CN101633980A - Roasting process of sulfuric acid of rare-earth ore - Google Patents
Roasting process of sulfuric acid of rare-earth ore Download PDFInfo
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- CN101633980A CN101633980A CN200810150424A CN200810150424A CN101633980A CN 101633980 A CN101633980 A CN 101633980A CN 200810150424 A CN200810150424 A CN 200810150424A CN 200810150424 A CN200810150424 A CN 200810150424A CN 101633980 A CN101633980 A CN 101633980A
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Abstract
The invention discloses a roasting process of sulfuric acid of rare-earth ore, comprising the steps of using rare-earth raw ore and rare-earth concentrate as raw materials, adding sulfuric acid according to acid-to-concentrate ratio, evenly mixing, roasting the rare-earth raw ore and rare-earth concentrate added with acid in a high-temperature chamber furnace, adding water into roasted ore at room temperature, then leaching and filtering to obtain once-leaching solution and once-leaching slag filter cake; using industrial magnesia to neutralize the once-leaching solution, adding water into the once-leaching slag filter cake for twice leaching, filtering the neutralized once-leaching solution to obtain neutralized solution and neutralized slag filter cake, carrying out acid dissolving on the neutralization slag filter cake and filtering, mixing the filtered solution after entering the water leaching solution to obtain the water leaching solution product, filtering the once-leaching slag filter cake after twice leaching to obtain the twice-leaching solution and the twice-leaching slag, returning the twice-leaching solution to substitute water to leach for recycling in the next batch of roasted ore. With the manufacturing process of the invention, the effect of solidifying iron and phosphorus is obvious when carrying out roasting and water leaching on the rare-earth raw ore and concentrate of Rainer of Australia, and the total yield of rare earth is higher.
Description
Technical field
The invention belongs to the rare-earth products preparing technical field, particularly a kind of rare-earth mine sulfuric acid baking treatment process.
Background technology
Ore deposit, Australia Lehner company Theresa Weld mountain, this mineral deposit is the abundantest rare-earth mineral of global reserves.The raw ore average grade on Theresa Weld mountain is 14.8%, the concentrate grade 35%～40% of flotation, and the maximum rare-earth mineral-Inner Mongol white clouds pile of stones, earth or grass raw ore average grade of China is 8%.Technology is in the past refined iron in the process in this ore deposit, and phosphorus, impurity such as thorium are difficult to separate, and cause the rare earth yield low, and infusion can not conform to quality requirements, and also can't satisfy the ingredient requirement of downstream extracting and separating.
Summary of the invention
The raw ore, the concentrate that the purpose of this invention is to provide ore deposit, a kind of Australian Lehner company Theresa Weld mountain are processed, and can effectively separate the iron in the ore, phosphorus, impurity such as thorium, and rare earth or the high roasting process of sulfuric acid of rare-earth ore of hand rate.
For achieving the above object, a kind of roasting process of sulfuric acid of rare-earth ore of the present invention is realized by following steps:
One, uses rare-earth original ore, rare earth ore concentrate as raw material, added sulfuric acid by sour ore deposit than 1.0: 1～2.0: 1 and mix;
Two, above-mentioned rare-earth original ore, the rare earth ore concentrate that adds acid placed the high temperature box furnace roasting, maturing temperature is 380 ℃～420 ℃, roasting time 1h～1.5h;
Three, the ore after good adds water at normal temperatures and leaches with roasting in the step 2, and extraction time is 1.5 hours, filters then, obtains an immersion liquid, and soaks the slag filter cake;
Four, with the immersion liquid that makes in the step 3 with in the industrial magnesium oxide and transfer pH to 3.0～4.0, one to soak the slag filter cake to add water and carry out two and soak, two times of soaking were 0.5 hour;
Five, the immersion liquid after becoming reconciled in above-mentioned is filtered, obtain neutralizer and in and the slag filter cake, to neutralizer and in and slag filter cake sampling analysis, in and slag filter cake concentration be the sour molten after-filtration of 0.5mol/L dilute sulphuric acid, filtered liquid enter infusion mix the product infusion;
Six, one in the step 4 soaked slag filter cake two and soaks after-filtration, slag is soaked in two immersion liquid and two, the slag sampling analysis is soaked in two immersion liquid and two, will above-mentioned two immersion liquid return the replacement water logging and go out the next batch roasted ore and recycle.
In the above-mentioned rare-earth mine sulfuric acid baking treatment process, step 1, two described rare-earth original ores and vitriolic acid ore deposit ratio are that 1.5: 1～2.0: 1, maturing temperature are 380 ℃～420 ℃, roasting time 1h～1.5h.
In the above-mentioned rare-earth mine sulfuric acid baking treatment process, step 1, two described rare earth ore concentrates and vitriolic technology condition acid ore deposit ratio are that 1.0: 1～1.5: 1, maturing temperature are that 380 ℃～400 ℃, roasting time are 1h～1.5h.
Adopt manufacturing process of the present invention, the effect of solid iron, phosphorus was remarkable when Australian Lehner rare-earth original ore or Australian Lehner sulfuric acid of rare-earth concentrate roasting water logging were gone out, the rare earth total recovery is higher: Australian Lehner rare-earth original ore rare earth total recovery can reach 70%, Fe in the slag
2O
3Account for 74～85%, PO in the slag
4 3-Account for 80～90%, Gu the effect of iron, phosphorus is remarkable, each economic target all conforms to quality requirements in the infusion.Australia's Lehner rare earth ore concentrate rare earth total recovery can reach 92～94%, Fe in the slag
2O
3Account for 40～60%, PO in the slag
4 3-Account for 85～90%, Gu iron, phosphorus effect are remarkable, each economic target all conforms to quality requirements in the infusion.More than in the infusion of two kinds of ores each economic target all conform to quality requirements, can satisfy the ingredient requirement of downstream extracting and separating.
Table 1 is Lehner rare earth ore concentrate of the present invention and the contrast of packet header f_c_ce_la concentrate sulfuric acid baking each economic target:
Table 1-Lehner rare earth ore concentrate and the contrast of packet header f_c_ce_la concentrate sulfuric acid baking each economic target
The economic and technical norms contrast
Sulphuric acid soln contrast after the neutralization
Embodiment
Embodiment 1
The first step is got Australian Lehner rare-earth original ore 100 grams, adds vitriol oil 160g by sour ore deposit than 1.6 and mixes, and places high temperature box furnace at 380 ℃ of following roasting time 1.2h of maturing temperature.Second step roasted ore that roasting is good adds water 500ml at normal temperatures and carries out water logging, and extraction time is 1.5 hours.Filter, obtain the about 500ml of an immersion liquid and and soak the slag filter cake, an immersion liquid sampling analysis.The 3rd step, with in the industrial magnesium oxide and transfer pH to 3.0～4.0, one to soak the slag filter cake to add water 400ml and carry out two and soak, two times of soaking were 0.5 hour with an immersion liquid.The after-filtration of becoming reconciled in one immersion liquid, neutralizer and in and the slag filter cake, neutralizer and in and slag filter cake sampling analysis.In and the slag filter cake molten according to the dilute sulphuric acid acid that analytical results adds a certain amount of 0.5mol/L, filter, filtered liquid enter infusion mix the product infusion.This step soaks slag filter cake two with one and has soaked filtration, gets two immersion liquid and two and soaks slag, and the slag sampling analysis is soaked in two immersion liquid and two.Remaining two immersion liquid are returned and are replaced water logging to go out the next batch roasted ore recycling.
Embodiment 2
The first step is got Australian Lehner rare-earth original ore 100 grams, adds vitriol oil 180g by sour ore deposit than 1.8 and mixes, and places high temperature box furnace at 420 ℃ of following roasting time 1.2h of maturing temperature.Second step roasted ore that roasting is good adds water 500ml at normal temperatures and carries out water logging, and extraction time is 1.5 hours.Filter, obtain the about 500ml of an immersion liquid and and soak the slag filter cake, an immersion liquid sampling analysis.The 3rd step, with in the industrial magnesium oxide and transfer pH to 3.0～4.0, one to soak the slag filter cake to add water 400ml and carry out two and soak, two times of soaking were 0.5 hour with an immersion liquid.The after-filtration of becoming reconciled in one immersion liquid, neutralizer and in and the slag filter cake, neutralizer and in and slag filter cake sampling analysis.In and the slag filter cake molten according to the dilute sulphuric acid acid that analytical results adds a certain amount of 0.5mol/L, filter, filtered liquid enter infusion mix the product infusion.This step soaks slag filter cake two with one and has soaked filtration, gets two immersion liquid and two and soaks slag, and the slag sampling analysis is soaked in two immersion liquid and two.Remaining two immersion liquid are returned and are replaced water logging to go out the next batch roasted ore recycling.
Embodiment 3
The first step is got Australian Lehner rare-earth original ore 100 grams, adds vitriol oil 120g by sour ore deposit than 1.2 and mixes, and places high temperature box furnace at 380 ℃ of following roasting time 1.2h of maturing temperature.Second step roasted ore that roasting is good adds water 1100ml at normal temperatures and carries out water logging, and extraction time is 1.5 hours.Filter, obtain the about 1100ml of an immersion liquid and and soak the slag filter cake, an immersion liquid sampling analysis.The 3rd step, with in the industrial magnesium oxide and transfer pH to 3.0～4.0, one to soak the slag filter cake to add water 500ml and carry out two and soak, two times of soaking were 0.5 hour with an immersion liquid.The after-filtration of becoming reconciled in one immersion liquid, neutralizer and in and the slag filter cake, neutralizer and in and slag filter cake sampling analysis.In and the slag filter cake molten according to the dilute sulphuric acid acid that analytical results adds a certain amount of 0.5mol/L, filter, filtered liquid enter infusion mix the product infusion.This step soaks slag filter cake two with one and has soaked filtration, gets two immersion liquid and two and soaks slag, and the slag sampling analysis is soaked in two immersion liquid and two.Remaining two immersion liquid are returned and are replaced water logging to go out the next batch roasted ore recycling.
Embodiment 4
The first step is got Australian Lehner rare-earth original ore 100 grams, adds vitriol oil 150g by sour ore deposit than 1.5 and mixes, and places high temperature box furnace at 400 ℃ of following roasting time 1.2h of maturing temperature.Second step roasted ore that roasting is good adds water 1100ml at normal temperatures and carries out water logging, and extraction time is 1.5 hours.Filter, obtain the about 1100ml of an immersion liquid and and soak the slag filter cake, an immersion liquid sampling analysis.The 3rd step, with in the industrial magnesium oxide and transfer pH to 3.0～4.0, one to soak the slag filter cake to add water 500ml and carry out two and soak, two times of soaking were 0.5 hour with an immersion liquid.The after-filtration of becoming reconciled in one immersion liquid, neutralizer and in and the slag filter cake, neutralizer and in and slag filter cake sampling analysis.In and the slag filter cake molten according to the dilute sulphuric acid acid that analytical results adds a certain amount of 0.5mol/L, filter, filtered liquid enter infusion mix the product infusion.This step soaks slag filter cake two with one and has soaked filtration, gets two immersion liquid and two and soaks slag, and the slag sampling analysis is soaked in two immersion liquid and two.Remaining two immersion liquid are returned and are replaced water logging to go out the next batch roasted ore recycling.
Claims (3)
1. roasting process of sulfuric acid of rare-earth ore is characterized in that: described this roasting process of sulfuric acid of rare-earth ore realizes by following steps,
One, uses rare-earth original ore, rare earth ore concentrate as raw material, added sulfuric acid by sour ore deposit than 1.0: 1～2.0: 1 and mix;
Two, above-mentioned rare-earth original ore, the rare earth ore concentrate that adds acid placed the high temperature box furnace roasting, maturing temperature is 380 ℃～420 ℃, roasting time 1h～1.5h;
Three, the ore after good adds water at normal temperatures and leaches with roasting in the step 2, and extraction time is 1.5 hours, filters then, obtains an immersion liquid, and soaks the slag filter cake;
Four, with the immersion liquid that makes in the step 3 with in the industrial magnesium oxide and transfer pH to 3.0～4.0, one to soak the slag filter cake to add water and carry out two and soak, two times of soaking were 0.5 hour;
Five, the immersion liquid after becoming reconciled in above-mentioned is filtered, obtain neutralizer and in and the slag filter cake, to neutralizer and in and slag filter cake sampling analysis, in and slag filter cake concentration be the sour molten after-filtration of 0.5mol/L dilute sulphuric acid, filtered liquid enter infusion mix the product infusion;
Six, one in the step 4 soaked slag filter cake two and soaks after-filtration, slag is soaked in two immersion liquid and two, the slag sampling analysis is soaked in two immersion liquid and two, will above-mentioned two immersion liquid return the replacement water logging and go out the next batch roasted ore and recycle.
2. a kind of roasting process of sulfuric acid of rare-earth ore according to claim 1 is characterized in that: step 1, two described rare-earth original ores and vitriolic acid ore deposit ratio are that 1.5: 1～2.0: 1, maturing temperature are 380 ℃～420 ℃, roasting time 1h～1.5h.
3. a kind of roasting process of sulfuric acid of rare-earth ore according to claim 1 is characterized in that: step 1, two described rare earth ore concentrates and vitriolic technology condition acid ore deposit ratio are that 1.0: 1～1.5: 1, maturing temperature are that 380 ℃～400 ℃, roasting time are 1h～1.5h.
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| CN200810150424A CN101633980A (en) | 2008-07-23 | 2008-07-23 | Roasting process of sulfuric acid of rare-earth ore |
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106460087A (en) * | 2014-05-15 | 2017-02-22 | 淡水河谷公司 | System and process for selective rare earth extraction with sulfur recovery |
| CN109022838A (en) * | 2018-09-14 | 2018-12-18 | 包头稀土研究院 | The processing method of fluorine-containing rare-earth mineral particle |
| CN115058609A (en) * | 2022-06-20 | 2022-09-16 | 中国科学院地球化学研究所 | Method for leaching rare earth in basalt weathering crust |
| 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 |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1721559A (en) * | 2004-12-15 | 2006-01-18 | 北京有色金属研究总院 | Process for comprehensive recovery of rare earth and thorium from rare earth ore |
-
2008
- 2008-07-23 CN CN200810150424A patent/CN101633980A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1721559A (en) * | 2004-12-15 | 2006-01-18 | 北京有色金属研究总院 | Process for comprehensive recovery of rare earth and thorium from rare earth ore |
Non-Patent Citations (1)
| Title |
|---|
| 徐光宪主编: "《稀土》", 31 August 1995, 冶金工业出版社 * |
Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106460087A (en) * | 2014-05-15 | 2017-02-22 | 淡水河谷公司 | System and process for selective rare earth extraction with sulfur recovery |
| CN109022838A (en) * | 2018-09-14 | 2018-12-18 | 包头稀土研究院 | The processing method of fluorine-containing rare-earth mineral particle |
| CN109022838B (en) * | 2018-09-14 | 2020-03-06 | 包头稀土研究院 | Method for treating fluorine-containing rare earth mineral particles |
| CN115058609A (en) * | 2022-06-20 | 2022-09-16 | 中国科学院地球化学研究所 | Method for leaching rare earth in basalt weathering crust |
| 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 |
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Application publication date: 20100127 |