CN102703697A - 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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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 ground such as China Inner Mongol, Xinjiang, Yunnan, and the distinguishing feature of this type 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 that this type ore is studied.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 a raw material, at 1225 ℃ of reduction temperatures, recovery time 30min; Join under the condition of carbon ratio 2 and carry out drastic reduction, the reduction material obtains iron grade 91.61% behind stage grinding-coarse and fine separation; The iron powder of the recovery 93.23%, REO content 12.25% in the mine tailing, the recovery 98.73%; Can be used as the raw material of sorting rare earth, but this technology is not mentioned the recovery to niobium, and the further extraction of rare earth also do not done study in great detail.(" Northeastern University's journal (natural science edition) ", 1996,17 (1): such as Fang Jue 35-40) to Nb
2O
51.82%, the niobium concentrate of TFe51.6% has proposed the processing scheme that selective reduction-molten branch-ferro-niobium is smelted; 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 technology exists is that energy consumption is big; Requirement to equipment is high, and the industriallization difficulty is big.Chen Hong (" bao steel technology ", 1998,5:26-29) adopt direct reduction technique, contain ferro-niobium breeze (TFe53.7%, REO content 1.5%, Nb to what obtain through gravity treatment
2O
5Content 1.77%) handle iron-removal rate to 96.5%, Nb in the nonmagnetics
2O
5Content brings up to 6.91%, yet this technology is not done further research to the extraction of niobium, 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, does not then have economy, otherwise effective technique to realize its comprehensive recovery as yet for rare earth and niobium, causes that this type 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 a raw material, is difficult to separate the present situation with enrichment through physical concentration to present rare earth-niobium-iron symbiosis rare metal ore deposit middle-weight rare earths and niobium, proposes the method for a kind of comprehensive recovery rare earth, niobium and iron.
Technical scheme of the present invention is made up 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, making ball behind the mixing, dry bulb group is at 1000～1200 ℃ of heating 120～180min, and product ball milling to-0.074mm content accounts for more than 60%, and magnetic separation under the field intensity of 500～2000Oe obtains reduced iron powder and magnetic tailing;
(2) in the magnetic tailing that step 1 obtains, add the sodium sulfate of its quality 2～10% and 1.2～2 times the vitriol oil respectively; Mixing; 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 leaches 30～150min at 75～100 ℃, obtains a leach liquor and a leached mud after the solid-liquid separation;
(3) add water to the leached mud that step 2 obtains by 5/1～15/1 liquid-solid ratio, leach 30～150min, obtain secondary leach liquor and secondary leached mud after the solid-liquid separation;
PH of leaching solution to 1.0～2.0 of (4) adopting lime carbonate neutralization procedure 2 to obtain; Obtain calcium sulfate and a neutralization solution after the solid-liquid separation; Add ammoniacal liquor and regulate the pH value 4.0～5.0 of a neutralization solution; Obtain the niobium hydroxide deposition,, obtain the niobium concentrate at 700～900 ℃ of calcining deposition 60～90min;
(5) add secondary pH of leaching solution to 0.5～2.0 that sodium hydroxide regulating step 3 obtains; Obtain the secondary neutralization solution; Analytical solution middle-weight rare earths content is 1/1～1/1.5 interpolation oxalic acid to secondary neutralization solution by rare earth/oxalic acid mass ratio, obtains the rare-earth oxalate deposition; At 800～950 ℃ of calcining deposition 30～60min, obtain rare earth oxide.
The invention has the advantages that: be applicable to from the physical concentration method can't the separation and concentration rare metal the higher mineral intergrowth of hard to manage low-grade rare earth-niobium-iron mineral intergrowth, particularly silicon, aluminium content in comprehensive rare earth, niobium and the iron of reclaiming.Method of the present invention can realize directly preparing the rare earth oxide of REO content＞92%, the 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 recovery＞60%.Method simple and feasible of the present invention, the comprehensive utilization of rare earth-niobium hard to manage-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.
Description of drawings
Fig. 1 is a 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% interpolation CaCO
3With make ball behind the NaCl mixing, dry bulb group is at 1000 ℃ of heating 180min, product is milled to-0.074mm content accounts for 70%, magnetic separation under the field intensity of 600Oe obtains reduced iron powder and magnetic tailing, iron powder TFe content 90.23%, the recovery of iron is 90.85%.In magnetic tailing, add the sodium sulfate of its quality 2% and 2 times the vitriol oil respectively, mixing, at 150 ℃ of acidifying 240min, the acidifying slag adds water by 1/1 liquid-solid ratio, leaches 150min at 75 ℃, obtains a leach liquor and a leached mud after the solid-liquid separation; Leached mud is added water logging by 5/1 liquid-solid ratio go out 120min, obtain secondary leach liquor and secondary leached mud after the solid-liquid separation; Adopt pH of leaching solution to 1.0 of lime carbonate neutralization, obtain calcium sulfate and a neutralization solution after the solid-liquid separation, add the pH value to 4.0 that ammoniacal liquor is regulated a neutralization solution, obtain the niobium hydroxide deposition, obtain Nb at 700 ℃ of calcining deposition 90min
2O
5The niobium concentrate of content 25.82%, the recovery of niobium are 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 is 1/1 interpolation oxalic acid to secondary neutralization solution, obtains the rare-earth oxalate deposition, at 800 ℃ of calcining deposition 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% interpolation CaCO
3With make ball behind the NaCl mixing, dry bulb group is at 1100 ℃ of heating 150min, product is milled to-0.074mm content accounts for 65%, magnetic separation under the field intensity of 800Oe obtains reduced iron powder and magnetic tailing, iron powder TFe content 90.69%, the recovery of iron is 91.26%.In magnetic tailing, add the sodium sulfate of its quality 5% and 1.5 times the vitriol oil respectively, mixing, 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 the solid-liquid separation; Leached mud is added water logging by 9/1 liquid-solid ratio go out 90min, obtain secondary leach liquor and secondary leached mud after the solid-liquid separation; Adopt pH of leaching solution to 1.5 of lime carbonate neutralization, obtain calcium sulfate and a neutralization solution after the solid-liquid separation, add the pH value to 5.0 that ammoniacal liquor is regulated a neutralization solution, obtain the niobium hydroxide deposition, obtain Nb at 800 ℃ of calcining deposition 70min
2O
5The niobium concentrate of content 25.42%, the recovery of niobium are 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 is 1/1.5 interpolation oxalic acid to secondary neutralization solution, obtains the rare-earth oxalate deposition, at 900 ℃ of calcining deposition 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% interpolation CaCO
3With make ball behind the NaCl mixing, dry bulb group is at 1180 ℃ of heating 120min, product is milled to-0.074mm content accounts for 80%, magnetic separation under the field intensity of 1200Oe obtains reduced iron powder and magnetic tailing, iron powder TFe content 90.34%, the recovery of iron is 91.47%.In magnetic tailing, add the sodium sulfate of its quality 10% and 1.2 times the vitriol oil respectively, mixing, 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 the solid-liquid separation; Leached mud is added water logging by 15/1 liquid-solid ratio go out 30min, obtain secondary leach liquor and secondary leached mud after the solid-liquid separation; Adopt pH of leaching solution to 2.0 of lime carbonate neutralization, obtain calcium sulfate and a neutralization solution after the solid-liquid separation, add the pH value to 5.0 that ammoniacal liquor is regulated a neutralization solution, obtain the niobium hydroxide deposition,, obtain Nb at 900 ℃ of calcining deposition 60min
2O
5The niobium concentrate of content 25.07%, the recovery of niobium are 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 is 1/1.5 interpolation oxalic acid to secondary neutralization solution; Obtain the rare-earth oxalate deposition, precipitate the rare earth oxide that 50min obtain REO content 92.41% 850 ℃ of calcinings, rare earth yield is 76.13%.
Claims (1)
1. the recovery method of rare earth-niobium-iron mineral intergrowth is characterized in that being made up 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, making ball behind the mixing, dry bulb group is at 1000～1200 ℃ of heating 120～180min, and product ball milling to-0.074mm content accounts for more than 60%, and magnetic separation under the field intensity of 500～2000Oe obtains reduced iron powder and magnetic tailing;
(2) in the magnetic tailing that step 1 obtains, add the sodium sulfate of its quality 2～10% and 1.2～2 times the vitriol oil respectively; Mixing; 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 leaches 30～150min at 75～100 ℃, obtains a leach liquor and a leached mud after the solid-liquid separation;
(3) add water to the leached mud that step 2 obtains by 5/1～15/1 liquid-solid ratio, leach 30～150min, obtain secondary leach liquor and secondary leached mud after the solid-liquid separation;
PH of leaching solution to 1.0～2.0 of (4) adopting lime carbonate neutralization procedure 2 to obtain; Obtain calcium sulfate and a neutralization solution after the solid-liquid separation; Add ammoniacal liquor and regulate the pH value 4.0～5.0 of a neutralization solution; Obtain the niobium hydroxide deposition,, obtain the niobium concentrate at 700～900 ℃ of calcining deposition 60～90min;
(5) add secondary pH of leaching solution to 0.5～2.0 that sodium hydroxide regulating step 3 obtains; Obtain the secondary neutralization solution; Analytical solution middle-weight rare earths content is 1/1～1/1.5 interpolation oxalic acid to secondary neutralization solution by rare earth/oxalic acid mass ratio, obtains the rare-earth oxalate deposition; At 800～950 ℃ of calcining deposition 30～60min, obtain rare earth oxide.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107922997A (en) * | 2015-08-26 | 2018-04-17 | 日立金属株式会社 | Separate light rare earth elements and the useful method of heavy rare earth element |
| CN110106373A (en) * | 2019-04-17 | 2019-08-09 | 甘肃稀土新材料股份有限公司 | A method of preparing low magnesium calcium sulphate dihydrate by-product from rare earth sulfate 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 |
| CN115821078A (en) * | 2022-11-30 | 2023-03-21 | 包头稀土研究院 | Method for cooperatively treating fluorite concentrate and iron tailings |
| CN115893490A (en) * | 2022-11-23 | 2023-04-04 | 郑州大学 | Method for comprehensively extracting niobium, titanium and rare earth from pyrochlore ore |
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN107922997A (en) * | 2015-08-26 | 2018-04-17 | 日立金属株式会社 | Separate light rare earth elements and the useful method of heavy rare earth element |
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| CN110106373A (en) * | 2019-04-17 | 2019-08-09 | 甘肃稀土新材料股份有限公司 | A method of preparing low magnesium calcium sulphate dihydrate by-product from rare earth sulfate solution |
| 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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