Cyclic and comprehensive utilization method of sodium-free mangano-manganic oxide production mother solution

A technology of trimanganese tetraoxide and mother liquor, applied in the direction of improving process efficiency, etc., can solve the problems of high production cost, difficult and efficient LiOH, simple and convenient recycling, etc.

Inactive Publication Date: 2013-05-29
CENT SOUTH UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0007] Aiming at the problem that LiOH is difficult to efficiently and simply recycle in the existing sodium-free manganese tetraoxide production process, resulting in high production costs, the present invention provides a method for recycling and comprehensive utilization of mother liquor produced by sodium-free manganese tetroxide , realizing the efficient, cheap and simple recycling of LiOH in the production process of sodium-free manganese tetraoxide

Method used

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  • Cyclic and comprehensive utilization method of sodium-free mangano-manganic oxide production mother solution
  • Cyclic and comprehensive utilization method of sodium-free mangano-manganic oxide production mother solution
  • Cyclic and comprehensive utilization method of sodium-free mangano-manganic oxide production mother solution

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Effect test

Embodiment 1

[0021] Sodium-free manganese tetraoxide production mother liquor mainly contains Mn 2+ , Ca 2+ , Mg 2+ , Na + , SO 4 2- Plasma, the specific composition is shown in Table 1.

[0022] 1. Measure 10L of trimanganese tetraoxide production mother liquor, prepare 2.78L of sodium phosphate solution with a concentration of 370g / L, slowly add sodium phosphate solution into trimanganese tetraoxide production mother liquor, stir while adding, and react at room temperature for 1h, Then filter to obtain sodium sulfate solution, lithium phosphate, and manganese phosphate precipitates, wash the precipitates twice with deionized water, dry, grind and pass through a 300-mesh sieve to obtain 728.9 grams of mixed powder of lithium phosphate and manganese phosphate. The sodium sulfate solution was concentrated, cooled and crystallized to obtain solid sodium sulfate.

[0023] 2. Slaked Lime Conversion Lithium Phosphate and Manganese Phosphate Mixed Powder

[0024] Weigh 330 grams of mixed...

Embodiment 2

[0036] Sodium-free manganese tetraoxide production mother liquor mainly contains Mn 2+ , Ca 2+ , Mg 2+ , Na + , SO 4 2- Plasma, the specific composition is shown in Table 2.

[0037] 1. Measure 10L of sodium-free manganese tetraoxide production mother liquor, prepare 3.02L of sodium phosphate solution with a concentration of 185g / L, slowly add the sodium phosphate solution into the production mother liquor of trimanganese tetraoxide, stir while adding, at room temperature React for 1 h, then filter to obtain sodium sulfate solution, lithium phosphate, and manganese phosphate precipitates, wash the precipitates twice with deionized water, dry, grind and pass through a 300-mesh sieve to obtain 357 grams of mixed powder of lithium phosphate and manganese phosphate. The sodium sulfate solution was concentrated, cooled and crystallized to obtain solid sodium sulfate.

[0038] 2. Slaked Lime Conversion Lithium Phosphate and Manganese Phosphate Mixed Powder

[0039] Weigh 330...

Embodiment 3

[0051] Sodium-free manganese tetraoxide production mother liquor mainly contains Mn 2+ , Ca 2+ , Mg 2+ , Na + , SO 4 2- Plasma, the specific composition is shown in Table 3.

[0052] Measure 10L of trimanganese tetraoxide production mother liquor, prepare 1.74L of sodium phosphate solution with a concentration of 185g / L, slowly add sodium phosphate solution into trimanganese tetraoxide production mother liquor, stir while adding, react at room temperature for 1h, and then filter , to obtain sodium sulfate solution and lithium phosphate, manganese phosphate precipitate, the precipitate was washed twice with deionized water, dried, ground and passed through a 300 mesh sieve to obtain 193.6 grams of lithium phosphate and manganese phosphate mixed powder. The sodium sulfate solution was concentrated, cooled and crystallized to obtain solid sodium sulfate.

[0053] 2. Slaked Lime Conversion Lithium Phosphate and Manganese Phosphate Mixed Powder

[0054] Weigh 165 grams of m...

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Abstract

The invention relates to a cyclic and comprehensive utilization method of a sodium-free mangano-manganic oxide production mother solution, which comprises the following steps: 1, adding a sodium phosphate solution into a sodium-free mangano-manganic oxide production mother solution, controlling the mol ratio of the sodium phosphate to lithium sulfate at (2.0-2.4):3, and filtering after reaction is finished, wherein the filter residues are lithium phosphate and manganese phosphate solids; and 2, washing the obtained filter residues, drying, grinding, screening, adding the lithium phosphate and manganese phosphate powder and calcium hydroxide into hot water according to a lithium phosphate / calcium hydroxide mol ratio of 1:(2.25-3), and reacting to obtain a lithium hydroxide solution; and treating the obtained solution through an ion exchange resin to obtain a lithium hydroxide solution of which the calcium ion concentration is lower than 1 ppm, and using the lithium hydroxide solution as a precipitating agent in the sodium-free mangano-manganic oxide preparation process. According to the invention, the cyclic utilization rate of lithium is up to 96% or above, the byproducts of sodium sulfate and calcium chloride are generated simultaneously, the economic benefits are favorable, the production process is less prone to cause environmental pollution, the equipment investment is low, and industrial production can be easily realized.

Description

technical field [0001] The invention relates to a method for recycling and comprehensive utilization of a sodium-free trimanganese tetraoxide production mother liquor, in particular to a method for recycling lithium hydroxide in a sodium-free trimanganese tetraoxide production mother liquor. Background technique [0002] The commonly used production method of manganese tetraoxide is the manganese ore method, that is, the manganese ore is leached with sulfuric acid, purified and removed to obtain a manganese sulfate solution, and the precipitate is neutralized with caustic soda to form Mn(OH) 2 , and then oxidize Mn(OH) with an oxidizing agent 2 get Mn 3 o 4 . mn 3 o 4 It is the raw material for preparing lithium manganese oxide, the positive electrode material of the battery. The sodium content of the battery material needs to be strictly controlled to be less than 5ppm, but it is difficult to wash with caustic soda, and the sodium content is difficult to meet the requi...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B3/44C22B47/00
CPCY02P10/20
Inventor 杨喜云段习韬石西昌徐徽陈亚陈白珍
Owner CENT SOUTH UNIV
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