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Preparation method of high-purity manganese sulfate

A manganese sulfate, high-purity technology, applied in manganese sulfate and other directions, can solve the problems of limited sources, reduced product purity, difficult removal of calcium and magnesium, etc., to reduce the chance of precipitation, low operating costs, and easy industrialization.

Pending Publication Date: 2021-11-30
四川沃林山水环保科技有限公司
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Problems solved by technology

But this process has the following disadvantages: (1), pyrolusite with low calcium and magnesium content is only produced in individual countries in Africa at present, and the source is very limited
Coupled with the current increase in shipping costs, the production cost of high-purity manganese sulfate has increased significantly
(2), in the recrystallization process, along with the evaporation of water, the concentration of calcium and magnesium in the solution also increases gradually, reaches a certain degree, calcium sulfate and magnesium sulfate and product manganese sulfate form eutectic precipitation, thereby reduced product purity
On the one hand, the removal cost of fluoride ions is relatively high, on the other hand, the restriction on the concentration of impurity fluorine ions is getting higher and higher, so this process cannot produce high-purity manganese sulfate products that meet the requirements
[0009] To sum up, in the production technologies of high-purity manganese sulfate that have been disclosed so far, except for using electrolytic manganese or pyrolusite with low calcium and magnesium content as raw materials, other processes have the problem that calcium and magnesium are difficult to remove, and the purity of manganese sulfate is difficult to meet the requirements.

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  • Preparation method of high-purity manganese sulfate

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[0034] The present invention provides a method of preparing high purity sulfate, and the method provided by the present invention can first remove calcium magnesium ions, and then remove heavy metal ions, and then remove heavy metal ions, then remove calcium magnesium ions, and will remove calcium magnesium first below The method of ion, re-removing heavy metal ions is recorded as a method, and the first removal of heavy metal ions will be removed, and the method of removing calcium magnesium ions is described as a method 2, respectively.

[0035] In the present invention, the method includes the steps of:

[0036] (1) Mix the crude manganese salt solution and pH control agent, adding a solution of ammonium bicarbonate solution to the obtained mixture, and after the addition of ammonium bicarbonate, the reaction mixture is sequentially expanded and solid-liquid separation, to obtain carbonated manganese;

[0037] (2) The manganese carbonate is dissolved in electron-level sulfuric ...

Embodiment 1

[0060] The manganese sulfate (Ca, Mg concentration of) (Ca, Mg concentration is 135 ppm and 406 ppm), and 400 g of ammonium chloride was dissolved in 2L water, and after stirring dissolved, the manganese concentration of the solution was adjusted to 100 g / L. The 1.5L solution was taken in a 10L glass reaction kettle, and heated to 102 ° C with a heat conductive oil interlayer. Under the conditions of retaining the solution temperature ≥ 102 ° C and continuously stirred, a 6 L of 30 ml / L (ammonium hydrogencarbonate: mole ratio 2.2: 1) was added to 30 mL per minute with a peristaltic pump. When necessary, the amount of boiling water is added to supplement the moisture loss due to evaporation. After the carbonate solution was completed, he was kept at 102 ° C for 1 h, and then naturally cooled to room temperature. Filter, the filter cake washed five times with high purity water. The filter cake was transferred to the beaker, slowly added 5 mol / L electron grade sulfuric acid sol...

Embodiment 2

[0062] The operation steps and Example 1 were exactly the same, only ammonium chloride was exchanged with ammonium chloride, and manganese sulfate was dried after vacuum 100 ° C.

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Abstract

The invention relates to the technical field of new energy ternary lithium battery positive electrode materials, and provides a preparation method of high-purity manganese sulfate, the preparation method comprises the following steps: controlling the pH value to 5-6 and the temperature to 100 DEG C or above in a manganese carbonate precipitation process, and removing calcium and magnesium ions in a crude manganese salt solution by using an ammonium bicarbonate solution under the conditions, then dissolving the obtained manganese carbonate precipitate in electronic-grade sulfuric acid, adding ammonium sulfide to remove heavy metal impurity ions, filtering, and evaporating the obtained filtrate to obtain the high-purity manganese sulfate. In addition, according to the method, heavy metal impurity ions can be removed firstly, and then calcium and magnesium ions are removed through ammonium bicarbonate precipitation. According to the method provided by the invention, calcium and magnesium ions can be conveniently removed by controlling precipitation conditions, the obtained high-purity manganese sulfate meets the requirements of electronic-grade manganese sulfate, and the method is low in operation cost, simple in steps and easy to industrialize.

Description

Technical field [0001] The present invention relates to the technical field of new energy ternary lithium battery positive materials, and more particularly to a method of preparing high purity sulfate. Background technique [0002] High purity sulfate (manganese sulfate) is one of the production of the anode material of the three-dimensional lithium battery and the lithium manganganate battery. High purity sulfate sulfate to impurities, such as the product quality standard (Hg / T 4823-2015) of the Ministry of Industry and Information Technology, in Table 1: Table 1 shows the requirements of various impurities in high purity sulfate. [0003] Table 1. Purity requirements of the Ministry of Industry and Information Technology on the manganese sulfate (HG / T 4823-2015) [0004] [0005] Because the requirements for impurity content are high, the difficulty of high purity sulfate production process is the process of removal of impurities. In all impurities, the removal of calcium...

Claims

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Application Information

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IPC IPC(8): C01G45/10
CPCC01G45/10C01P2006/80
Inventor 郭正权
Owner 四川沃林山水环保科技有限公司
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