CN105200247B - A kind of method for improving low-grade ore solubility and feed liquid removal of impurities - Google Patents
A kind of method for improving low-grade ore solubility and feed liquid removal of impurities Download PDFInfo
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- CN105200247B CN105200247B CN201510635882.3A CN201510635882A CN105200247B CN 105200247 B CN105200247 B CN 105200247B CN 201510635882 A CN201510635882 A CN 201510635882A CN 105200247 B CN105200247 B CN 105200247B
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- rare earth
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- 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
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Abstract
The present invention relates to a kind of method for improving low-grade ore solubility and feed liquid removal of impurities, this method is by adding acid for adjusting pH then to add in BaCl to the 0.5 low-grade Rare Earth Mine of dissolving2Remove SO4 2‑, alkali is added to adjust pH to 4.0 ~ 5.0 and removes impurity iron and impurity aluminum, is eventually adding flocculating agent precipitation, the isolated Rare Earth Mine feed liquid of press filtration, rare earth element yield >=97%, Fe after ageing2O3≤ 0.03%, Al2O3≤1.0%.The present invention is remarkably improved the solubility of low-grade ore, can obviously reduce the impurity content in feed liquid, improves the availability of low-grade Rare Earth Mine, avoids the waste of rare earth resources, with good economic efficiency and social benefit.
Description
Technical field
The invention belongs to technical field of wet metallurgy, and in particular to a kind of raising low-grade ore solubility and feed liquid removal of impurities
Method.
Background technology
China is rare earth resources, production, outlet and consumption big country, and with the development of new and high technology, market is to rare-earth products
The requirement of quality and impurity content is higher and higher.
Low-grade Rare Earth Mine is begun to use to be produced with a large amount of exploitations and quick consumption, separation enterprise of rare earth.
Need the solubility of the raising Rare Earth Mine in production operation.
Impurity phase present in low-grade Rare Earth Mine is to more, if being directly entered extraction and separation without pretreatment,
Inevitably result in impurity forms three-phase emulsion when running up to a certain amount of, split-phase and the circulation of extraction process are influenced, when serious
May result in parking extraction three-phase object could continue to produce, and be affected to entire production procedure.
Invention content
The purpose of the present invention is overcoming low-grade ore solubility low, the problem of feed liquid impurity is more, provide it is a kind of improve it is low
Grade ore deposit solubility and the method for feed liquid removal of impurities.
The present invention realizes in the following way:
A kind of method for improving low-grade Rare Earth Mine solubility and feed liquid removal of impurities, which is characterized in that include the following steps:
(1)A certain amount of water is added in reaction vessel, low-grade ore is added in simultaneously under stiring and acid is reacted, control
The ratio of water and low-grade ore processed is ore deposit:Water=1:1.5 ~ 2, it is 0.5 to adjust pH value in reaction, continuously adds acid after reaction, until
Constant pH value is 0.5, a concentration of 1.2 ~ 1.7 mol/L of solution rare earth elements;
(2)Detecting step(1)The SO of acquired solution4 2-Concentration, with SO4 2-:BaCl2=1:1.5 concentration ratio adds in
BaCl2, 1 ~ 3 h is stirred at 80 ~ 90 DEG C;
(3)To step(2)Alkali is added in acquired solution, it is 4.0 ~ 5.0 to adjust pH value, stirs 1 ~ 3 h;
(4)To step(3)Flocculating agent is added in acquired solution, is aged the isolated Rare Earth Mine feed liquid of press filtration after 2-4 h,
Rare earth element yield >=97%, Fe2O3≤ 0.03%, Al2O3≤1.0% 。
Preferably, the acid is hydrochloric acid.
Preferably, its a concentration of 9 ~ 10 mol/L of the hydrochloric acid.
Preferably, its addition flow of the hydrochloric acid is 37 ~ 50 L/min.
Preferably, the alkali is sodium hydroxide.
Preferably, its a concentration of 5 ~ 7 mol/L of the sodium hydroxide.
Preferably, its addition flow of the sodium hydroxide is 5 ~ 10 L/min.
Preferably, the flocculating agent is polyacrylamide.
The principle of the present invention is:The pH of miberal powder course of dissolution is controlled by acid adding, highly acidity improves the molten of low-grade ore
Solution rate, dissolved efficiency highest when pH is 0.5, dissolved rare earth feed liquid concentration are maintained at 1.2 ~ 1.7 mol/L, are conducive to improve
The removal rate of aluminium hydroxide reduces, also follow-up extraction procedure preferably, can effectively improve the total recovery of Rare Earth Mine;Then add in
BaCl2Precipitate SO4 2-;Then increase liquid caustic soda readjustment pH, during which to control rate of alkaline, it is dilute to avoid the occurrence of the excessively high appearance of local pH
Soil precipitation, pH ferric hydroxide precipitates at 3.68 are complete, and aluminium removal effect is preferable when 4.0 ~ 5.8, but hereafter rare earth will appear
Precipitation causes yield to decline, therefore it is more suitable 4.0 ~ 5.0 to adjust back pH controls.
The beneficial effects of the invention are as follows:
1. the present invention is remarkably improved the solubility of low-grade ore, rare earth element yield >=97%.
2. the present invention can obviously reduce the impurity content in feed liquid, Fe2O3≤ 0.03%, Al2O3≤ 1.0%, it effectively reduces
There is three-phase object emulsion in next step extraction and separation operation.
3. the addition speed of the invention by reasonably controlling miberal powder and hydrochloric acid makes reaction temperature improve and control one
A suitable range reduces the use of steam, cost-effective.
4. the present invention improves the availability of low-grade Rare Earth Mine, the waste of rare earth resources is avoided, is had good
Economic benefit and social benefit.
Specific embodiment
With reference to specific embodiment, the invention will be further described, but does not limit the scope of the invention and apply
Range.
Embodiment 1
A kind of method for improving low-grade Rare Earth Mine solubility and feed liquid removal of impurities, which is characterized in that include the following steps:
(1)A certain amount of water is added in reaction vessel, adds in low-grade ore and a concentration of 9 mol/L simultaneously under stiring
Hydrochloric acid reacted, hydrochloric acid its to add in flow be 47 L/min, the ratio for controlling water and low-grade ore is ore deposit:Water=1:1.7
It is 0.5 to adjust pH value in reaction, continuously adds acid after reaction, until it is 0.5 that pH value is constant, solution rare earth elements are a concentration of
1.5 mol/L;
(2)Detecting step(1)The SO of acquired solution4 2-Concentration, with SO4 2-:BaCl2=1:1.5 concentration ratio adds in
BaCl2, 1 ~ 3 h is stirred at 85 DEG C;
(3)To step(2)The sodium hydroxide of a concentration of 6 mol/L is added in acquired solution with 7 L/min of flow, adjusts pH
It is 4.4 to be worth, and stirs 2 h;
(4)To step(3)Flocculating agent polyacrylamide is added in acquired solution, is aged the isolated rare earth of press filtration after 3 h
Mineral aggregate liquid, rare earth element yield >=99%, Fe2O3≤ 0.02%, Al2O3≤0.6%。
Embodiment 2
A kind of method for improving low-grade Rare Earth Mine solubility and feed liquid removal of impurities, which is characterized in that include the following steps:
(1)A certain amount of water is added in reaction vessel, adds in low-grade ore and a concentration of 9 mol/L simultaneously under stiring
Hydrochloric acid reacted, hydrochloric acid its to add in flow be 37 L/min, the ratio for controlling water and low-grade ore is ore deposit:Water=1:1.5
It is 0.5 to adjust pH value in reaction, continuously adds acid after reaction, until it is 0.5 that pH value is constant, solution rare earth elements are a concentration of
1.2 mol/L;
(2)Detecting step(1)The SO of acquired solution4 2-Concentration, with SO4 2-:BaCl2=1:1.5 concentration ratio adds in
BaCl2, 1 h is stirred at 80 DEG C;
(3)To step(2)The sodium hydroxide of a concentration of 5 mol/L is added in acquired solution with 5 L/min of flow, adjusts pH
It is 4.0 to be worth, and stirs 1 h;
(4)To step(3)Flocculating agent polyacrylamide is added in acquired solution, is aged the isolated rare earth of press filtration after 2 h
Mineral aggregate liquid, rare earth element yield >=98%, Fe2O3≤ 0.03%, Al2O3≤1.0%。
Embodiment 3
A kind of method for improving low-grade Rare Earth Mine solubility and feed liquid removal of impurities, which is characterized in that include the following steps:
(1)A certain amount of water is added in reaction vessel, adds in low-grade ore and a concentration of 10 mol/ simultaneously under stiring
The hydrochloric acid of L is reacted, it adds in flow as 50 L/min to hydrochloric acid, and it is ore deposit to control the ratio of water and low-grade ore:Water=1:2,
It is 0.5 to adjust pH value in reaction, continuously adds acid after reaction, until it is 0.5 that pH value is constant, solution rare earth elements are a concentration of
1.7 mol/L;
(2)Detecting step(1)The SO of acquired solution4 2-Concentration, with SO4 2-:BaCl2=1:1.5 concentration ratio adds in
BaCl2, 3 h are stirred at 90 DEG C;
(3)To step(2)The sodium hydroxide of a concentration of 7 mol/L is added in acquired solution with 10 L/min of flow, is adjusted
PH value is 5.0, stirs 3 h;
(4)To step(3)Flocculating agent polyacrylamide is added in acquired solution, is aged the isolated rare earth of press filtration after 4 h
Mineral aggregate liquid, rare earth element yield >=97%, Fe2O3≤ 0.02%, Al2O3≤0.8%。
Embodiment 4
A kind of method for improving low-grade Rare Earth Mine solubility and feed liquid removal of impurities, which is characterized in that include the following steps:
(1)A certain amount of water is added in reaction vessel, adds in low-grade ore and a concentration of 9 mol/L simultaneously under stiring
Hydrochloric acid reacted, hydrochloric acid its to add in flow be 40 L/min, the ratio for controlling water and low-grade ore is ore deposit:Water=1:1.8
It is 0.5 to adjust pH value in reaction, continuously adds acid after reaction, until it is 0.5 that pH value is constant, solution rare earth elements are a concentration of
1.6mol/L;
(2)Detecting step(1)The SO of acquired solution4 2-Concentration, with SO4 2-:BaCl2=1:1.5 concentration ratio adds in
BaCl2, 1 h is stirred at 88 DEG C;
(3)To step(2)The sodium hydroxide of a concentration of 6 mol/L is added in acquired solution with 8 L/min of flow, adjusts pH
It is 4.5 to be worth, and stirs 3 h;
(4)To step(3)Flocculating agent polyacrylamide is added in acquired solution, is aged the isolated rare earth of press filtration after 3 h
Mineral aggregate liquid, rare earth element yield >=99%, Fe2O3≤ 0.01%, Al2O3≤0.9%。
Claims (1)
- A kind of 1. method for improving low-grade Rare Earth Mine solubility and feed liquid removal of impurities, which is characterized in that include the following steps:(1)A certain amount of water is added in reaction vessel, adds in the salt of low-grade ore and a concentration of 9 mol/L simultaneously under stiring Acid is reacted, it adds in flow as 47 L/min to hydrochloric acid, and it is ore deposit to control the ratio of water and low-grade ore:Water=1:1.7, it adjusts PH value in reaction is 0.5, continuously adds acid after reaction, until it is 0.5 that pH value is constant, solution rare earth elements a concentration of 1.5 mol/L;(2)Detecting step(1)The SO of acquired solution4 2-Concentration, with SO4 2-:BaCl2=1:1.5 concentration ratio add in BaCl2, 1 ~ 3 h is stirred at 85 DEG C;(3)To step(2)The sodium hydroxide of a concentration of 6 mol/L is added in acquired solution with 7 L/min of flow, adjusting pH value is 4.4, stir 2 h;(4)To step(3)Flocculating agent polyacrylamide is added in acquired solution, is aged the isolated rare earth mineral aggregate of press filtration after 3 h Liquid, rare earth element yield >=99%, Fe2O3≤ 0.02%, Al2O3≤0.6%。
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Address after: 532200 Industrial Road East 8, Chongzuo City Industrial Zone, the Guangxi Zhuang Autonomous Region Patentee after: Guangxi Guosheng rare earth new material Co.,Ltd. Address before: 532200 Industrial Road East 8, Chongzuo City Industrial Zone, the Guangxi Zhuang Autonomous Region Patentee before: CHINALCO GUANGXI GUOSHENG RARE EARTH DEVELOPMENT CO.,LTD. |