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Separation and recovery method of sodium phosphate and sodium fluoride in mixed rare earth concentrate alkaline smelting process

A mixed rare earth, separation and recovery technology, applied in the field of separation and recovery of sodium phosphate and sodium fluoride in the rare earth smelting process, can solve the problems of high radioactivity, serious problems, increased costs, etc., and achieve the effect of high process stability

Inactive Publication Date: 2011-12-14
INNER MONGOLIA UNIV OF SCI & TECH
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Concentrated sulfuric acid roasting is the most important method for smelting mixed rare earth ores. This method has strong adaptability to rare earth minerals and can stably produce rare earth compounds. However, this process also has serious problems: 1. The pollution of the three wastes is too serious, Seriously affected the surrounding ecological environment; 2. Produced a large amount of thorium pyrophosphate tailings, which are highly radioactive and difficult to reuse, so they can only be designated by the environmental protection department for storage, and high storage fees must be paid; 3 , Many useful elements in minerals are lost in the form of three wastes, and it also increases the cost of environmental protection

Method used

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  • Separation and recovery method of sodium phosphate and sodium fluoride in mixed rare earth concentrate alkaline smelting process
  • Separation and recovery method of sodium phosphate and sodium fluoride in mixed rare earth concentrate alkaline smelting process
  • Separation and recovery method of sodium phosphate and sodium fluoride in mixed rare earth concentrate alkaline smelting process

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Experimental program
Comparison scheme
Effect test

Embodiment 1

[0019] (1) Roast the mixed rare earth concentrate with REO grade of 65.42%, the roasting temperature is 500°C, and the roasting time is 60 minutes.

[0020] (2) The roasted ore is leached with hydrochloric acid, the concentration of hydrochloric acid is 7mol / L, the consumption of hydrochloric acid: the quality of mixed rare earth concentrate: the quality of concentrated hydrochloric acid=1: 2.0, the leaching temperature is 95 ° C, and the time is 1.5 hours to obtain acid leaching residue and acid Dip. In the leaching process, thiourea is used as a reducing agent, and the added mass of thiourea is 0.055 times the mass of the mixed rare earth concentrate.

[0021] (3) Add sodium hydroxide solution to the acid leaching residue after hydrochloric acid leaching for alkali decomposition, the mass concentration of sodium hydroxide solution is 50%, the alkali decomposition temperature is 150° C., and the time is 1.5 hours.

[0022] (4) Continuously repeat the above steps to make 7 ba...

Embodiment 2

[0029] (1) Roast the mixed rare earth concentrate with REO of 55.20%, the roasting temperature is 540°C, and the roasting time is 30 minutes.

[0030] (2) The roasted ore is leached with hydrochloric acid, the concentration of hydrochloric acid is 7mol / L, the amount of hydrochloric acid: the mass of mixed rare earth concentrate: the mass of concentrated hydrochloric acid=1:2.8, the leaching temperature is 75 ° C, and the time is 1 hour. In the leaching process, thiourea is used as a reducing agent, and the added mass of thiourea is 0.075 times the mass of the original ore.

[0031] (3) Add sodium hydroxide solution to the acid leaching residue after hydrochloric acid leaching for alkali decomposition, the mass concentration of sodium hydroxide solution is 75%, the alkali decomposition temperature is 200° C., and the time is 1.2 hours.

[0032] (4) Continuously repeating the above steps to make 9 batches of mixed rare earth concentrates to obtain 9 batches of alkali-decomposed ...

Embodiment 3

[0034] (1) Roast the mixed rare earth concentrate with REO of 67.75%, the roasting temperature is 480°C, and the roasting time is 90 minutes.

[0035] (2) The roasted ore is leached with hydrochloric acid, the concentration of hydrochloric acid is 10mol / L, the amount of hydrochloric acid: the mass of mixed rare earth concentrate: the mass of concentrated hydrochloric acid=1:2.2, the leaching temperature is 80°C, and the time is 2.5 hours. In the leaching process, thiourea is used as a reducing agent, and the added mass of thiourea is 0.095 times the mass of the original ore.

[0036] (3) Add sodium hydroxide solution to the acid leaching residue after hydrochloric acid leaching for alkali decomposition, the mass concentration of sodium hydroxide solution is 50%, the alkali decomposition temperature is 230° C., and the time is 0.5 hours.

[0037] (4) 11 batches of mixed rare earth concentrates were continuously repeated according to the above steps to obtain 11 batches of alkal...

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Abstract

The invention relates to a method for separating and recovering sodium phosphate and sodium fluoride in the alkaline smelting process of mixed rare earth concentrate. The characteristics are: after the mixed rare earth concentrate is roasted, acid leached, and alkali decomposed, the product after alkali decomposition is washed with water to obtain a washing solution, and sodium phosphate and sodium fluoride are separated and recovered from the washing solution, and sodium hydroxide is realized. effective use. The water washing adopts the method of countercurrent washing, and after three steps of heating crystallization, condensation crystallization and concentration, sodium fluoride, sodium phosphate crystals and excess sodium hydroxide concentrated solution or crystals are obtained in sequence. No other impurities are added in the whole process, no three wastes are produced, the recycling cost is low, less water is used, waste is turned into treasure, and it has strong stability, which completely solves the problem of phosphorus and fluorine recovery in the smelting process of mixed rare earth ore.

Description

technical field [0001] The invention relates to a separation and recovery method of sodium phosphate and sodium fluoride in the alkaline smelting process of mixed rare earth concentrate, especially the separation and recovery of sodium phosphate and sodium fluoride in the rare earth smelting process, belonging to the field of hydrometallurgy and waste comprehensive utilization . Background technique [0002] At present, rare earths, as an extremely important strategic resource in my country, play an increasingly important role in aerospace, military, materials, machinery, and chemical industries. From the perspective of the distribution of rare earth reserves, my country's rare earth ores are mainly distributed in the Baiyan Obo ore body in Baotou. This kind of rare earth ore mainly exists in the form of bastnaesite and monazite mixed ore, which is a typical refractory and difficult to smelt mineral. In the process of beneficiation and smelting, there have always been probl...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B1/02C22B3/04B01D9/02C22B59/00C01D3/02C01B25/30
CPCY02P10/20
Inventor 李梅柳召刚胡艳宏王觅堂高凯张栋梁张晓伟
Owner INNER MONGOLIA UNIV OF SCI & TECH
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