CN102703697B - Method for recovering rare earth-niobium-ferrum paragenic ore - Google Patents
Method for recovering rare earth-niobium-ferrum paragenic ore Download PDFInfo
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- CN102703697B CN102703697B CN201210221985.1A CN201210221985A CN102703697B CN 102703697 B CN102703697 B CN 102703697B CN 201210221985 A CN201210221985 A CN 201210221985A CN 102703697 B CN102703697 B CN 102703697B
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Abstract
The invention relates to a method for recovering rare earth-niobium-ferrum paragenic ore. The method is characterized by comprising the steps of grinding raw ore, adding CaCO3 and NaCl, mixing evenly and then pelletizing, heating, conducting ball grinding and magnetic separation to obtain reduced iron powder and magnetic separation tailings; adding sodium sulfate and concentrated sulphuric acid in the magnetic separation tailings, mixing evenly, and acidizing to obtain acidized residue, adding waer into acidized residue for primary leaching, and conducting solid-liquid separation to obtain primary leachate and primary leaching residue; adding water into the primary leachate, leaching, and conducting solid-liquid separation to obtain secondary leachate and secondary leaching residue; neutralizing the primary leachate by adopting calcium carbonate, conducting solid-liquid separation to obtain calcium sulfate and primary neutralizing solution, adding ammonia water to regulate pH value of the primary neutralizing solution to obtain niobium hydroxide precipitate, calcinating the precipitate to obtain niobium concentrate; and adding sodium hydroxide to regulate pH value of the secondary leachate to obtain secondary neutralizing solution, adding oxalic acid into the secondary neutralizing solution to obtain rare earth oxalate precipitation, calcinating the precipitation to obtain rare earth oxide. The invention provides a method for comprehensively recovering rare earth, niobium and ferrum.
Description
Technical field
The present invention relates to the recovery method of a kind of rare earth-niobium-iron mineral intergrowth.
Background technology
Abundant rare earth-niobium-iron mineral intergrowth resource has been contained on the ground such as China Inner Mongol, Xinjiang, Yunnan, and the distinguishing feature of this class resource is that valuable element content is low, and embedding cloth close relation adopts the physical concentration method effectively to separate and enrichment.
Domestic many scholars adopt metallurgical method to be studied this class ore.As Gao Peng etc. (" Northeastern University's journal (natural science edition) ", 2010,31 (6): 886-889) with TFe32.17%, REO7.14%, Nb
2o
50.127% raw ore is raw material, 1225 ℃ of reduction temperatures, recovery time 30min, join under the condition of carbon ratio 2 and carry out drastic reduction, reducing material is after stage grinding-coarse and fine separation, obtain iron grade 91.61%, the iron powder of the rate of recovery 93.23%, REO content 12.25% in mine tailing, the rate of recovery 98.73%, can be used as the raw material of sorting rare earth, but this technique is not mentioned the recovery to niobium, and the further extraction of rare earth is not also done and studied in great detail.(" Northeastern University's journal (natural science edition) ", 1996,17 (1): 35-40) to Nb such as Fang Jue
2o
51.82%, the niobium concentrate of TFe51.6%, the processing scheme that selective reduction-molten minute-ferro-niobium is smelted has been proposed, can obtain the ferro-niobium of content of niobium 14%, the total yield of niobium>80%, the total yield of iron>90%, the subject matter that this technique exists is that energy consumption is large, to equipment require highly, the industrialization difficulty is large.Chen Hong (" bao steel technology ", 1998,5:26-29) adopt Direct Reduction Technology, to through gravity treatment, obtain containing ferro-niobium breeze (TFe53.7%, REO content 1.5%, Nb
2o
5content 1.77%) processed iron-removal rate to 96.5%, Nb in nonmagnetics
2o
5content brings up to 6.91%, however this technique the extraction of niobium is not made further research, and whole flow process is not considered the recovery of rare earth.
From ongoing research, metallurgy method can effectively realize the recovery of iron in rare earth-niobium-iron mineral intergrowth, for rare earth and niobium economy is not yet arranged, effectively technology realizes its comprehensive recovery, causes that this class comprehensive utilization of resources rate is low, value of the product is low.
Summary of the invention
The present invention is with a kind of TFe38.25%, REO content 1.43%, Nb
2o
5content 1.62%, SiO
2content 23.18%, Al
2o
3rare earth-the niobium of content 6.85%-iron mineral intergrowth is raw material, for current rare earth-niobium-iron symbiosis rare metal ore deposit middle-weight rare earths and niobium, is difficult to separate and the present situation of enrichment by physical concentration, proposes a kind of method of comprehensive recovering rare earth, niobium and iron.
Technical scheme of the present invention is comprised of following steps:
(1) raw ore ore grinding to-0.074mm content accounts for more than 60%, press massfraction 5～20% and 5～30% interpolation CaCO
3and NaCl, mixing rear pelletizing, dry bulb group is at 1000～1200 ℃ of heating 120～180min, and be milled to-0.074mm of product content accounts for more than 60%, and magnetic separation under the field intensity of 500～2000Oe, obtain reduced iron powder and magnetic tailing;
(2) add the sodium sulfate of its quality 2～10% and the vitriol oil of 1.2～2 times in the magnetic tailing obtained to step 1 respectively, mix, obtain the acidifying slag at 150～350 ℃ of acidifying 90～240min, liquid-solid ratio by 1/1～1.5/1 adds water to the acidifying slag, once leach 30～150min at 75～100 ℃, obtain a leach liquor and a leached mud after solid-liquid separation;
(3) add water to by 5/1～15/1 liquid-solid ratio the leached mud that step 2 obtains, leach 30～150min, obtain secondary leach liquor and secondary leached mud after solid-liquid separation;
(4) pH of leaching solution to 1.0～2.0 that adopt calcium carbonate neutralization procedure 2 to obtain, obtain calcium sulfate and a neutralization solution after solid-liquid separation, add ammoniacal liquor and regulate the pH value 4.0～5.0 of a neutralization solution, obtain the niobium hydroxide precipitation, at 700～900 ℃ of calcining precipitation 60～90min, obtain the niobium concentrate;
(5) the secondary pH of leaching solution to 0.5 that interpolation sodium hydroxide regulating step 3 obtains～2.0, obtain the secondary neutralization solution, the analytical solution Rare-Earth Content, by rare earth/oxalic acid mass ratio, be that 1/1～1/1.5 interpolation oxalic acid is to the secondary neutralization solution, obtain the rare-earth oxalate precipitation, at 800～950 ℃ of calcining precipitation 30～60min, obtain rare earth oxide.
The invention has the advantages that: be applicable to can't the separation and concentration rare metal from the physical concentration method the higher mineral intergrowth of difficult low-grade rare earth-niobium-iron mineral intergrowth, particularly silicon, aluminium content in comprehensive recovering rare earth, niobium and iron.Method of the present invention can realize directly preparing the rare earth oxide of REO content>92%, reduced iron powder and the Nb of TFe content>90% from the rare earth-niobium of high silicon high alumina-iron mineral intergrowth
2o
5the niobium concentrate of content>25%, rare earth yield>75%, iron recovery>90%, the niobium rate of recovery>60%.Method simple and feasible of the present invention, the comprehensive utilization of difficult rare earth-niobium-iron mineral intergrowth that can't Separation and Recovery for the physical concentration method provides feasible technological line, is with a wide range of applications.
The accompanying drawing explanation
Fig. 1 is technical scheme schema of the present invention.
Embodiment
Embodiment 1:REO (rare earth oxide) content 1.43%, Nb
2o
5content 1.62%, the raw ore ore grinding of TFe (all iron content) 38.25% to-0.074mm content reaches 65%, by quality 5% and 30%, adds CaCO
3mix rear pelletizing with NaCl, dry bulb group is at 1000 ℃ of heating 180min, and be milled to-0.074mm of product content accounts for 70%, and magnetic separation under the field intensity of 600Oe, obtain reduced iron powder and magnetic tailing, iron powder TFe content 90.23%, and the rate of recovery of iron is 90.85%.Add the sodium sulfate of its quality 2% and the vitriol oil of 2 times respectively in magnetic tailing, mix, at 150 ℃ of acidifying 240min, the acidifying slag adds water by 1/1 liquid-solid ratio, at 75 ℃, leaches 150min, obtains a leach liquor and a leached mud after solid-liquid separation; Leached mud is added to water logging by 5/1 liquid-solid ratio and go out 120min, obtain secondary leach liquor and secondary leached mud after solid-liquid separation; Adopt a pH of leaching solution to 1.0 of calcium carbonate neutralization, obtain calcium sulfate and a neutralization solution after solid-liquid separation, add the pH value to 4.0 that ammoniacal liquor is regulated a neutralization solution, obtain the niobium hydroxide precipitation, at 700 ℃ of calcining precipitation 90min, obtain Nb
2o
5the niobium concentrate of content 25.82%, the rate of recovery of niobium is 60.78%.Add sodium hydroxide and regulate secondary pH of leaching solution to 1.0, obtain the secondary neutralization solution, by rare earth/oxalic acid mass ratio, be that 1/1 interpolation oxalic acid is to the secondary neutralization solution, obtain the rare-earth oxalate precipitation, at 800 ℃ of calcining precipitation 60min, obtain the rare earth oxide of REO content 92.65%, rare earth yield is 76.62%.
Embodiment 2:REO content 1.43%, Nb
2o
5content 1.62%, the raw ore ore grinding of TFe content 38.25% to-0.074mm content reaches 80%, by quality 10% and 18%, adds CaCO
3mix rear pelletizing with NaCl, dry bulb group is at 1100 ℃ of heating 150min, and be milled to-0.074mm of product content accounts for 65%, and magnetic separation under the field intensity of 800Oe, obtain reduced iron powder and magnetic tailing, iron powder TFe content 90.69%, and the rate of recovery of iron is 91.26%.Add the sodium sulfate of its quality 5% and the vitriol oil of 1.5 times respectively in magnetic tailing, mix, at 250 ℃ of acidifying 150min, the acidifying slag adds water at 100 ℃ of leaching 30min by 1.2/1 liquid-solid ratio, obtains a leach liquor and a leached mud after solid-liquid separation; Leached mud is added to water logging by 9/1 liquid-solid ratio and go out 90min, obtain secondary leach liquor and secondary leached mud after solid-liquid separation; Adopt a pH of leaching solution to 1.5 of calcium carbonate neutralization, obtain calcium sulfate and a neutralization solution after solid-liquid separation, add the pH value to 5.0 that ammoniacal liquor is regulated a neutralization solution, obtain the niobium hydroxide precipitation, at 800 ℃ of calcining precipitation 70min, obtain Nb
2o
5the niobium concentrate of content 25.42%, the rate of recovery of niobium is 61.33%.Add sodium hydroxide and regulate secondary pH of leaching solution to 2.0, obtain the secondary neutralization solution, by rare earth/oxalic acid mass ratio, be that 1/1.5 interpolation oxalic acid is to the secondary neutralization solution, obtain the rare-earth oxalate precipitation, at 900 ℃ of calcining precipitation 30min, obtain the rare earth oxide of REO content 92.37%, rare earth yield is 75.86%.
Embodiment 3:REO content 1.43%, Nb
2o
5content 1.62%, the raw ore ore grinding of TFe content 38.25% to-0.074mm content accounts for 85%, by quality 20% and 8%, adds CaCO
3mix rear pelletizing with NaCl, dry bulb group is at 1180 ℃ of heating 120min, and be milled to-0.074mm of product content accounts for 80%, and magnetic separation under the field intensity of 1200Oe, obtain reduced iron powder and magnetic tailing, iron powder TFe content 90.34%, and the rate of recovery of iron is 91.47%.Add the sodium sulfate of its quality 10% and the vitriol oil of 1.2 times respectively in magnetic tailing, mix, at 350 ℃ of acidifying 90min, the acidifying slag adds water at 80 ℃ of leaching 90min by 1.5/1 liquid-solid ratio, obtains a leach liquor and a leached mud after solid-liquid separation; Leached mud is added to water logging by 15/1 liquid-solid ratio and go out 30min, obtain secondary leach liquor and secondary leached mud after solid-liquid separation; Adopt a pH of leaching solution to 2.0 of calcium carbonate neutralization, obtain calcium sulfate and a neutralization solution after solid-liquid separation, add the pH value to 5.0 that ammoniacal liquor is regulated a neutralization solution, obtain the niobium hydroxide precipitation, at 900 ℃ of calcining precipitation 60min, obtain Nb
2o
5the niobium concentrate of content 25.07%, the rate of recovery of niobium is 60.83%.Add sodium hydroxide and regulate secondary pH of leaching solution to 1.8, obtain the secondary neutralization solution, by rare earth/oxalic acid mass ratio, be that 1/1.5 interpolation oxalic acid is to the secondary neutralization solution, obtain the rare-earth oxalate precipitation, obtain the rare earth oxide of REO content 92.41% at 850 ℃ of calcining precipitation 50min, rare earth yield is 76.13%.
Claims (1)
1. the recovery method of rare earth-niobium-iron mineral intergrowth is characterized in that being comprised of following steps:
(1) raw ore ore grinding to-0.074mm content accounts for more than 60%, press massfraction 5～20% and 5～30% interpolation CaCO
3and NaCl, mixing rear pelletizing, dry bulb group is at 1000～1200 ℃ of heating 120～180min, and be milled to-0.074mm of product content accounts for more than 60%, and magnetic separation under the field intensity of 500～2000Oe, obtain reduced iron powder and magnetic tailing;
(2) add the sodium sulfate of its quality 2～10% and the vitriol oil of 1.2～2 times in the magnetic tailing obtained to step 1 respectively, mix, obtain the acidifying slag at 150～350 ℃ of acidifying 90～240min, liquid-solid ratio by 1/1～1.5/1 adds water to the acidifying slag, once leach 30～150min at 75～100 ℃, obtain a leach liquor and a leached mud after solid-liquid separation;
(3) add water to by 5/1～15/1 liquid-solid ratio the leached mud that step 2 obtains, leach 30～150min, obtain secondary leach liquor and secondary leached mud after solid-liquid separation;
(4) pH of leaching solution to 1.0～2.0 that adopt calcium carbonate neutralization procedure 2 to obtain, obtain calcium sulfate and a neutralization solution after solid-liquid separation, add ammoniacal liquor and regulate the pH value 4.0～5.0 of a neutralization solution, obtain the niobium hydroxide precipitation, at 700～900 ℃ of calcining precipitation 60～90min, obtain the niobium concentrate;
(5) the secondary pH of leaching solution to 0.5 that interpolation sodium hydroxide regulating step 3 obtains～2.0, obtain the secondary neutralization solution, the analytical solution Rare-Earth Content, by rare earth/oxalic acid mass ratio, be that 1/1～1/1.5 interpolation oxalic acid is to the secondary neutralization solution, obtain the rare-earth oxalate precipitation, at 800～950 ℃ of calcining precipitation 30～60min, obtain rare earth oxide.
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| WO2017034009A1 (en) | 2015-08-26 | 2017-03-02 | 日立金属株式会社 | Useful method for separating light rare earth elements and heavy rare earth elements |
| CN110106373B (en) * | 2019-04-17 | 2021-10-26 | 甘肃稀土新材料股份有限公司 | Method for preparing low-magnesium calcium sulfate dihydrate by-product from sulfuric acid rare earth solution |
| CN113149075A (en) * | 2021-04-21 | 2021-07-23 | 中国地质科学院郑州矿产综合利用研究所 | Method for preparing niobium pentoxide from low-grade niobium ore |
| CN115893490A (en) * | 2022-11-23 | 2023-04-04 | 郑州大学 | Method for comprehensively extracting niobium, titanium and rare earth from pyrochlore ore |
| CN115821078A (en) * | 2022-11-30 | 2023-03-21 | 包头稀土研究院 | Method for cooperatively treating fluorite concentrate and iron tailings |
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