Method for extracting rare earth and recovering fluorine resource from bastnaesite

A technology of bastnaesite and bastnaesite, which is applied in the field of rare earth hydrometallurgy, can solve the problems of reducing the profit margin of production enterprises, long production process, and high financial pressure, so as to reduce the cost of sewage treatment and simplify the production process , the effect of reducing production costs

Active Publication Date: 2021-11-19
四川省冕宁县方兴稀土有限公司
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  • Abstract
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  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The process currently has the following two major technical defects: one is that the production process is relatively long, the process control requirements are relatively high, and the energy consumption and material consumption are relatively large; The obtained waste water has relatively heavy salt content, and the combined acid-base method to treat rare earth concentrates will produce fluorine-containing waste water with high alkalinity. After the fluorine in the waste water is recovered, the salt content in the waste water will be high, usually sodium salt , can reach about 13g / L
[0004] Although the current rare earth industry discharge standards do not have specific requirements for the content of sodium salts, the discharge of high-salt sewage will affect the environment. With the gradual implementation of national policies, the environmental protection pressure of the rare earth industry is increasing, and the discharged wastewater is harmful to high-salt wastewater. The requirements are getting higher and higher. The government's environmental protection department clearly requires the recovery of salt in wastewater, and the salt content can only be discharged within the normal range. Therefore, rare earth enterprises are now required to use high-salt recovery systems.
According to the rare earth enterprises that process 8,000 tons of rare earth concentrates per year, the one-time direct investment of the current high-salt recovery system is about 30 million, not including the operating costs. , the financial pressure is very high, and it also reduces the profit margin of the production enterprise

Method used

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  • Method for extracting rare earth and recovering fluorine resource from bastnaesite
  • Method for extracting rare earth and recovering fluorine resource from bastnaesite
  • Method for extracting rare earth and recovering fluorine resource from bastnaesite

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Experimental program
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Effect test

Embodiment 1

[0049] Such as figure 1 Shown, the existing common acid-base combined method is processed the production technology of bastnaesite, comprises the following steps:

[0050] S1. Oxidative roasting of rare earth concentrates (REO≥68.5%) at a roasting temperature of 580-600°C;

[0051] S2. The concentrated ore after roasting is leached with hydrochloric acid, and the acidity of the leachate is not more than 0.3mol / L. At this time, the cerium distribution C / R≤8% (CeO / REO) is obtained to obtain the leachate and the leach residue;

[0052] S3, carrying out alkaline conversion to the leaching residue, the concentration of NaOH is [OH － ]≥1.5mol / L to obtain alkali-converted slag, wash the alkali-converted slag with water, control the pH value between 7-8, and the washing solution is fluorine-containing wastewater;

[0053] S4, adding the washed alkali-turned slag into hydrochloric acid for pickling, the pH value of the hydrochloric acid is 1.0-1.5, and C / R≤25%;

[0054] S5, the solu...

Embodiment 2

[0059] Such as figure 2 Shown, a kind of bastnaesite of the present invention extracts the method for rare earth, comprises the following steps:

[0060] S1. Carrying out oxidative roasting of the rare earth concentrate, the roasting temperature is 450-530°C, and the roasting time is 1-3 hours, to obtain the roasted product;

[0061] S2. Carry out hydrochloric acid leaching on the roasted product, the acidity of the acid solution is controlled at 0.3-0.8mol / L, the acidity of the whole reaction system is controlled below 0.5mol / L, the cerium partition C / R≤5%, and the primary leachate and primary leach residue;

[0062] S3. Add clear water to the primary leaching slag, stir and heat up to above 90°C, then add hydrochloric acid complexing agent, the amount of hydrochloric acid complexing agent added is 0.46-0.66 times the total weight of REO in the rare earth ore (here the weight of hydrochloric acid is equivalent to Industrial hydrochloric acid with a mass fraction of 31%), t...

example 1

[0070] A method for extracting rare earth from bastnaesite, comprising the following steps:

[0071] S1. Take the bastnaesite with REO grade of 67.25% and oxidize and roast it in a constant temperature muffle furnace at 530°C for 2.5 hours, and call the oxidized and roasted bastnaesite ore roasted ore. The fluorine content in the roasted ore At 8.54%, the REO content is 80.06%;

[0072] S2. Divide the oxidized and roasted bastnaesite into 5 groups according to a batch of 500g for testing; during the test, take 5 3000mL beakers, numbered 1-5 respectively, and control the acidity of the bottom water in each beaker to 0.3 -0.8mol / L, the acidity of the bottom water is shown in Table 1:

[0073] Table 1 Number 1-5 Bottom Water Acidity Table (The data shown is the concentration of hydrochloric acid)

[0074] Numbering number 1 number 2 number 3 No 4 Number 5 Acidity (mol / L) 0.36 0.45 0.55 0.64 0.77

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Abstract

The invention discloses a method for extracting rare earth and recycling fluorine resources from bastnaesite. The method comprises the following steps that S1, oxidizing roasting is carried out on rare earth concentrate, and then hydrochloric acid leaching is carried out to obtain primary leaching liquid and primary leaching residues; S2, clear water and a hydrochloric acid complexing agent are added into the primary leaching residues, and secondary leaching residues and secondary leaching liquid are obtained after filtering; S3, quenching and tempering and filtering treatment are carried out on the primary leaching liquid and the secondary leaching liquid, and quenched and tempered residues are obtained; and S4, the quenched and tempered residues are dissolved by using hydrochloric acid, filtering and separating are carried out to obtain filter residues, chlorohydric acid pickling is carried out on the filter residues for multiple times, and then drying and packaging are carried out. According to the method, the fluorine resources are recovered by adding the hydrochloric acid complexing agent and the like, alkali conversion is not needed, energy is greatly saved, the production process is simplified, the product cryolite with high added value is formed, due to the fact that high-salt wastewater is not generated, a high-salt recovery system is not needed, the sewage treatment cost is greatly reduced, and the defects in the prior art are overcome.

Description

technical field [0001] The invention relates to the technical field of rare earth hydrometallurgy, in particular to a method for extracting rare earth from bastnaesite and recovering fluorine resources. Background technique [0002] The rare earth ore in Maoniuping, Sichuan is mainly bastnaesite rare earth ore. The content of fluorine in this ore is relatively high. Fluorine generally exists in the form of calcium fluoride or bastnaesium rare earth. Valuable rare earth is actually mainly considering how to separate the fluorine and rare earth in the mine. [0003] At present, domestic manufacturers of bastnaesite mainly adopt the following process: the acid-base combined production process is used to separate the rare earth and fluorine first, and then defluoride the fluorine-containing wastewater. The process currently has the following two major technical defects: one is that the production process is relatively long, the process control requirements are relatively high, ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C22B59/00C22B3/10C22B1/02C01F17/282C01F17/10C01F7/54
CPCC22B59/00C22B3/10C22B1/02C01F7/54C01F17/282C01F17/10Y02P10/20
Inventor 卢立海蔡蔚邓思祥魏云李霞
Owner 四川省冕宁县方兴稀土有限公司
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