, crystallization, dehydration, it is dry after to get product of the present invention.
3. the method for manganese sulfate is prepared with troilite as described in claim 1, it is characterized in that：
Its method and step is as follows：
The first step：Using troilite as raw material, after adding sulfuric acid leaching, the manganese sulfate solution of a concentration of 300g/L is tuned into, is stood；
Second step：Cleaner MnF2, deliming, magnesium addition are added in, the dosage of MnF2 is the 100% of impurity theoretical amount, maintains solution
PH value 6, reacted 1 hour at a temperature of being maintained at 30 DEG C；
Third walks：Add in cleaner MnS again into second step solution, except Co, Ni, Pb, Cd or Cr beavy metal impurity, MnS or
The dosage of manganese powder is the 100% of impurity theoretical amount, maintains the pH value 6 of solution, and it is small that 1 is reacted at a temperature of being maintained at 30 DEG C
When, the introducing of impurity can be avoided by making cleaner with MnF2 and MnS；
4th step：By the solution filtering of third step, normal pressure concentration, crystallization, dehydration, it is dry after to get product of the present invention.
4. the method for manganese sulfate is prepared with troilite as described in claim 1, it is characterized in that：
Its method and step is as follows：
The first step：Using troilite as raw material, after adding sulfuric acid leaching, the manganese sulfate solution of a concentration of 450g/L is tuned into, is stood；
Second step：Cleaner MnF2, deliming, magnesium addition are added in, the dosage of MnF2 is the 150% of impurity theoretical amount, maintains solution
PH value 8, reacted 1.5 hours at a temperature of being maintained at 75 DEG C；
Third walks：Add in cleaner MnS again into second step solution, except Co, Ni, Pb, Cd or Cr beavy metal impurity, MnS or
The dosage of manganese powder is the 150% of impurity theoretical amount, maintains the pH value 8 of solution, and it is small that 1.5 are reacted at a temperature of being maintained at 75 DEG C
When, the introducing of impurity can be avoided by making cleaner with MnF2 and MnS；
4th step：By the solution filtering of third step, normal pressure concentration, crystallization, dehydration, it is dry after to get product of the present invention.
5. a kind of utilize the manganese sulfate product as made from claim 1-4 any one of them methods, it is characterized in that：The sulfuric acid
The content of beary metal of manganese product is respectively less than 0.2ppm.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201611194408.2A CN108217739A (en) | 2016-12-21 | 2016-12-21 | It is a kind of to prepare the method for manganese sulfate and its product obtained with troilite |
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| CN201611194408.2A CN108217739A (en) | 2016-12-21 | 2016-12-21 | It is a kind of to prepare the method for manganese sulfate and its product obtained with troilite |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109502651A (en) * | 2018-12-28 | 2019-03-22 | 湖南有色金属研究院 | A method of purification prepares manganese sulfate and battery electrode manganese dioxide from the Zinc electrolysis earth of positive pole |
| CN110512075A (en) * | 2019-09-10 | 2019-11-29 | 河南豫光锌业有限公司 | A kind of method of cobaltous sulfate manganese mixed liquor deeply purifying and removing cadmium |
-
2016
- 2016-12-21 CN CN201611194408.2A patent/CN108217739A/en active Pending
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109502651A (en) * | 2018-12-28 | 2019-03-22 | 湖南有色金属研究院 | A method of purification prepares manganese sulfate and battery electrode manganese dioxide from the Zinc electrolysis earth of positive pole |
| CN110512075A (en) * | 2019-09-10 | 2019-11-29 | 河南豫光锌业有限公司 | A kind of method of cobaltous sulfate manganese mixed liquor deeply purifying and removing cadmium |
| CN110512075B (en) * | 2019-09-10 | 2021-06-08 | 河南豫光锌业有限公司 | Method for deeply purifying and removing cadmium from cobalt-manganese sulfate mixed liquid |
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Application publication date: 20180629 |