CN111394571A - Method for improving decomposition efficiency of rare earth mineral and sulfuric acid - Google Patents

Method for improving decomposition efficiency of rare earth mineral and sulfuric acid Download PDF

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Publication number
CN111394571A
CN111394571A CN202010306415.7A CN202010306415A CN111394571A CN 111394571 A CN111394571 A CN 111394571A CN 202010306415 A CN202010306415 A CN 202010306415A CN 111394571 A CN111394571 A CN 111394571A
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rare earth
sulfuric acid
roasting
temperature
minerals
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CN111394571B (en
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崔建国
徐萌
侯睿恩
王哲
陈禹夫
高婷
蔚腊先
李雪菲
郭金铖
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Baotou Rare Earth Research Institute
Ruike Rare Earth Metallurgy and Functional Materials National Engineering Research Center Co Ltd
Santoku Corp
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Ruike Rare Earth Metallurgy and Functional Materials National Engineering Research Center Co Ltd
Santoku Corp
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    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B1/00—Preliminary treatment of ores or scrap
    • C22B1/02—Roasting processes
    • C22B1/06—Sulfating roasting
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
    • C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
    • C—CHEMISTRY; METALLURGY
    • C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B59/00—Obtaining rare earth metals
    • Y—GENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00—Technologies related to metal processing
    • Y02P10/20—Recycling

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  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Environmental & Geological Engineering (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Chemistry (AREA)
  • Manufacture And Refinement Of Metals (AREA)

Abstract

The invention relates to a method for improving the decomposition efficiency of rare earth minerals and sulfuric acid, and belongs to the field of hydrometallurgy. The method comprises the steps of mixing rare earth concentrate with concentrated sulfuric acid and iron powder for sectional roasting, supplementing a certain amount of water to the solidified minerals in the low-temperature roasting process, optimizing a solid-liquid-gas reaction system, improving the diffusion speed of sulfuric acid in the reaction process, reducing the consumption of sulfuric acid and increasing the decomposition rate of rare earth. During the high-temperature roasting process, the high-efficiency decomposition of excessive sulfuric acid and the generation of iron phosphate and thorium pyrophosphate are mainly used, and the radioactivity and phosphorus resources are fixed and enter the slag. The two-stage roasting simplifies the tail gas components, facilitates subsequent tail gas treatment, reduces the tail gas treatment cost and reduces the environmental pollution.

Description

Method for improving decomposition efficiency of rare earth mineral and sulfuric acid
Technical Field
The invention belongs to the field of wet metallurgy, and particularly relates to a method for improving the decomposition efficiency of rare earth minerals and sulfuric acid.
Background
The ore type rare earth minerals mainly comprise bastnaesite, monazite and mixed rare earth minerals, the smelting technology is different due to the difference of the mineral compositions, the bastnaesite mainly adopts an oxidizing roasting-hydrochloric acid leaching process, the minerals are decomposed into rare earth fluoride and rare earth oxide through oxidizing roasting, when hydrochloric acid for roasting is preferentially dissolved, the concentration and the adding process of hydrochloric acid are controlled, the extraction of trivalent rare earth and the primary separation of tetravalent cerium are realized, and the components such as cerium fluoride, cerium dioxide and the like are contained in residue slag. The process can simply recover valuable rare earth with low cost, but fluorine resources are not utilized, rare earth resources are not extracted completely, and in addition, the diffusion risk of radioactive thorium elements exists. The monazite and the mixed rare earth concentrate are treated by adopting a high-temperature roasting decomposition process of concentrated sulfuric acid, and the mixed rare earth concentrate is uniformly mixed with the concentrated sulfuric acid and iron powder and then is roasted at a high temperature in a rotary kiln at the temperature of 500-. The process is favored by the advantages of low cost of the main process, high degree of continuity and the like, but has the problems of high consumption of sulfuric acid, difficult tail gas treatment, incomplete rare earth decomposition and the like.
In order to solve the problems, the patent name of the method for preparing the mixed rare earth chloride from the Bayan obo rare earth concentrate (application number: 201811249616.7) is that the rare earth concentrate and concentrated sulfuric acid are mixed according to the mass ratio of 1: 0.7-1.5 to be roasted in three sections to obtain roasted ore, wherein the roasting temperature of the first section is controlled to be 100-150 ℃, the evaporation of liquid phase components is reduced at a lower temperature, and the ring formation phenomenon caused by the fact that materials are stuck in a kiln is prevented. Chinese patent 'a method for decomposing high-grade mixed rare earth concentrate by roasting concentrated sulfuric acid at two sections' (application number: 201910424021.9), the method mixes rare earth concentrate (REO > 60%) and concentrated sulfuric acid at normal temperature according to the acid-mineral ratio of 1: 1.3-5.5, the roasting temperature is 180-380 ℃, and the roasting time is 1-5 hours. And directly roasting the low-temperature roasted ore at 380-900 ℃ for 0.5-4.5 hours at high temperature. The two-stage roasting of the method is still designed from the view point of tail gas treatment, the consumption of sulfuric acid is high, and the subsequent treatment process is complicated.
The patent name "a method for decomposing high-grade mixed rare earth concentrate by adding iron and roasting with low-temperature concentrated sulfuric acid" (application number: 201910424015.3) is characterized by that the mixed rare earth concentrate is mixed with sulfuric acid and iron powder, and then roasted at low temperature to obtain roasted ore, and then water-immersed, and said method is still based on the low-temperature roasting principle, so that thorium and phosphorus are fed into the solution, and the iron thorium slag can be obtained by neutralization, but the water-immersed slag still has radioactivity, and the thorium content in the iron thorium slag is too high, so that at present, there is no good treatment method, and the loss of rare earth can be easily resulted in the neutralization process, and the rare.
None of the above patent documents relates to the means for improving the reaction efficiency of mineral decomposition by sulfuric acid in the low temperature roasting process (150 ℃ C. and 250 ℃ C.), thereby effectively reducing the consumption of sulfuric acid. And in the high-temperature roasting process (400-.
Disclosure of Invention
Based on the reasons, the invention provides a method for improving the decomposition efficiency of rare earth minerals and sulfuric acid, which optimizes a solid-liquid-gas reaction system by supplementing a certain amount of moisture to solidified mineral particles in the low-temperature roasting (150 ℃ F.) process (250 ℃ C.), improves the diffusion speed of sulfuric acid in the reaction process, improves the decomposition efficiency of the rare earth minerals and further reduces the consumption of the sulfuric acid.
The method of the invention comprises the following steps:
mixing rare earth minerals and concentrated sulfuric acid according to the weight ratio of 1:0.7-1.2, and adding iron powder to ensure that the molar ratio of the total amount of iron to phosphorus in the minerals is 1.2-1.5: 1;
the reaction materials enter a first stage reaction device, the temperature of the first stage materials is 150-250 ℃, and the time is 60-120 min. In the reaction process, after the mixture is solidified into particles from a paste shape, supplementing water to the particles, and continuing to react. After the first-stage reaction is finished, the material enters a second-stage reaction device, the temperature of the material is 400-600 ℃, and the time is 10-40 min.
Further, the rare earth mineral is monazite, a mixed rare earth mineral or bastnaesite added with phosphate.
Furthermore, the water is supplemented, and the water supplementing amount is 1-10% according to the weight ratio of water to the rare earth minerals.
Compared with the prior art, the method has the following advantages:
(1) in the low-temperature roasting process, a solid-liquid-gas reaction system is maintained by supplementing water, so that the sulfuric acid diffusion speed is increased, the sulfuric acid consumption is reduced, and the rare earth decomposition rate is improved.
In the process of low-temperature roasting (150 ℃ F. & 250 ℃ C.), a certain amount of moisture is supplemented to the solidified mineral particles, so that a solid-liquid-gas reaction system is optimized, the diffusion speed of sulfuric acid in the reaction process is increased, the decomposition efficiency of rare earth minerals is improved, and the consumption of sulfuric acid is reduced.
(2) High-temperature roasting promotes sulfuric acid decomposition, ensures the acidity of the water extract to be in a proper range, and is convenient for next neutralization and impurity removal.
(3) And (3) roasting at high temperature to generate iron phosphate and thorium pyrophosphate, so that the iron, phosphorus and thorium are fixed in the water-immersed slag, and the radioactivity and the trend of phosphorus are controlled.
As the residual acid is accelerated to decompose the monazite mineral by supplementing water at the low-temperature stage, a small amount of residual sulfuric acid after the reaction is finished is efficiently decomposed in the high-temperature roasting process (400-600 ℃), and the thorium ion fixation of the decomposition product phosphoric acid is accelerated. The process has wide applicability to rare earth minerals, has good decomposition effect on mixed rare earth minerals, monazite and bastnaesite added with phosphorus minerals, generates iron phosphate and thorium phosphate in the high-temperature roasting process, fixes radioactive elements thorium and phosphorus in slag, and further achieves the aim of purifying rare earth leachate.
Drawings
FIG. 1 is a process flow diagram of the method for improving the decomposition efficiency of rare earth minerals with sulfuric acid according to the present invention.
Detailed Description
The following description sufficiently illustrates specific embodiments of the invention to enable those skilled in the art to practice and reproduce it.
FIG. 1 is a process flow chart of the method for improving the decomposition efficiency of rare earth minerals and sulfuric acid according to the present invention.
Mixing rare earth minerals and concentrated sulfuric acid according to the weight ratio of 1:0.7-1.2, and adding iron powder to ensure that the molar ratio of the total amount of iron to phosphorus in the rare earth minerals is 1.2-1.5: 1;
the materials enter a first stage reaction device, the temperature of the first stage materials is 150-250 ℃, and the time is 60-120 min. In the reaction process, after the mixture is solidified into particles from a paste shape, supplementing water to the particles, and continuing to react. After the first-stage reaction is finished, the material enters a second-stage reaction device, the temperature of the material is 400-600 ℃, and the time is 10-40 min.
The rare earth mineral is monazite, mixed rare earth mineral or bastnaesite added with phosphate. Supplementing water according to the weight ratio of water to rare earth mineral of 1-10%.
Example 1
Uniformly mixing mixed rare earth concentrate (REO: 54.22%, P: 8.94%, TFe: 4.97%) and concentrated sulfuric acid according to the weight ratio of 1:1.2, adding iron powder, enabling the molar ratio of the total amount of iron to phosphorus in minerals to be 1.2:1, carrying out low-temperature roasting decomposition at 200 ℃, supplementing water with 7% of the mass of minerals after the concentrate mixed with sulfuric acid is roasted into solid particles, maintaining the concentrate in a pasty state, directly roasting at the high temperature after the low-temperature roasting is finished for 90 minutes, wherein the roasting temperature is 550 ℃, the roasting time is 20 minutes, the REO decomposition rate is 98.7%, and the thorium leaching rate is 97.5% after the roasting.
Example 2
Adding part of apatite into bastnaesite (REO: 65.52%, P: 0.16%, TFe: 2.2%), mixing with concentrated sulfuric acid at a weight ratio of 1:0.9, adding iron powder to make the molar ratio of the total amount of iron to phosphorus in the ore be 1.4:1, roasting at 150 deg.C for decomposition, supplementing 5% of water to the ore mass after the ore concentrate mixed with sulfuric acid is roasted into solid particles, keeping the ore concentrate in a paste state, directly roasting at high temperature after 100 minutes of low-temperature roasting, wherein the roasting temperature is 400 deg.C, the roasting time is 40 minutes, the REO decomposition rate is 98.2%, and the thorium leaching rate is 96.3% after roasting.
Example 3
Uniformly mixing mixed rare earth concentrate (REO: 61.66%, P: 4.66%, TFe: 1.14%) and concentrated sulfuric acid according to the weight ratio of 1:0.7, adding iron powder, enabling the molar ratio of the total amount of iron to phosphorus in minerals to be 1.3:1, carrying out low-temperature roasting decomposition at 180 ℃, supplementing water with the amount of 1% of the mass of the minerals after the concentrate mixed with sulfuric acid is roasted into solid particles, maintaining the concentrate in a pasty state, directly roasting at the high temperature after the low-temperature roasting is finished for 120 minutes, wherein the roasting temperature is 450 ℃, the roasting time is 30 minutes, the REO decomposition rate is 98.3%, and the thorium leaching rate is 96.8% after the roasting is finished.
Example 4
Uniformly mixing mixed rare earth concentrate (REO: 61.66%, P: 4.66%, TFe: 1.14%) and concentrated sulfuric acid according to the weight ratio of 1:1, adding iron powder, enabling the molar ratio of the total amount of iron to phosphorus in minerals to be 1.4:1, carrying out low-temperature roasting decomposition at 250 ℃, supplementing 10% of water by the mass of minerals after the concentrate mixed with sulfuric acid is roasted into solid particles, maintaining the concentrate in a pasty state, directly carrying out high-temperature roasting after the low-temperature roasting is finished for 60 minutes, wherein the roasting temperature is 500 ℃, the roasting time is 20 minutes, and after the roasting and sintering, the REO decomposition rate is 98.5%, and the thorium leaching rate is 97.2%.
Example 5
The monazite (REO: 60.03%, P: 11.07%, TFe: 1.03%) and concentrated sulfuric acid are mixed uniformly according to the weight ratio of 1:1.1, after iron powder is added, the molar ratio of the total amount of iron to phosphorus in the mineral is 1.5:1, low-temperature roasting decomposition is carried out at 230 ℃, after the concentrate mixed with sulfuric acid is roasted into solid particles, water with the amount of 3% of the mass of the mineral is supplemented, the concentrate is maintained in a pasty state, after the low-temperature roasting is finished for 90 minutes, the concentrate is directly roasted at the high temperature of 600 ℃ for 10 minutes, after the roasting is finished, the REO decomposition rate is 97.8%, and the thorium leaching rate is 97.9%.
The terminology used herein is for the purpose of description and illustration, rather than of limitation. As the present invention may be embodied in several forms without departing from the spirit or essential characteristics thereof, it should also be understood that the above-described embodiments are not limited by any of the details of the foregoing description, but rather should be construed broadly within its spirit and scope as defined in the appended claims, and therefore all changes and modifications that fall within the meets and bounds of the claims, or equivalences of such meets and bounds are therefore intended to be embraced by the appended claims.

Claims (3)

1. A method for improving the decomposition efficiency of rare earth minerals and sulfuric acid comprises the following steps:
mixing rare earth minerals and concentrated sulfuric acid according to the weight ratio of 1:0.7-1.2, and adding iron powder to ensure that the molar ratio of the total amount of iron to phosphorus in the rare earth minerals is 1.2-1.5: 1;
the reaction materials enter a first stage reaction device, the temperature of the first stage materials is 150-250 ℃, and the time is 60-120 min; in the reaction process, after the mixture is solidified into particles from a paste shape after reaction, supplementing water to the particles, and continuing the reaction; after the first-stage reaction is finished, the material enters a second-stage reaction device, the temperature of the material is 400-600 ℃, and the time is 10-40 min.
2. The method of claim 1, wherein the rare earth mineral is monazite, mixed rare earth mineral or bastnaesite added with phosphate.
3. The method for improving the decomposition efficiency of rare earth minerals with sulfuric acid according to claim 1, wherein the moisture is supplemented at a weight ratio of water to rare earth minerals of 1 to 10%.
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Cited By (4)

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Publication number Priority date Publication date Assignee Title
CN114737049A (en) * 2021-12-27 2022-07-12 包头华美稀土高科有限公司 Method for removing phosphorus in rare earth leaching solution
CN115323177A (en) * 2022-08-11 2022-11-11 甘肃稀土新材料股份有限公司 Method for extracting rare earth from rare earth waste by low-temperature intensified roasting method
CN115449624A (en) * 2022-08-11 2022-12-09 甘肃稀土新材料股份有限公司 Method for treating high-iron low-phosphorus rare earth ore
CN115537588A (en) * 2022-11-04 2022-12-30 内蒙古科技大学 Clean extraction process for decomposing mixed rare earth concentrate

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Publication number Priority date Publication date Assignee Title
CN114737049A (en) * 2021-12-27 2022-07-12 包头华美稀土高科有限公司 Method for removing phosphorus in rare earth leaching solution
CN115323177A (en) * 2022-08-11 2022-11-11 甘肃稀土新材料股份有限公司 Method for extracting rare earth from rare earth waste by low-temperature intensified roasting method
CN115449624A (en) * 2022-08-11 2022-12-09 甘肃稀土新材料股份有限公司 Method for treating high-iron low-phosphorus rare earth ore
CN115537588A (en) * 2022-11-04 2022-12-30 内蒙古科技大学 Clean extraction process for decomposing mixed rare earth concentrate

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