CN103243226A - Method for preparing rare earth concentrate from low-grade light rare earth tailings - Google Patents
Method for preparing rare earth concentrate from low-grade light rare earth tailings Download PDFInfo
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Abstract
The invention relates to a method for preparing rare earth concentrate from low-grade light rare earth tailings. The method is characterized in that rare earth concentrate is prepared by magnetic separation, flotation and acid dissolution combined technologies according to different contents of rare earth element and iron content in tailings. Concrete technology comprises the following steps: firstly levigating and screening tailings, and carrying out magnetic separation and acid dissolution in order or carrying out flotation and acid dissolution in order or carrying out magnetic separation, flotation and acid dissolution in order or directly carrying out acid dissolution based on different selections of rare earth element and iron content in tailings; filtering after acid dissolution, adding alkali into a filtrate to adjust pH, and depositing rare earth element from the filtrate to obtain rare earth concentrate; washing filter residue by the use of water, and returning washing water to prepare an acid solution. The method is characterized in that a simple technology can be used to highly efficiently extract rare earth element from low-grade rare earth tailings so as to obtain high-grade rare earth concentrate; and meanwhile, production wastewater is recycled so as to raise service efficiency of water and further recover rare earth element in wastewater.
Description
Technical field
The invention belongs to solid waste regeneration field, be specifically related to a kind of method for preparing rare earth ore concentrate with low-grade light rare earths mine tailing.
Background technology
Owing to its particular configurations of electronic shell of rare earth element and special physicochemical character are widely used in petrochemical complex, metal metallurgy smelting, agricultural, pottery, glass and electronic industry etc.Along with science and technology development, rare earth shows the effect that is difficult to substitute day by day 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, the rare earth reserves occupy the first in the world, and ree content height, kind are many.General when the 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 pollution, endangers peripheral resident's life and health, but also taken a large amount of soils, consumption fund, influences economic benefit of enterprises.
Mineral resources have formed sharp-pointed contradiction as a kind of Nonrenewable resources between the supply that it is limited and the unlimited demand.In the face of the present situation of global Mineral resources shortage, resource is carried out the material recycle repeatedly that recycle namely realizes " resource-product-renewable resource ", thereby realize synthesization, the innoxious use of resource, be the inevitable choice of the sustainable development of socio-economy.Containing various useful elements in the mine tailing, is a kind of potential secondary resource.But in general, in the 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, turns harm into good, and is the important channel of realizing resources effective utilization.
Summary of the invention
The present invention seeks to low-grade light rare earths mine tailing is raw material, the preparation rare earth ore concentrate.
For achieving the above object, the technical solution used in the present invention is: with low-grade light rare earths mine tailing different according to content of rare earth and iron level, adopting magnetic separation, flotation, the molten method that combines of acid is rare earth ore concentrate more than 60% to produce the rare earth taste.Its production technique is: at first low-grade light rare earths mine tailing is carried out ore grinding and screening, obtaining particle diameter is that 100 orders are to the former powder of rare-earth tailing between 200 orders; Select different treatment process: a. to be 1%～4%, when Fe content is 10%～20%, the mine tailing after the screening is sent into flotation unit carry out flotation that it is molten to carry out acid then when REO content according to REO in the mine tailing and Fe content different then; B. when REO content be 4%～6%, when Fe content is 10%～20%, directly to carry out acid molten with the mine tailing after the screening; C. be 1%～4%, when Fe content is 20%～40%, the mine tailing after the screening carried out magnetic separation that and then carry out flotation, it is molten to carry out acid afterwards when REO content; D. when REO content be 4%～6%, when Fe content is 20%～40%, with the screening after mine tailing carry out magnetic separation, it is molten to carry out acid then; 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 was 1～20 when acid was molten, H in the 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; Add at least a in volatile salt, bicarbonate of ammonia, ammoniacal liquor, yellow soda ash, the sodium bicarbonate in the filtrate, to 4.5, the rare earth element in the 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 used for the broad liquid of preparating acid.
After above-mentioned treatment process is handled, rare earth element in the mine tailing mainly enters into rare earth ore concentrate, a small amount of rare earth element enters in magnetic separation or the flotation tailings, and a small amount of rare earth element enters into true tailings, also has a spot of rare earth element to enter among the factory effluent; And most ferro elements have entered into magnetic separation or flotation tailings in the mine tailing, and the iron of a part enters into rare earth ore concentrate, and a spot of iron enters into true tailings, also has a spot of iron to enter into factory effluent.
Described low-grade light rare earths mine tailing middle-weight rare earths 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 handle low-grade (REO=1%～6%); 2, rare earth yield is the highest can reach more than 90%; 3, the gained rare earth ore concentrate is of high grade, can reach 60%; 4, waste water can recycle, and quantity discharged is few, and temperature of reaction is low, energy-saving and emission-reduction; 5, reaction times weak point, the production efficiency height; 6, technical process is simple, and is easy to operate.
Description of drawings
This figure is the process flow sheet that extracts rare earth from rare-earth tailing.
At first low-grade light rare earths mine tailing is carried out ore grinding and screening, obtaining particle diameter is that 100 orders are to the former powder of rare-earth tailing between 200 orders; Select different treatment process according to REO in the mine tailing and Fe content different then:
A. be 1%～4%, when Fe content is 10%～20%, the mine tailing after the screening sent into flotation unit and carried out flotation that it is molten to carry out acid then when REO content; 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 was 1～20 when acid was molten, H in the 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; Add at least a in volatile salt, bicarbonate of ammonia, ammoniacal liquor, yellow soda ash, the sodium bicarbonate in the filtrate, to 4.5, the rare earth element in the 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 used for the broad liquid of preparating acid.
B. when REO content be 4%～6%, when Fe content is 10%～20%, directly to carry out acid molten with the mine tailing after the screening; 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 was 1～20 when acid was molten, H in the 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; Add at least a in volatile salt, bicarbonate of ammonia, ammoniacal liquor, yellow soda ash, the sodium bicarbonate in the filtrate, to 4.5, the rare earth element in the 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 used for the broad liquid of preparating acid.
C. be 1%～4%, when Fe content is 20%～40%, the mine tailing after the screening carried out magnetic separation that and then carry out flotation, it is molten to carry out acid afterwards when REO content; 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 was 1～20 when acid was molten, H in the 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; Add at least a in volatile salt, bicarbonate of ammonia, ammoniacal liquor, yellow soda ash, the sodium bicarbonate in the filtrate, to 4.5, the rare earth element in the 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 used for the broad liquid of preparating acid.
D. when REO content be 4%～6%, when Fe content is 20%～40%, with the screening after mine tailing carry out magnetic separation, it is molten to carry out acid then; 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 was 1～20 when acid was molten, H in the 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; Add at least a in volatile salt, bicarbonate of ammonia, ammoniacal liquor, yellow soda ash, the sodium bicarbonate in the filtrate, to 4.5, the rare earth element in the 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 used for the broad liquid of preparating acid.
Embodiment
The present invention will be further described below in conjunction with embodiment, is not limiting the scope of the invention:
Embodiment 1
Be raw material with low-grade light rare earths mine tailing, REO wherein is that 3.97%, Fe content is 15.7%.At first mine tailing is carried out 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 carries out flotation operation.REO content after the flotation in the mine tailing can reach 39.2%.It is molten to use 0.2mol/L hydrochloric acid to carry out acid to the mine tailing after the flotation, and solid-to-liquid ratio is 1: 5, and the sour molten reaction times is 2h, and sour solubility temperature is normal temperature.The molten back of acid solution is filtered, add ammoniacal liquor in the filtrate to regulate pH, reach at 4.2 o'clock at pH and stop to add ammoniacal liquor, thereby make rare earth element being precipitated out as much as possible in the solution.The solution that will generate precipitation is then sent into whizzer and is carried out centrifugal treating, with the solid oven dry that obtains after centrifugal, finally obtains the rare earth taste and be 70.4% rare earth ore concentrate.The total rate of recovery of true tailings middle-weight rare earths element reaches 90.8%.
Embodiment 2:
Be raw material with low-grade light rare earths mine tailing, the REO in the ore deposit is 4.90%, and iron level is 11.3%.At first that mine tailing is levigate, the former powder of the mine tailing that obtains after levigate is directly carried out sour molten processing.Taking by weighing the former powder of a certain amount of rare-earth tailing, is the nitration mixture of 0.8mol/L with hydrochloric acid and nitric acid preparation in 3: 1 by volume hydrogen ion concentration, adds nitration mixture in 1: 3 ratio of solid-to-liquid ratio in the former powder of mine tailing, at normal temperatures sour molten 2h.Filter after acid is molten.With a certain amount of deionized water wash filter residue, contain certain density rare earth element in the washings, in order further to reclaim rare earth element, reduce wastewater discharge simultaneously, need washings is back in the configuration of acid solution.The filtrate of acid after molten is regulated pH with sodium bicarbonate, make the pH of filtrate reach 4.2, at this moment the rare earth element in the solution is precipitated out in a large number, thereby centrifugal, oven dry obtains rare earth ore concentrate.The content of REO is 65.7% in the gained rare earth ore concentrate, and the total yield of rare earth is 88.9%.
Embodiment 3: with the REO in the ore deposit be 5.32%, iron level is that 28.6% low-grade light rare earths mine tailing is raw material.At first mine tailing being carried out ore grinding handles.The former powder of the mine tailing that will obtain behind ore grinding is sent into magnetic separator and is carried out magnetic separation, and the REO content after the magnetic separation in the mine tailing can reach 7.19%.Take by weighing the former powder of rare-earth tailing after a certain amount of magnetic separation, in the former powder of mine tailing, add H in 1: 5 ratio of solid-to-liquid ratio
+Concentration is the mixed acid solution of hydrochloric acid/nitric acid preparation of 0.75mol/L, and hydrochloric acid and nitric acid ratio are 1: 1 in the nitration mixture.The acid solubility temperature is normal temperature, and the sour molten time is 2h.Filter after acid is molten.Filtrate after acid is molten is regulated pH with bicarbonate of ammonia, makes the pH of filtrate reach 4.0, and at this moment the rare earth element in the 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:
Be raw material with low-grade light rare earths mine tailing, the REO in the 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 the 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 that filters out is sent into magneticstrength greater than 10000 Gausses' magnetic separator, magneticly elects the iron in the former powder, makes in the former powder REO content bring up to 2.26%.To send into flotation unit then and carry out flotation, thereby the REO content in the former powder is brought up to 26.28% except the former powder whipping appts stirring pulping after the intact iron.It is molten to use the hydrochloric acid soln of 1.0mol/L to carry out acid at 1: 10 by solid-to-liquid ratio under 25 ℃ in the former powder of mine tailing then, and sour molten 2h filters after acid is molten.Filter residue washs with deionized water, and water lotion is used for the broad liquid of preparating acid; Filtrate neutralizes with ammoniacal liquor, regulates filtrate pH to 4.2 rare earth element in the filtrate is precipitated out, and centrifugal, oven dry makes content of rare earth and reaches 67.6% rare earth ore concentrate, and the rare earth element total yield is 90.3%.
Claims (8)
1. one kind prepares the method for rare earth ore concentrate with low-grade light rare earths mine tailing, and it is characterized in that: processing step is: a. carries out ore grinding and the former powder of Screening Treatment mine tailing with original debris; B. according to the magnetic separation of the different choice of mine tailing middle-weight rare earths element and iron level elder generation 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, add alkali in the filtrate to regulate pH, the rare earth element in the filtrate is precipitated out, and then obtains rare earth ore concentrate; D. filter residue is washed with water, washing water return preparating acid solution.
2. according to claim 1ly a kind ofly prepare the method for rare earth ore concentrate with low-grade light rare earths mine tailing, it is characterized in that: used rare-earth tailing middle-weight rare earths content is 1%～6%, and iron level is 10%～40%.
3. according to claim 1ly a kind ofly prepare the method for rare earth ore concentrate with low-grade light rare earths mine tailing, it is characterized in that: after ore grinding and the Screening Treatment the former powder of mine tailing footpath at 100 orders between 200 orders.
4. a kind of method for 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 used acid of acid is hydrochloric acid, nitric acid, sulfuric acid or hydrochloric acid, nitric acid and sulfuric acid, the volume ratio of hydrochloric acid, nitric acid and sulfuric acid is (0～3) hydrochloric acid when using mixing acid: (0～3) nitric acid: (0～3) sulfuric acid, acid solutions are 0.1mol/L～1.5mol/L.
5. according to claim 1ly a kind ofly prepare the method for rare earth ore concentrate with low-grade light rare earths mine tailing, it is characterized in that: sour when molten solid-to-liquid ratio between the former powder of mine tailing and the acid solution be 1～20.
6. according to claim 1ly a kind ofly prepare the method for rare earth ore concentrate with low-grade light rare earths mine tailing, it is characterized in that: the sour molten reaction times is 1h～10h.
7. according to claim 1ly a kind ofly prepare the method for rare earth ore concentrate with low-grade light rare earths mine tailing, it is characterized in that: sour solubility temperature is 20 ℃～100 ℃.
8. according to claim 1ly a kind ofly prepare the method for rare earth ore concentrate with low-grade light rare earths mine tailing, it is characterized in that: the filtrate after acid is molten is used at least a with pH regulator to 3.5～4.5 in volatile salt, bicarbonate of ammonia, ammoniacal liquor, yellow soda ash, the sodium bicarbonate.
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105568003A (en) * | 2015-12-31 | 2016-05-11 | 包头稀土研究院 | Method for enriching niobium from Bayan obo tailings |
| CN106191477A (en) * | 2016-08-24 | 2016-12-07 | 北京矿冶研究总院 | Method for separating and recovering rare earth from seabed cobalt-manganese multi-metal oxidized ore |
| CN109277169A (en) * | 2018-09-03 | 2019-01-29 | 王康 | A kind of preparation process of rare earth ore concentrate |
| CN111151374A (en) * | 2020-01-07 | 2020-05-15 | 包钢集团矿山研究院（有限责任公司） | Method for improving rare earth grade of mixed rare earth ore |
| WO2022188248A1 (en) * | 2021-03-12 | 2022-09-15 | 中国地质科学院矿产综合利用研究所 | Method for recovering rare earth from eudialyte |
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| CN101705380A (en) * | 2009-11-30 | 2010-05-12 | 北京有色金属研究总院 | Method for recovering rare earth from rare earth-containing aluminum-silicon materials |
| CN101824536A (en) * | 2009-03-03 | 2010-09-08 | 北京有色金属研究总院 | Process for extracting rare-earth from sulfuric acid treating phosphorite process |
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2012
- 2012-02-09 CN CN2012100288927A patent/CN103243226A/en active Pending
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101824536A (en) * | 2009-03-03 | 2010-09-08 | 北京有色金属研究总院 | Process for extracting rare-earth from sulfuric acid treating phosphorite process |
| CN101705380A (en) * | 2009-11-30 | 2010-05-12 | 北京有色金属研究总院 | Method for recovering rare earth from rare earth-containing aluminum-silicon materials |
Cited By (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN105568003A (en) * | 2015-12-31 | 2016-05-11 | 包头稀土研究院 | Method for enriching niobium from Bayan obo tailings |
| CN105568003B (en) * | 2015-12-31 | 2017-11-17 | 包头稀土研究院 | The method of niobium is enriched with a kind of mine tailing from Bayan Obo |
| CN106191477A (en) * | 2016-08-24 | 2016-12-07 | 北京矿冶研究总院 | Method for separating and recovering rare earth from seabed cobalt-manganese multi-metal oxidized ore |
| CN109277169A (en) * | 2018-09-03 | 2019-01-29 | 王康 | A kind of preparation process of rare earth ore concentrate |
| CN111151374A (en) * | 2020-01-07 | 2020-05-15 | 包钢集团矿山研究院（有限责任公司） | Method for improving rare earth grade of mixed rare earth ore |
| CN111151374B (en) * | 2020-01-07 | 2023-04-18 | 包钢集团矿山研究院（有限责任公司） | Method for improving rare earth grade of mixed rare earth ore |
| WO2022188248A1 (en) * | 2021-03-12 | 2022-09-15 | 中国地质科学院矿产综合利用研究所 | Method for recovering rare earth from eudialyte |
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