Method for high-purity manganese sulfate monohydrate
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A technology of manganese sulfate and pure one, applied in the field of preparation of high-purity manganese sulfate monohydrate, can solve the problems of high cost of raw materials and many metal impurities, and achieve the effect of less impurities and stable quality
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Problems solved by technology
[0003] The technical problem to be solved in the present invention is: to solve the problem of many ot
Method used
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Embodiment approach 1
[0025] A. Mix 1,000 grams of electrolytic manganese dioxide tail powder and 2 L of deionized water evenly, add 600 ml of concentrated sulfuric acid to stir and react, and separate solid and liquid; this step removes most of the impurities such as sulfates, carbonates, and sulfides.
[0026] B. Add 1800ml of 30% hydrogen peroxide and an appropriate amount of sulfuric acid to the solid isolate obtained in step A, keep the pH=3, and stir and react at normal temperature for 2 hours.
[0027] C. Gradually add barium hydroxide solution to the solution in step B, and keep stirring until PH = 5.4, then the solid-liquid separation.
[0028] D. According to the Pb content measured in the solution obtained by the solid-liquid separation in step C, add barium sulfide solution with a molar ratio of 2 times, stir evenly, heat to 60-80°C, and separate the solid and liquid.
[0029]
[0030] E. Add the solution obtained from solid-liquid separation in step D into coconut shell activated carb...
Embodiment approach 2
[0035] The difference from Embodiment 1 is that in step B, the pH is kept at 3.5, and the reaction is stirred at room temperature for 4 hours.
Embodiment approach 3
[0037] The difference from Embodiments 1 and 2 is that in step B, the pH is kept at 3, and the reaction is stirred at room temperature for 3 hours.
[0038] The various impurity contents that measure after the dried manganese sulfate monohydrate of above each embodiment gained are as following table:
[0039]
[0040] Note: The unit of the data in the table is ppm
[0041] It can be seen from the above table that the impurity content of the high-purity manganese sulfate products obtained in each embodiment of the present invention is relatively low, which can fully meet the needs of lithium battery positive electrode materials.
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Abstract
The invention relates to the preparation field of chemical products and particularly relates to a method for high-purity manganese sulfate monohydrate. The method specifically comprises the following steps of: taking tail powder of electrolytic manganese dioxide as a raw material, carrying out water washing and acid washing, then carrying out leaching and reducing on MnO2 by taking hydrogen peroxide as a reducing agent, adding barium hydroxide solution, removing Fe<3+>, Si<2+> and Al<3+>, adding barium sulfide solution into the obtained solution, heating the solution to 60-80 DEG C after uniform stirring, carrying out solid-liquid separation, and removing heavy metal elements such as Pb; adding activated carbon in the solution, carrying out stirring and solid-liquid separation at 60-80 DEG C, adding polyacrylamide as a flocculant into the solution after being subjected to activated carbon separation, standing for 24-36 hours after uniform stirring, and carrying out the solid-liquid separation; and carrying out high-temperature crystallization on the obtained solution so as to obtain a manganese sulfate monohydrate product. According to the method, the tail powder produced during the production of the electrolytic manganese dioxide is adequately utilized, the high-purity manganese sulfate monohydrate is produced at a relatively low cost, and then manganese sulfate for ternary materials applied to lithium battery industries is further obtained.
Description
technical field [0001] The invention relates to the field of preparation of chemical products, in particular to a preparation method of high-purity manganese sulfate monohydrate. Background technique [0002] Manganese sulfate is a basic chemical raw material. Manganese sulfate monohydrate can be obtained by drying at high temperature. Manganese sulfate used for ternary materials in the lithium battery industry has relatively strict requirements on indicators such as K, Na, Ca, Mg, Fe and heavy metals. There are many traditional methods for preparing manganese sulfate, but the prepared manganese sulfate often contains more metal impurities, which cannot meet the requirements of high-performance lithium batteries. CN102674467A discloses a preparation method of manganese sulfate. The method uses metal manganese as a raw material, through the 2 SO 4 React with MnS and remove other impurities to obtain high-purity manganese sulfate. This method uses high-purity metal manga...
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