High-purity manganese sulfide and method for preparing the same

A technology of manganese sulfide and hydrogen sulfide, applied in chemical instruments and methods, inorganic chemistry, manganese compounds, etc., can solve the problems of low product purity, inability to industrialize large-scale production, and difficulty in washing

Active Publication Date: 2015-06-24
SHENZHEN MODERN SKY TECH CO LTD
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0002] Manganese sulfide is used in powder metallurgy, weak magnetic semiconductor materials, optical, electrical and magnetic materials, and preparation of high-purity manganese salts. Traditional high-temperature reduction methods and solid-phase synthesis methods produce products with low purity and high energy consumption.
[0003] CN101555040A discloses a kind of preparation method of nano-MnS, but the method prepares MnS to exist NaCl washing difficulty, NaCl 2 S contains a lot of polysulfides, which causes product entrainment. The autoclave reaction in the polytetrafluoroethylene liner cannot be industrialized and mass-produced. Drying in an oven at 60 ° C can easily cause defects such as oxidation, and it is impossible to prepare high-purity MnS products.

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preparation example Construction

[0028] The preparation method of manganese sulfide of the present invention, realizes by following chemical reaction:

[0029] MSO 4 +MnS→MS+MnSO 4

[0030] (M: Co, Ni, Cu, Zn, Pb, As, Fe, etc.)

[0031] MnSO 4 +2NH 3 / H 2 O+H 2 S↑→MnS+(NH 4 ) 2 SO 4 +2H 2 o

[0032] The present invention uses manganese sulfate as a starting raw material, separates and removes the content of each heavy metal element in the raw material manganese sulfate through pretreatment to further control the content of each metal element in the product manganese sulfide element, and finally obtains high-purity manganese sulfide.

[0033] In a specific embodiment, the production method of manganese sulfide of the present invention, comprises the steps:

[0034] (1) Pretreatment step: Add manganese sulfide to manganese sulfate solution with a concentration of 50g / L-300g / L, and then separate solid and liquid to obtain purified manganese sulfate solution and solid;

[0035] In a preferred embodim...

Embodiment 1

[0064] refer to figure 1 and figure 2 , the present embodiment manganese sulfide is prepared through the following steps:

[0065] (1) Pretreatment step: prepare 20 kg of commercially available feed-grade manganese sulfate into a manganese sulfate solution with a concentration of 100g / L, then add 30g of MnS to the above solution, heat the mixture to 90°C after mixing, and then stir to react After 2 hours, solid-liquid separation by filtration is carried out, valuable metals are recovered from the solid, and the clarified liquid enters the next step of operation.

[0066] (2) Spray reaction step: open the manganese sulfate valve 2 to send the above-mentioned pretreated manganese sulfate solution into the spray absorption reactor through the manganese sulfate feed port 12, and then open the circulation pump 4 to circulate, wherein the circulation pump The flow rate is 4m 3 / h, then turn on H 2 S valve 10, adjust H 2 The flow of S is 1.3m 3 About / h, open the liquid ammoni...

Embodiment 2

[0069] refer to figure 1 and figure 2, the present embodiment manganese sulfide is prepared through the following steps:

[0070] (1) Pretreatment step: liquid SO 2 Manganese sulfate solution obtained by reacting with low-grade manganese dioxide, wherein the quality of manganese sulfate is 200kg, MnSO 4 The concentration of the solution is 120g / L, then add 400g MnS to the above solution, mix and heat the mixed solution to 95°C, then stir and react for 3 hours, then carry out solid-liquid separation by filtration, recover valuable metals from the solid, and enter the clarified liquid into Next step.

[0071] (2) Spray reaction step: open the manganese sulfate valve to send the above-mentioned pretreated manganese sulfate solution into the spray absorption reactor through the manganese sulfate feed port 12, and then turn on the circulation pump 4 for circulation, wherein the flow rate of the circulation pump 100m 3 / h, then turn on H 2 S valve 10, adjust H 2 The flow of ...

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Abstract

The invention relates to high-purity manganese sulfide and a method for preparing high-purity manganese sulfide. The method comprises the following steps of: (1) a pretreatment step: adding manganese sulfide to manganese sulfate solution, and then performing solid-liquid separation; (2) a spray reaction step: adding liquid ammonia to the solution obtained in the step (1) to obtain spray solution; and circularly spraying the spray solution through a circulating pump so that the spray solution joins in a circular spray reaction with hydrogen sulfide gas; terminating the spray reaction until the mass concentration of manganese ions in the reactant solution is less than 500 ppm; and performing solid-liquid separation on the solution after the spray reaction is terminated; and (3) washing and drying, thereby obtaining the manganese sulfide product. The invention also relates to manganese sulfide prepared by the preparation method, wherein the purity of the manganese sulfide is above 99.90wt% and the moisture content of the manganese sulfide is less than 0.5%; the mass content of Fe in the manganese sulfide is less than 0.80 ppm; and preferably, the mass content of each of K and Na is less than 5.0 ppm, while the mass content of Ca is less than 25 ppm and the mass content of Mg is less than 10 ppm, in the manganese sulfide.

Description

technical field [0001] The invention relates to the technical field of inorganic fine chemicals, in particular to a high-purity manganese sulfide and a preparation method thereof. Background technique [0002] Manganese sulfide is used in powder metallurgy, weak magnetic semiconductor materials, optical, electrical and magnetic materials, and preparation of high-purity manganese salts. Traditional high-temperature reduction methods and solid-phase synthesis methods produce products with low purity and high energy consumption. [0003] CN101555040A discloses a kind of preparation method of nano-MnS, but the method prepares MnS to exist NaCl washing difficulty, NaCl 2 S contains a lot of polysulfides, which causes product entrainment. The autoclave reaction in the polytetrafluoroethylene liner cannot be industrially produced on a large scale. Drying in an oven at 60 ° C can easily cause defects such as oxidation, and it is impossible to prepare high-purity MnS products. Cont...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C01G45/00
Inventor 吴筱菁
Owner SHENZHEN MODERN SKY TECH CO LTD
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