CN103526054A - Method for preparing rare earth ore concentrates by using low-grade light rare earth tailings - Google Patents
Method for preparing rare earth ore concentrates by using low-grade light rare earth tailings Download PDFInfo
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- CN103526054A CN103526054A CN201210229918.4A CN201210229918A CN103526054A CN 103526054 A CN103526054 A CN 103526054A CN 201210229918 A CN201210229918 A CN 201210229918A CN 103526054 A CN103526054 A CN 103526054A
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Abstract
The invention relates to a method for preparing rare earth ore concentrates by using low-grade light rare earth tailings, and the method is characterized in that according to the difference in the contents of rare earth elements and iron in tailings, rare earth ore concentrates are prepared by using a magnetic separation, flotation and acid dissolving combination process. The specific process comprises the following steps: firstly, levigating and screening tailings; according to the difference in the contents of the rare earth elements and iron in the tailings, selecting a process of carrying out magnetic separation firstly and then carrying out acid dissolving, or a process of carrying out flotation firstly and then carrying out acid dissolving, or a process of sequentially carrying out magnetic separation, flotation and acid dissolving, or a process of directly carrying out acid dissolving; after acid dissolving is completed, filtering the obtained object, adding alkali into filter liquor to adjust the pH value of the filter liquor, so that the rare earth elements in the filter liquor are precipitated, and then a rare earth ore concentrate is obtained; washing filter residues by using water, returning washing water for preparing an acid solution. The method disclosed by the invention has the characteristics that rare earth elements can be efficiently extracted from low-grade rare earth tailings by using a simple process so as to obtain a high-grade ore concentrate; meanwhile, production wastewater is recycled, so that the utilization efficiency of water is improved, and rare earth elements in the wastewater can be further recovered.
Description
Technical field
The invention belongs to solid waste regeneration field, be specifically related to a kind of method of preparing rare earth ore concentrate with low-grade light rare earths mine tailing.
Background technology
Because its unique electron structure of rare earth element and special physicochemical property are widely used in petrochemical complex, metal metallurgy smelting, agricultural, pottery, glass and electronic industry etc.Along with scientific and technical development, rare earth day by day shows the effect that is difficult to substitute in new high-tech industry.
Rare earth is the strategic resource of China, and China has the abundantest in the world rare earth resources.As the important rare-earth mining area of China, rare earth reserves occupy the first in the world, and ree content is high, kind is many.General when mining area mineral wealth are exploited utilization, can form the extremely huge mine tailing of quantity.Mine tailing is as a kind of solid waste, and it is arbitrarily stacked and so not only surrounding environment has been caused to pollution, harm periphery resident's life and health, but also taken a large amount of soils, consumption fund, affect the economic benefit of enterprise.
Mineral resources, as a kind of Nonrenewable resources, have formed sharp-pointed contradiction between the supply that it is limited and unlimited demand.In the face of the present situation of Global Mineral shortage, resource is carried out to the material iterative cycles utilization that recycle realizes " resource-product-renewable resource ", thereby realize synthesization, the innoxious use of resource, be the inevitable choice of the sustainable development of socio-economy.In mine tailing, containing various useful elements, is a kind of potential secondary resource.But in general, in mine tailing useful element taste lower, impurity component is more, is universally acknowledged refractory mineral.Therefore, the available approach of research mine tailing, turns waste into wealth these mine tailings, turn harm into good, and be the important channel of realizing resources effective utilization.
Summary of the invention
The present invention seeks to take low-grade light rare earths mine tailing is raw material, prepares rare earth ore concentrate.
For achieving the above object, the technical solution used in the present invention is: different by low-grade light rare earths mine tailing according to content of rare earth and iron level, adopting magnetic separation, flotation, the molten method combining of acid take and producing rare earth taste is more than 60% rare earth ore concentrate.Its production technique is: first low-grade light rare earths mine tailing is carried out to ore grinding and screening, obtaining particle diameter is that 100 orders are to the former powder of rare-earth tailing between 200 orders; Then according to the difference of REO in mine tailing and Fe content select different treatment process: a. when REO content is 1%～4%, Fe content is while being 10%～20%, the mine tailing after screening sent into flotation unit and carry out flotation, then carries out acid molten; B. when REO content is 4%～6%, Fe content is while being 10%～20%, the mine tailing after screening directly carried out to acid molten; C. when REO content is 1%～4%, Fe content is while being 20%～40%, the mine tailing after screening carried out to magnetic separation, and then carry out flotation, carries out afterwards acid molten; D. when REO content is 4%～6%, Fe content is while being 20%～40%, and the mine tailing after screening is carried out to magnetic separation, then carries out acid molten; When acid is molten, the solid-to-liquid ratio of the mixing acid of mine tailing and hydrochloric acid, nitric acid and sulfuric acid or hydrochloric acid, nitric acid and sulfuric acid is 1～20, H in acid solution
+concentration is 0.1mol/L～1.5mol/L, and sour solubility temperature is 20 ℃～100 ℃, and the sour molten reaction times is 1h～10h; Mine tailing after molten to acid filters, and obtains filtrate and filter residue; In filtrate, add at least one in volatile salt, bicarbonate of ammonia, ammoniacal liquor, sodium carbonate, sodium bicarbonate, to 4.5, the rare earth element in filtrate be precipitated out pH regulator to 3.5, through centrifugal to obtain rare earth ore concentrate; Filter residue is washed, and water lotion is for the broad liquid of preparating acid.
After above-mentioned treatment process is processed, rare earth element in mine tailing mainly enters into rare earth ore concentrate, a small amount of rare earth element enters in magnetic separation or flotation tailings, and a small amount of rare earth element enters into true tailings, also has a small amount of rare earth element to enter among factory effluent; And most ferro elements have entered into magnetic separation or flotation tailings in mine tailing, the iron of a part enters into rare earth ore concentrate, and a small amount of iron enters into true tailings, also has a small amount of iron to enter into factory effluent.
Described low-grade light rare earths mine tailing Rare-Earth Content is 1%～6%, and iron level is 10%～40%.
The present invention through implementing its advantage is: the rare-earth tailing that 1, can process low-grade (REO=1%～6%); 2, rare earth yield is the highest can reach more than 90%; 3, gained rare earth ore concentrate is of high grade, can reach 60%; 4, waste water energy recycles, and quantity discharged is few, and temperature of reaction is low, energy-saving and emission-reduction; 5, the reaction times short, production efficiency is high; 6, technical process is simple, easy to operate.
Accompanying drawing explanation
This figure is the process flow sheet of Extraction of rare earth from rare-earth tailing.
First low-grade light rare earths mine tailing is carried out to ore grinding and screening, obtaining particle diameter is that 100 orders are to the former powder of rare-earth tailing between 200 orders; Then according to the difference of REO in mine tailing and Fe content, select different treatment process:
A. when REO content is 1%～4%, Fe content is while being 10%～20%, the mine tailing after screening sent into flotation unit and carry out flotation, then carries out acid molten; When acid is molten, the solid-to-liquid ratio of the mixing acid of mine tailing and hydrochloric acid, nitric acid and sulfuric acid or hydrochloric acid, nitric acid and sulfuric acid is 1～20, H in acid solution
+concentration is 0.1mol/L～1.5mol/L, and sour solubility temperature is 20 ℃～100 ℃, and the sour molten reaction times is 1h～10h; Mine tailing after molten to acid filters, and obtains filtrate and filter residue; In filtrate, add at least one in volatile salt, bicarbonate of ammonia, ammoniacal liquor, sodium carbonate, sodium bicarbonate, to 4.5, the rare earth element in filtrate be precipitated out pH regulator to 3.5, through centrifugal to obtain rare earth ore concentrate; Filter residue is washed, and water lotion is for the broad liquid of preparating acid.
B. when REO content is 4%～6%, Fe content is while being 10%～20%, the mine tailing after screening directly carried out to acid molten; When acid is molten, the solid-to-liquid ratio of the mixing acid of mine tailing and hydrochloric acid, nitric acid and sulfuric acid or hydrochloric acid, nitric acid and sulfuric acid is 1～20, H in acid solution
+concentration is 0.1mol/L～1.5mol/L, and sour solubility temperature is 20 ℃～100 ℃, and the sour molten reaction times is 1h～10h; Mine tailing after molten to acid filters, and obtains filtrate and filter residue; In filtrate, add at least one in volatile salt, bicarbonate of ammonia, ammoniacal liquor, sodium carbonate, sodium bicarbonate, to 4.5, the rare earth element in filtrate be precipitated out pH regulator to 3.5, through centrifugal to obtain rare earth ore concentrate; Filter residue is washed, and water lotion is for the broad liquid of preparating acid.
C. when REO content is 1%～4%, Fe content is while being 20%～40%, the mine tailing after screening carried out to magnetic separation, and then carry out flotation, carries out afterwards acid molten; When acid is molten, the solid-to-liquid ratio of the mixing acid of mine tailing and hydrochloric acid, nitric acid and sulfuric acid or hydrochloric acid, nitric acid and sulfuric acid is 1～20, H in acid solution
+concentration is 0.1mol/L～1.5mol/L, and sour solubility temperature is 20 ℃～100 ℃, and the sour molten reaction times is 1h～10h; Mine tailing after molten to acid filters, and obtains filtrate and filter residue; In filtrate, add at least one in volatile salt, bicarbonate of ammonia, ammoniacal liquor, sodium carbonate, sodium bicarbonate, to 4.5, the rare earth element in filtrate be precipitated out pH regulator to 3.5, through centrifugal to obtain rare earth ore concentrate; Filter residue is washed, and water lotion is for the broad liquid of preparating acid.
D. when REO content is 4%～6%, Fe content is while being 20%～40%, and the mine tailing after screening is carried out to magnetic separation, then carries out acid molten; When acid is molten, the solid-to-liquid ratio of the mixing acid of mine tailing and hydrochloric acid, nitric acid and sulfuric acid or hydrochloric acid, nitric acid and sulfuric acid is 1～20, H in acid solution
+concentration is 0.1mol/L～1.5mol/L, and sour solubility temperature is 20 ℃～100 ℃, and the sour molten reaction times is 1h～10h; Mine tailing after molten to acid filters, and obtains filtrate and filter residue; In filtrate, add at least one in volatile salt, bicarbonate of ammonia, ammoniacal liquor, sodium carbonate, sodium bicarbonate, to 4.5, the rare earth element in filtrate be precipitated out pH regulator to 3.5, through centrifugal to obtain rare earth ore concentrate; Filter residue is washed, and water lotion is for the broad liquid of preparating acid.
Embodiment
Below in conjunction with embodiment, the present invention will be further described, not limiting the scope of the invention:
Embodiment 1
The low-grade light rare earths mine tailing of take is raw material, and REO is wherein that 3.97%, Fe content is 15.7%.First mine tailing is carried out to ore grinding, the laggard row filter of ore grinding, obtain particle diameter at 100 orders to the mine tailing between 200 orders.Then mine tailing is sized mixing, ore pulp is sent to floatation equipment and carries out flotation operation.REO content after flotation in mine tailing can reach 39.2%.To the mine tailing after flotation, use 0.2mol/L hydrochloric acid to carry out acid molten, solid-to-liquid ratio is 1: 5, and the sour molten reaction times is 2h, and sour solubility temperature is normal temperature.The molten rear solution of acid is filtered, to adding in filtrate ammoniacal liquor to regulate pH, at pH, reach at 4.2 o'clock and stop adding ammoniacal liquor, thereby make rare earth element in solution many being precipitated out as far as possible.Then the solution that generates precipitation is sent into whizzer and carry out centrifugal treating, the solid obtaining after centrifugal is dried, finally obtain rare earth taste and be 70.4% rare earth ore concentrate.The total rate of recovery of true tailings rare earth elements reaches 90.8%.
Embodiment 2:
The low-grade light rare earths mine tailing of take is raw material, and the REO in ore deposit is 4.90%, and iron level is 11.3%.First mine tailing is levigate, the former powder of the mine tailing obtaining after levigate is directly carried out to sour molten processing.Take the former powder of a certain amount of rare-earth tailing, with hydrochloric acid and nitric acid, within 3: 1 by volume, prepare the nitration mixture that hydrogen ion concentration is 0.8mol/L, in the solid-to-liquid ratio ratio of 1: 3, in the former powder of mine tailing, add nitration mixture, at normal temperatures sour molten 2h.After acid is molten, filter.With a certain amount of deionized water wash filter residue, in washings, contain certain density rare earth element, for further recovering rare earth element, reduce wastewater discharge simultaneously, washings need be back in the configuration of acid solution.Filtrate by acid after molten regulates pH with sodium bicarbonate, makes the pH of filtrate reach 4.2, and at this moment the rare earth element in solution is precipitated out in a large number, thereby centrifugal, dry and obtain rare earth ore concentrate.In gained rare earth ore concentrate, the content of REO is 65.7%, and the total yield of rare earth is 88.9%.
Embodiment 3: the REO of take in ore deposit as 5.32%, iron level is 28.6% low-grade light rare earths mine tailing is raw material.First mine tailing is carried out to ore grinding processing.The former powder of the mine tailing obtaining after ore grinding is sent into magnetic separator and carry out magnetic separation, the REO content after magnetic separation in mine tailing can reach 7.19%.Take the former powder of rare-earth tailing after a certain amount of magnetic separation, in the solid-to-liquid ratio ratio of 1: 5, in the former powder of mine tailing, add H
+concentration is the mixed acid solution of hydrochloric acid/nitric acid preparation of 0.75mol/L, and in nitration mixture, hydrochloric acid and nitric acid ratio are 1: 1.Acid solubility temperature is normal temperature, and the sour molten time is 2h.After acid is molten, filter.Filtrate after acid is molten regulates pH with bicarbonate of ammonia, makes the pH of filtrate reach 4.0, and at this moment the rare earth element in solution is precipitated out in a large number, thereby obtains the rare earth ore concentrate of REO content 63.5%, and the total yield of rare earth is 91.8%.
Embodiment 4:
The low-grade light rare earths mine tailing of take is raw material, and the REO in ore deposit is 1.79%, and iron level is 21.8%.Rare-earth tailing is sent into the levigate former powder of mine tailing of making in ball mill, the former powder of mine tailing is screened, with obtain particle diameter at 100 orders to the former powder between 200 orders.The former powder filtering out is sent into the magnetic separator that magneticstrength is greater than 10000 Gausses, magneticly elects the iron in former powder, makes REO content in former powder bring up to 2.26%.By having removed iron former powder whipping appts stirring pulping afterwards, then send into flotation unit and carry out flotation, thereby the REO content in former powder is brought up to 26.28%.Then the former powder of mine tailing is used at 25 ℃ the hydrochloric acid soln of 1.0mol/L to carry out acid at 1: 10 by solid-to-liquid ratio molten, sour molten 2h, filters after acid is molten.Filter residue washs with deionized water, and water lotion is for the broad liquid of preparating acid; Filtrate neutralizes with ammoniacal liquor, regulates filtrate pH to 4.2 that the rare earth element in filtrate is precipitated out, and centrifugal, oven dry makes content of rare earth and reaches 67.6% rare earth ore concentrate, and rare earth element total yield is 90.3%.
Claims (8)
1. with low-grade light rare earths mine tailing, prepare a method for rare earth ore concentrate, it is characterized in that: processing step is: a. carries out ore grinding and the former powder of Screening Treatment mine tailing by original debris; B. according to the first magnetic separation of the different choice of mine tailing rare earth elements and iron level sourer molten or first flotation sourer molten or after magnetic separation, flotation acid molten or directly to carry out acid molten; C. sourly filter after molten, to adding alkali in filtrate, regulate pH, the rare earth element in filtrate is precipitated out, and then obtains rare earth ore concentrate; D. filter residue is washed with water, washing water return to preparating acid solution.
2. a kind of method of preparing rare earth ore concentrate with low-grade light rare earths mine tailing according to claim 1, is characterized in that: rare-earth tailing Rare-Earth Content used is 1%～6%, and iron level is 10%～40%.
3. a kind of method of preparing rare earth ore concentrate with low-grade light rare earths mine tailing according to claim 1, is characterized in that: after ore grinding and Screening Treatment the former powder of mine tailing footpath at 100 orders between 200 orders.
4. a kind of method of preparing rare earth ore concentrate with low-grade light rare earths mine tailing according to claim 1, it is characterized in that: the mixing acid that the molten acid used of acid is hydrochloric acid, nitric acid, sulfuric acid or hydrochloric acid, nitric acid and sulfuric acid, while using mixing acid, the volume ratio of hydrochloric acid, nitric acid and sulfuric acid is (0～3) hydrochloric acid: (0～3) nitric acid: (0～3) sulfuric acid, acid solutions is 0.1mol/L～1.5mol/L.
5. a kind of method of preparing rare earth ore concentrate with low-grade light rare earths mine tailing according to claim 1, is characterized in that: sour when molten solid-to-liquid ratio between the former powder of mine tailing and acid solution be 1～20.
6. a kind of method of preparing rare earth ore concentrate with low-grade light rare earths mine tailing according to claim 1, is characterized in that: the sour molten reaction times is 1h～10h.
7. a kind of method of preparing rare earth ore concentrate with low-grade light rare earths mine tailing according to claim 1, is characterized in that: sour solubility temperature is 20 ℃～100 ℃.
8. a kind of method of preparing rare earth ore concentrate with low-grade light rare earths mine tailing according to claim 1, is characterized in that: at least one in the filtrate use volatile salt after acid is molten, bicarbonate of ammonia, ammoniacal liquor, sodium carbonate, sodium bicarbonate is by pH regulator to 3.5～4.5.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111203425A (en) * | 2020-01-10 | 2020-05-29 | 泉州丰鹏环保科技有限公司 | Process and device for crushing and recovering alumina framework of waste FCC catalyst |
| WO2021073162A1 (en) * | 2019-10-14 | 2021-04-22 | 广东省科学院资源综合利用研究所 | Method for intensive recovery of valuable components from rare earth tailings |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2021073162A1 (en) * | 2019-10-14 | 2021-04-22 | 广东省科学院资源综合利用研究所 | Method for intensive recovery of valuable components from rare earth tailings |
| CN111203425A (en) * | 2020-01-10 | 2020-05-29 | 泉州丰鹏环保科技有限公司 | Process and device for crushing and recovering alumina framework of waste FCC catalyst |
| CN111203425B (en) * | 2020-01-10 | 2021-10-29 | 泉州丰鹏环保科技有限公司 | Process and device for crushing and recovering alumina framework of waste FCC catalyst |
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