CN108217746A - The method of high purity manganese sulfate and its product obtained are prepared with manganese carbonate miberal powder - Google Patents

The method of high purity manganese sulfate and its product obtained are prepared with manganese carbonate miberal powder Download PDF

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Publication number
CN108217746A
CN108217746A CN201611194542.2A CN201611194542A CN108217746A CN 108217746 A CN108217746 A CN 108217746A CN 201611194542 A CN201611194542 A CN 201611194542A CN 108217746 A CN108217746 A CN 108217746A
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manganese sulfate
sulfate solution
added
filtering
manganese
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CN201611194542.2A
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周芳
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Hengyang Rui Lin Manganese Technology Development Co Ltd
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Hengyang Rui Lin Manganese Technology Development Co Ltd
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Priority to CN201611194542.2A priority Critical patent/CN108217746A/en
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    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01GCOMPOUNDS CONTAINING METALS NOT COVERED BY SUBCLASSES C01D OR C01F
    • C01G45/00Compounds of manganese
    • C01G45/10Sulfates
    • CCHEMISTRY; METALLURGY
    • C01INORGANIC CHEMISTRY
    • C01PINDEXING SCHEME RELATING TO STRUCTURAL AND PHYSICAL ASPECTS OF SOLID INORGANIC COMPOUNDS
    • C01P2006/00Physical properties of inorganic compounds
    • C01P2006/80Compositional purity

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  • Chemical & Material Sciences (AREA)
  • Organic Chemistry (AREA)
  • Inorganic Chemistry (AREA)
  • Inorganic Compounds Of Heavy Metals (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

With manganese carbonate miberal powder prepare high purity manganese sulfate method and its product obtained, method and step it is as follows:The first step takes raw material to calcine after vulcanization Ore Leaching;Second step, removal of impurities;Third walks, purification;Up to the present invention.Not only raw material is easy to get the present invention, and production method is simple, easy to operation, solves the separation problem of heavy metal, can significantly reduce common manganese sulfate product beavy metal impurity content, particularly to removal potassium, sodium impurity it is with obvious effects, and obtain the extremely low manganese sulfate of potassium, sodium impurity content.

Description

The method of high purity manganese sulfate and its product obtained are prepared with manganese carbonate miberal powder
Technical field
The present invention relates to a kind of production method of chemical products, the method that high purity manganese sulfate is especially prepared with manganese carbonate miberal powder 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 offer prepares high purity manganese sulfate with manganese carbonate miberal powder Method and its product obtained.
Realizing above-mentioned purpose scheme of the present invention is:The method of high purity manganese sulfate and its production obtained are prepared with manganese carbonate miberal powder Product, method and step are as follows:
The first step:Manganese carbonate miberal powder with coal dust is mixed according to a certain percentage, is calcined;
Second step:44-55% sulfuric acid is added in, 75-85 DEG C or so, 1.4-1.6 atmospheric pressure is stirred to react, and filtering obtains sulphur Sour manganese solution;
Third walks:The manganese sulfate solution of second step is added in into cleaner MnF2, by adjusting pH value, goes calcium and magnesium ion It after removing, precipitates, filtering;
4th step:The manganese sulfate solution of third step is added in into cleaner MnS, by adjusting pH value, makes potassium, sodium ion removal Afterwards, it precipitates, filtering;
5th step:The manganese sulfate solution of 4th step is added in into cleaner FeF3, by adjusting pH value, makes calcium, magnesium, potassium, sodium Ion further after removal, precipitates, filtering;
6th step:By the manganese sulfate solution after removal of impurities, filtrate is concentrated, stands still for crystals, filters to get product of the present invention.
Further technical solution is the present invention:
The first step:Manganese carbonate miberal powder with coal dust is mixed according to a certain percentage, is calcined;
Second step:55% sulfuric acid is added in, 85 DEG C or so, 1.6 atmospheric pressure are stirred to react, and filtering obtains manganese sulfate solution;
Third walks:The manganese sulfate solution of second step is added in into cleaner MnF2, by adjusting pH value, goes calcium and magnesium ion It after removing, precipitates, filtering;
4th step:The manganese sulfate solution of third step is added in into cleaner MnS, by adjusting pH value, makes potassium, sodium ion removal Afterwards, it precipitates, filtering;
5th step:The manganese sulfate solution of 4th step is added in into cleaner FeF3, by adjusting pH value, makes calcium, magnesium, potassium, sodium Ion further after removal, precipitates, filtering;
6th step:By the manganese sulfate solution after removal of impurities, filtrate is concentrated, stands still for crystals, filters to get product of the present invention.
Further technical solution is the present invention:
Its method and step is as follows:
The first step:Manganese carbonate miberal powder with coal dust is mixed according to a certain percentage, is calcined;
Second step:44% sulfuric acid is added in, 75 DEG C or so, 1.4 atmospheric pressure are stirred to react, and filtering obtains manganese sulfate solution;
Third walks:The manganese sulfate solution of second step is added in into cleaner MnF2, by adjusting pH value, goes calcium and magnesium ion It after removing, precipitates, filtering;
4th step:The manganese sulfate solution of third step is added in into cleaner MnS, by adjusting pH value, makes potassium, sodium ion removal Afterwards, it precipitates, filtering;
5th step:The manganese sulfate solution of 4th step is added in into cleaner FeF3, by adjusting pH value, makes calcium, magnesium, potassium, sodium Ion further after removal, precipitates, filtering;
6th step:By the manganese sulfate solution after removal of impurities, filtrate is concentrated, stands still for crystals, filters 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:Manganese carbonate miberal powder with coal dust is mixed according to a certain percentage, is calcined;
Second step:50% sulfuric acid is added in, 80 DEG C or so, 1.5 atmospheric pressure are stirred to react, and filtering obtains manganese sulfate solution;
Third walks:The manganese sulfate solution of second step is added in into cleaner MnF2, by adjusting pH value, goes calcium and magnesium ion It after removing, precipitates, filtering;
4th step:The manganese sulfate solution of third step is added in into cleaner MnS, by adjusting pH value, makes potassium, sodium ion removal Afterwards, it precipitates, filtering;
5th step:The manganese sulfate solution of 4th step is added in into cleaner FeF3, by adjusting pH value, makes calcium, magnesium, potassium, sodium Ion further after removal, precipitates, filtering;
6th step:By the manganese sulfate solution after removal of impurities, filtrate is concentrated, stands still for crystals, filters 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, and production method is simple, is convenient for Operation, solves the separation problem of heavy metal, common manganese sulfate product beavy metal impurity content can be significantly reduced, particularly to going Except potassium, sodium impurity it is with obvious effects, and obtain the extremely low manganese sulfate of potassium, sodium impurity content.
The present invention is further described below in conjunction with specific embodiment.
Specific embodiment
Embodiment 1
With manganese carbonate miberal powder prepare high purity manganese sulfate method and its product obtained, method and step it is as follows:
The first step:Manganese carbonate miberal powder with coal dust is mixed according to a certain percentage, is calcined;
Second step:55% sulfuric acid is added in, 85 DEG C or so, 1.6 atmospheric pressure are stirred to react, and filtering obtains manganese sulfate solution;
Third walks:The manganese sulfate solution of second step is added in into cleaner MnF2, by adjusting pH value, goes calcium and magnesium ion It after removing, precipitates, filtering;
4th step:The manganese sulfate solution of third step is added in into cleaner MnS, by adjusting pH value, makes potassium, sodium ion removal Afterwards, it precipitates, filtering;
5th step:The manganese sulfate solution of 4th step is added in into cleaner FeF3, by adjusting pH value, makes calcium, magnesium, potassium, sodium Ion further after removal, precipitates, filtering;
6th step:By the manganese sulfate solution after removal of impurities, filtrate is concentrated, stands still for crystals, filters to get product of the present invention.
Embodiment 2
With manganese carbonate miberal powder prepare high purity manganese sulfate method and its product obtained, method and step it is as follows:
The first step:Manganese carbonate miberal powder with coal dust is mixed according to a certain percentage, is calcined;
Second step:44% sulfuric acid is added in, 75 DEG C or so, 1.4 atmospheric pressure are stirred to react, and filtering obtains manganese sulfate solution;
Third walks:The manganese sulfate solution of second step is added in into cleaner MnF2, by adjusting pH value, goes calcium and magnesium ion It after removing, precipitates, filtering;
4th step:The manganese sulfate solution of third step is added in into cleaner MnS, by adjusting pH value, makes potassium, sodium ion removal Afterwards, it precipitates, filtering;
5th step:The manganese sulfate solution of 4th step is added in into cleaner FeF3, by adjusting pH value, makes calcium, magnesium, potassium, sodium Ion further after removal, precipitates, filtering;
6th step:By the manganese sulfate solution after removal of impurities, filtrate is concentrated, stands still for crystals, filters to get product of the present invention.
Embodiment 3
With manganese carbonate miberal powder prepare high purity manganese sulfate method and its product obtained, method and step it is as follows:
Its method and step is as follows:
The first step:Manganese carbonate miberal powder with coal dust is mixed according to a certain percentage, is calcined;
Second step:50% sulfuric acid is added in, 80 DEG C or so, 1.5 atmospheric pressure are stirred to react, and filtering obtains manganese sulfate solution;
Third walks:The manganese sulfate solution of second step is added in into cleaner MnF2, by adjusting pH value, goes calcium and magnesium ion It after removing, precipitates, filtering;
4th step:The manganese sulfate solution of third step is added in into cleaner MnS, by adjusting pH value, makes potassium, sodium ion removal Afterwards, it precipitates, filtering;
5th step:The manganese sulfate solution of 4th step is added in into cleaner FeF3, by adjusting pH value, makes calcium, magnesium, potassium, sodium Ion further after removal, precipitates, filtering;
6th step:By the manganese sulfate solution after removal of impurities, filtrate is concentrated, stands still for crystals, filters 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. the method for high purity manganese sulfate is prepared with manganese carbonate miberal powder, it is characterized in that:
Its method and step is as follows:
The first step:Manganese carbonate miberal powder with coal dust is mixed according to a certain percentage, is calcined;
Second step:44-55% sulfuric acid is added in, 75-85 DEG C or so, 1.4-1.6 atmospheric pressure is stirred to react, and filtering obtains manganese sulfate Solution;
Third walks:The manganese sulfate solution of second step is added in into cleaner MnF2, by adjusting pH value, after removing calcium and magnesium ion, Precipitation, filtering;
4th step:The manganese sulfate solution of third step is added in into cleaner MnS, by adjusting pH value, after making potassium, sodium ion removal, Precipitation, filtering;
5th step:The manganese sulfate solution of 4th step is added in into cleaner FeF3, by adjusting pH value, makes calcium, magnesium, potassium, sodium ion It further after removal, precipitates, filtering;
6th step:By the manganese sulfate solution after removal of impurities, filtrate is concentrated, stands still for crystals, filters to get product of the present invention.
2. the method for high purity manganese sulfate is prepared with manganese carbonate miberal powder as described in claim 1, it is characterized in that:
Its method and step is as follows:
The first step:Manganese carbonate miberal powder with coal dust is mixed according to a certain percentage, is calcined;
Second step:55% sulfuric acid is added in, 85 DEG C or so, 1.6 atmospheric pressure are stirred to react, and filtering obtains manganese sulfate solution;
Third walks:The manganese sulfate solution of second step is added in into cleaner MnF2, by adjusting pH value, after removing calcium and magnesium ion, Precipitation, filtering;
4th step:The manganese sulfate solution of third step is added in into cleaner MnS, by adjusting pH value, after making potassium, sodium ion removal, Precipitation, filtering;
5th step:The manganese sulfate solution of 4th step is added in into cleaner FeF3, by adjusting pH value, makes calcium, magnesium, potassium, sodium ion It further after removal, precipitates, filtering;
6th step:By the manganese sulfate solution after removal of impurities, filtrate is concentrated, stands still for crystals, filters to get product of the present invention.
3. the method for high purity manganese sulfate is prepared with manganese carbonate miberal powder as described in claim 1, it is characterized in that:
Its method and step is as follows:
The first step:Manganese carbonate miberal powder with coal dust is mixed according to a certain percentage, is calcined;
Second step:44% sulfuric acid is added in, 75 DEG C or so, 1.4 atmospheric pressure are stirred to react, and filtering obtains manganese sulfate solution;
Third walks:The manganese sulfate solution of second step is added in into cleaner MnF2, by adjusting pH value, after removing calcium and magnesium ion, Precipitation, filtering;
4th step:The manganese sulfate solution of third step is added in into cleaner MnS, by adjusting pH value, after making potassium, sodium ion removal, Precipitation, filtering;
5th step:The manganese sulfate solution of 4th step is added in into cleaner FeF3, by adjusting pH value, makes calcium, magnesium, potassium, sodium ion It further after removal, precipitates, filtering;
6th step:By the manganese sulfate solution after removal of impurities, filtrate is concentrated, stands still for crystals, filters to get product of the present invention.
4. the method for high purity manganese sulfate is prepared with manganese carbonate miberal powder as described in claim 1, it is characterized in that:
Its method and step is as follows:
The first step:Manganese carbonate miberal powder with coal dust is mixed according to a certain percentage, is calcined;
Second step:50% sulfuric acid is added in, 80 DEG C or so, 1.5 atmospheric pressure are stirred to react, and filtering obtains manganese sulfate solution;
Third walks:The manganese sulfate solution of second step is added in into cleaner MnF2, by adjusting pH value, after removing calcium and magnesium ion, Precipitation, filtering;
4th step:The manganese sulfate solution of third step is added in into cleaner MnS, by adjusting pH value, after making potassium, sodium ion removal, Precipitation, filtering;
5th step:The manganese sulfate solution of 4th step is added in into cleaner FeF3, by adjusting pH value, makes calcium, magnesium, potassium, sodium ion It further after removal, precipitates, filtering;
6th step:By the manganese sulfate solution after removal of impurities, filtrate is concentrated, stands still for crystals, filters 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.
CN201611194542.2A 2016-12-21 2016-12-21 The method of high purity manganese sulfate and its product obtained are prepared with manganese carbonate miberal powder Pending CN108217746A (en)

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Application Number Priority Date Filing Date Title
CN201611194542.2A CN108217746A (en) 2016-12-21 2016-12-21 The method of high purity manganese sulfate and its product obtained are prepared with manganese carbonate miberal powder

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CN108217746A true CN108217746A (en) 2018-06-29

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