CN109722532A - A kind of the leaching mine method and rare-earth products of weathered superficial leaching rare-earth ore - Google Patents

A kind of the leaching mine method and rare-earth products of weathered superficial leaching rare-earth ore Download PDF

Info

Publication number
CN109722532A
CN109722532A CN201910169818.9A CN201910169818A CN109722532A CN 109722532 A CN109722532 A CN 109722532A CN 201910169818 A CN201910169818 A CN 201910169818A CN 109722532 A CN109722532 A CN 109722532A
Authority
CN
China
Prior art keywords
leaching
rare
earth
rare earth
mine
Prior art date
Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
Granted
Application number
CN201910169818.9A
Other languages
Chinese (zh)
Other versions
CN109722532B (en
Inventor
何正艳
张蓉
聂文蕊
徐志高
吴明
瞿军
沙傲阳
Current Assignee (The listed assignees may be inaccurate. Google has not performed a legal analysis and makes no representation or warranty as to the accuracy of the list.)
South Central Minzu University
Original Assignee
South Central University for Nationalities
Priority date (The priority date is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the date listed.)
Filing date
Publication date
Application filed by South Central University for Nationalities filed Critical South Central University for Nationalities
Priority to CN201910169818.9A priority Critical patent/CN109722532B/en
Publication of CN109722532A publication Critical patent/CN109722532A/en
Application granted granted Critical
Publication of CN109722532B publication Critical patent/CN109722532B/en
Active legal-status Critical Current
Anticipated expiration legal-status Critical

Links

Classifications

    • YGENERAL TAGGING OF NEW TECHNOLOGICAL DEVELOPMENTS; GENERAL TAGGING OF CROSS-SECTIONAL TECHNOLOGIES SPANNING OVER SEVERAL SECTIONS OF THE IPC; TECHNICAL SUBJECTS COVERED BY FORMER USPC CROSS-REFERENCE ART COLLECTIONS [XRACs] AND DIGESTS
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

Abstract

The present invention relates to field of hydrometallurgy, in particular to the leaching mine method and rare-earth products of a kind of weathered superficial leaching rare-earth ore.A kind of leaching mine method of weathered superficial leaching rare-earth ore provided by the invention, it includes following steps: leaching weathered superficial leaching rare-earth ore with leaching agent, the re dip solution flowed out from mine soil bottom is collected in two times;After carrying out removal of impurities and precipitating rare earth to the re dip solution that first time collects, the re dip solution collected with second is mixed, and adds leaching agent, and mixed liquor is returned to Rare Earth Mine as fresh leaching agent and carries out leaching operation.Leaching mine method simple possible provided by the invention reduces hydrometallurgy working load and economic and environment-friendly.

Description

A kind of the leaching mine method and rare-earth products of weathered superficial leaching rare-earth ore
Technical field
The present invention relates to field of hydrometallurgy, in particular to a kind of leaching mine method of weathered superficial leaching rare-earth ore And rare-earth products.
Background technique
Middle heavy rare earth reserves contained by weathered superficial leaching rare-earth ore account for 80% or more the world, compensate in mineral type Rare Earth Mine The low deficiency of heavy rare earth content, the downstream industry for receiving heavy rare earth in use are greatly paid close attention to, and are extremely valuable mineral resources, Its development and utilization plays very important effect in world's rare-earth trade.
Currently, the leaching technology that generally uses of weathered superficial leaching rare-earth ore is dump leaching process and Situ Leaching technique, two Person is first to inject a certain amount of leaching agent solution into mine soil, migrates downward into, and is adsorbed on clay mineral in mine soil Rare earth ion occur ion exchange, finally by mine soil bottom deflector hole and intercepting gutter collect re dip solution, and all It send to hydrometallurgy workshop, it, can recovering rare earth through impurity-removing precipitating.
Traditional re dip solution recycles leaching method, is mixed to all re dip solutions flowed out from mine soil bottom It closes and collects, then after concentrating and being cleaned with ammonium hydrogen carbonate, regulate and control pH value of solution, precipitate recovering rare earth.Above-mentioned traditional rare earth leachate circulation Leaching method is to carry out disposable collecting to the re dip solution flowed out from mine soil bottom, therefore collected re dip solution amount is big, Rare earth concentration is low, is typically only 0.5~1.5g/L.A large amount of re dip solution carries out removal of impurities and precipitating rare earth, and hydrometallurgy is made Industry load is big, and the production cycle is long, and it is higher to need to prepare structures, the capital expenditures such as more removal of impurities pond and sedimentation basin;Rare earth leaching Rare earth concentration is too low in liquid out, will lead to dedoping step rare earth loss it is more, the consumption of precipitating reagent increases, rare earth yield It is low.
In view of this, the present invention is specifically proposed.
Summary of the invention
The purpose of the present invention is to provide a kind of leaching mine methods of weathered superficial leaching rare-earth ore, and it is negative to reduce hydrometallurgy operation Lotus reduces the demand to structures such as removal of impurities pond, sedimentation basins, and rare earth leaching rate is high.
Another object of the present invention is to provide a kind of rare-earth products, Purity of Rare Earth is high.
Above-mentioned purpose to realize the present invention, the following technical scheme is adopted:
A kind of leaching mine method of weathered superficial leaching rare-earth ore provided by the invention, comprising the following steps:
Weathered superficial leaching rare-earth ore is leached with leaching agent, the re dip solution flowed out from mine soil bottom is collected in two times;
Re dip solution after carrying out removal of impurities and precipitating rare earth to the re dip solution that first time collects, with second of collection Mixing, adds leaching agent, and mixed liquor is returned to Rare Earth Mine as fresh leaching agent and carries out leaching operation.
The present invention also provides a kind of rare-earth products, according to a kind of leaching mine method of above-mentioned weathered superficial leaching rare-earth ore Leaching obtains.
Compared with the existing technology, the invention has the following advantages:
The present invention carries out the collection of re dip solution in two times, and operation is simple and feasible;Secondly, the present invention only receives first time The re dip solution of collection carries out impurity-removing precipitating operation, reduces hydrometallurgy working load, shortens the production cycle, reduces to removal of impurities The demand of the structures such as pond, sedimentation basin, reduces disposable investment;Secondly, dilute in second of re dip solution collected Soil and concentration impurity ion are lower, and rare earth and concentration impurity ion in the re dip solution collected for the first time, reduction pair can be improved The consumption of cleaner and precipitating reagent, and increase impurities removing efficiency and rare earth yield;In addition, the rare earth that the present invention collects second soaks Liquid out, directly with after impurity-removing precipitating first time collect re dip solution mixed, after adding appropriate leaching agent, without into The adjusting of row pH value of solution can return to mine use, simplify production process, and realize the recycling of mining area waste water, nothing Discharge of wastewater, process economics environmental protection.
Detailed description of the invention
In order to illustrate the technical solution of the embodiments of the present invention more clearly, below will be to needed in the embodiment attached Figure is briefly described, it should be apparent that, be described below in attached drawing be only certain embodiments of the present invention, therefore should not see Work is the restriction to protection scope, for those of ordinary skill in the art, without creative efforts, also It can be with other accompanying drawings can also be obtained according to these attached drawings.
Fig. 1 is weathered superficial leaching rare-earth ore deposit impregnating technology flow chart of the invention;
Fig. 2 is weathered superficial leaching rare-earth ore leaching process elution curve and secondary collection signal in the embodiment of the present invention 1 Figure.
Specific embodiment
Embodiment of the present invention is described in detail below in conjunction with embodiment, but those skilled in the art will Understand, the following example is merely to illustrate the present invention, and is not construed as limiting the scope of the invention.It is not specified in embodiment specific Condition person carries out according to conventional conditions or manufacturer's recommended conditions.Reagents or instruments used without specified manufacturer is The conventional products that can be obtained by commercially available purchase.
A kind of leaching mine method of the weathered superficial leaching rare-earth ore provided below the embodiment of the present invention carries out briefly It is bright.
A kind of leaching mine method of weathered superficial leaching rare-earth ore provided by the invention, includes the following steps:
S1, leaching weathered superficial leaching rare-earth ore
Top water work is carried out using the rare earth element in in-situ lixiviation processing leaching weathered superficial leaching rare-earth ore, then to push up water Industry.Specifically, leaching agent is injected in the ore body that Xiang Tianran is buried, migrates downward into, and is adsorbed on clay mineral in mine soil Rare earth ion occur ion exchange, so that rare earth is entered solution;It is carried out after leaching agent solution and all injecting ore body, then with top water Washing while improving rare earth yield, reduces pollution of the leaching agent to mine soil so that the solution being detained in mine soil is discharged.
Further, in leaching process, the clay mineral for adsorbing rare earth ion constitutes that structure is complicated and a size Non-uniform ion exchange " resin ".Wherein, the clay mineral for adsorbing rare earth ion is stationary phase, and leaching agent is mobile phase, from Sub- exchange reaction occurs between clay mineral and leaching agent.In rare earth ion and leaching agent on clay mineral cation into Row ion exchange, the cation in leaching agent are adsorbed up, and rare earth ion desorbs.In addition, weathered superficial leaching rare-earth Also contain ion phase metal impurities in mine, ion-exchange reactions can also occur with the cation in leaching agent and enters solution In, therefore can be leached with rare earth ion in leaching process, therefore have subsequent impurity-removing precipitating process.
Further, leaching agent is the mixture of one or more of ammonium sulfate, ammonium chloride, ammonium nitrate solution, leaching The mass concentration of agent is 1~4%, and the volume that leaching agent is added in every 1kg Rare Earth Mine is 0.2~0.8L.Wherein, leaching agent is answered This has stronger selectivity, can selectively with mine soil in rare earth element act on, and with the more difficult effect of other components, to reach To preferable separating effect, while inhibiting the leaching of some impurity.In addition, leaching agent and Rare Earth Mine liquid-solid ratio in a certain range Bigger, cation contacts more with the adsorbed rare earth ion of clay mineral in leaching agent, and it is anti-to be also more conducive to ion exchange The progress answered, rare earth leaching rate is also higher, still, after liquid-solid ratio increases to certain value, if continuing to increase, rare earth leaching rate It no longer improves, and since reagent consumption is big, causes the production cost increases to aggravate with carrying capacity of environment, therefore, leached in situ Cheng Zhong, suitable liquid-solid ratio are to guarantee one of the key factor of higher rare earth yield and economic benefit.
Further, top water is the mixture of one or more of distilled water, tap water, river water and well water, and every The volume that top water is added in 1kg Rare Earth Mine is 0.8~1.5L.
S2, re dip solution is collected in two times
As shown in Figure 1, being collected since when re dip solution outflow is arranged at Rare Earth Mine bottom, until the re dip solution collected Volume it is identical as the volume of leaching agent when or when outflow re dip solution concentration be reduced to after a maximum value 0.5g/L with When lower, stop collecting, to collect for the first time;The re dip solution flowed out after collecting for the first time is until there is no re dip solutions When outflow, stops collecting, be collected for second.
Further, the re dip solution collected for the first time, only Zhan always receives the 20~50% of liquid measure, therefore reduces hydrometallurgy work Industry load shortens the production cycle, and reduces the need to structures such as removal of impurities pond, sedimentation basins when the operation of subsequent impurity-removing precipitating It asks, reduces disposable investment;The rare earth concentration of second of re dip solution collected is lower than 0.5g/L simultaneously, can be improved Rare earth and concentration impurity ion in the re dip solution collected for the first time reduce the consumption to cleaner and precipitating reagent, and increase Impurities removing efficiency and rare earth yield.
S3, removal of impurities and settling step
Re dip solution after carrying out removal of impurities and precipitating rare earth to the re dip solution that first time collects, with second of collection Mixing, adds leaching agent, and mixed liquor is returned to Rare Earth Mine as fresh leaching agent and carries out leaching operation.
Further, use mass concentration be 5~20% ammonium hydrogen carbonate as cleaner removal of impurities, then adjust pH to 4.5~ 5.0,1~3h is stirred, supernatant liquor is transferred to sedimentation basin, with precipitating rare earth by still aging 1~6h.Wherein, cleaner with wait remove The volume ratio for the re dip solution that miscellaneous first time collects is 0.004~0.05:1, it is preferable that sulphur is used in present embodiment Acid, hydrochloric acid or ammonium hydroxide adjust pH.
Using ammonium salt leach rare earth when, the foreign ions such as aluminium, iron, calcium, potassium by mineral itself physicochemical properties, leaching The influence of agent solution and related leaching technology is exchanged into re dip solution with rare earth ion by ammonium ion.Weathering crust The major impurity of ion adsorption type rare earth ore leachate has remaining leaching agent, and the non-rare earth ion impurity leached jointly with rare earth from Son.Above-mentioned impurity must be removed before Extraction of rare earth, otherwise will increase the consumption of raw material, and have an effect on rare earth oxide Purity or carbonated rare earth be not easy to form crystalline precipitation.Non-rare earth impurity aluminium exchanges to rare earth ion molten together to some extent In liquid, it is unfavorable for subsequent Extraction of rare eart, the content of aluminium is also to examine the major criterion of rare-earth products quality.
Further, when using ammonium hydrogen carbonate as cleaner in dedoping step, aluminium ion is main in re dip solution Impurity be also formed simultaneously floccule in ammonium bicarbonate precipitation rare earth element and precipitate, lead to rare-earth products purity not Height, and aluminium ion hydrolysis generates gelatinous aluminium hydroxide, makes crystalline active area reduction, crystalline precipitation not easily generated.Therefore, The pH value of solution is adjusted to 4.5~5.0, only the foreign ions such as aluminium will form carbonic acid precipitating at this time, and rare earth does not precipitate.To Achieve the purpose that removal of impurities.
Further, it uses the ammonium hydrogen carbonate that mass concentration is 5~20% as precipitating reagent precipitating rare earth, stirs 1~3h, it is quiet Set 1~6h of ageing;Wherein, the volume ratio of precipitating reagent and the re dip solution after cleaning is 0.01~0.1:1.It is cleaning at this time When the ammonium hydrogen carbonate of above-mentioned amount being added in leaching liquid afterwards, pH is adjusted to 6-7, and rare earth ion will form carbonated rare earth precipitating at this time Get off, obtains carbonated rare earth product.
It should be noted that, although ammonium hydrogen carbonate is all made of in dedoping step and precipitation process, but carbon during two Sour hydrogen ammonium role be completely it is different, in dedoping step, ammonium hydrogen carbonate and aluminium ion are under 4.5~5.0 pH value Generate carbonic acid aluminum precipitation and rare earth does not precipitate.In precipitation process, ammonium hydrogen carbonate and rare earth ion form carbon under the pH value of 6-7 Acid rare earth precipitating.
Further, second of re dip solution collected, the rare earth directly collected with the first time after impurity-removing precipitating soak Liquid is mixed out, after adding appropriate leaching agent, without carrying out the adjusting of pH value of solution, can be returned to mine use, be simplified life Process is produced, and realizes the recycling of mining area waste water, non-wastewater discharge, process economics environmental protection.
Feature and performance of the invention are described in further detail with reference to embodiments.
Embodiment 1
S1, leaching weathered superficial leaching rare-earth ore
The weathered superficial leaching rare-earth ore sample for weighing 250g drying is slowly uniformly charged the glass column that diameter is 45mm In, 2~3 layers of filter paper are spread on ore bed surface, it is then with the speed of 0.4mL/min that 2% ammonium sulfate of 100mL is molten by constant flow pump Liquid, the volume (L) of ammonium sulfate and the liquid-solid ratio of Rare Earth Mine quality (kg) are 0.4:1 at this time, and ammonium sulfate is sent to mine At the top of sample, leaching operation is carried out.Top water operation is carried out after ammonium sulfate whole implantation glass column, then with 200mL distilled water, The liquid-solid ratio of distilled water (L) and Rare Earth Mine quality (kg) are 0.8:1 at this time.
S2, re dip solution is collected in two times
With beaker in glass column bottom collection re dip solution, after effluent volume reaches 100mL, stop receiving for the first time Collection reaches 100mL in the volume of leachate, and instantaneous concentration is respectively 0.32g/L (being less than 0.5g/L) and 0.16g/L at this time, and ammonium The concentration of root is higher, about 0.2mol/L.Then replacement beaker carries out second and collects, until stopping there is no liquid outflow It collects.
In the re dip solution collected for the first time, the concentration of rare earth and aluminium is respectively 2.15g/L and 0.34g/L, ammonium root Concentration is 0.089mol/L.In second of leachate collected, the concentration of rare earth and aluminium is respectively 0.0062g/L and 0.0075g/ L, the concentration of ammonium root are 0.019mol/L.
S3, removal of impurities and settling step
10% ammonium bicarbonate soln of 2.5mL is added in the 100ml re dip solution collected for the first time, and with sulfuric acid and ammonia Water adjusts pH value of solution to 4.5, and after stirring 1h, still aging 3h filters to obtain re dip solution after removal of impurities.
10% ammonium bicarbonate soln of 3.5mL is added after to above-mentioned removal of impurities in re dip solution, it is still aging after stirring 1h 3h filters to obtain carbonated rare earth and supernatant liquor, and in the carbonated rare earth product, Purity of Rare Earth 95.02%, rare earth yield is 96.33%.
The leachate that supernatant liquor is collected with second is mixed, then add moderate amount of sulfuric acid ammonium solid to make into solution Ammonium sulfate concentrations are 2%, the leaching agent that can be recycled.
Column leaching test is carried out to the weathered superficial leaching rare-earth ore sample that 250g is dried with the leaching agent of above-mentioned recycling, weight Multiple above-mentioned test, rare earth extraction rate are 98.41%.
Embodiment 2-6
A kind of weathering provided in the leaching mine method and embodiment for a kind of weathered superficial leaching rare-earth ore that 2-6 is provided is provided The leaching mine method basic operation of shell ion adsorption type rare earth ore is consistent, and difference is, concrete operations condition changes.
Embodiment 2
S1, leaching weathered superficial leaching rare-earth ore
Leaching agent is 3% ammonium sulfate, and pushing up liquid-solid ratio when water operation is 1.2:1.
S2, re dip solution is collected in two times
The re dip solution rare earth concentration collected for the first time is 3.63g/L, and impurity aluminum concentration is 0.41g/L.
S3, removal of impurities and settling step
5% ammonium bicarbonate soln of 5mL is added in dedoping step, and pH is adjusted to 4.8, stirs 1.5h, still aging 4h.
5% ammonium bicarbonate soln of 10mL is added into the leachate after removal of impurities, after stirring 2h, still aging 6h, the carbonic acid In rare-earth products, Purity of Rare Earth is up to 97.34%, rare earth yield 98.12%.
Ammonium sulfate solids are added into supernatant, make ammonium sulfate concentrations 3%, as circulation leaching agent, repeat above-mentioned examination It tests, discovery rare earth extraction rate is 99.16%.
Embodiment 3
S1, leaching weathered superficial leaching rare-earth ore
Leaching agent is 2% ammonium chloride of 50ml, and leaching liquid-solid ratio is 0.2:1, and pushing up liquid-solid ratio when water operation is 1.5:1.
S2, re dip solution is collected in two times
After effluent volume reaches 50mL, stop collecting for the first time.The re dip solution rare earth concentration of collection is for the first time 1.23g/L, impurity aluminum concentration are 0.11g/L.
S3, removal of impurities and settling step
20% ammonium bicarbonate soln of 0.2mL is added in dedoping step, and pH is adjusted to 5.0, stirs 1.5h, still aging 4h.
5% ammonium bicarbonate soln of 0.5mL is added into the leachate after removal of impurities, after stirring 2h, still aging 6h, the carbon In acid rare earth product, Purity of Rare Earth is up to 92.82%, rare earth yield 93.67%.
Chloride solid is added into supernatant, makes ammonium chloride concentration 2%, as circulation leaching agent, repeats above-mentioned examination It tests, discovery rare earth extraction rate is 98.02%.
Embodiment 4
S1, leaching weathered superficial leaching rare-earth ore
Leaching agent is the mixed solution of 150ml 2% ammonium sulfate and 2% ammonium nitrate, and leaching liquid-solid ratio is 0.6:1, and top water is made Liquid-solid ratio when industry is 1:1.
S2, re dip solution is collected in two times
After effluent volume reaches 150mL, stop collecting for the first time.The re dip solution rare earth concentration of collection is for the first time 4.82g/L, impurity aluminum concentration are 0.76g/L.
S3, removal of impurities and settling step
The ammonium bicarbonate soln of 6mL 15% is added in dedoping step, and pH is adjusted to 4.5, stirs 1h, still aging 1h.
The ammonium bicarbonate soln of 6mL 15% is added into the leachate after removal of impurities, after stirring 1h, still aging 1h, the carbon In acid rare earth product, Purity of Rare Earth 96.41%, rare earth yield 97.10%.
Ammonium sulfate and ammonium nitrate solid are added into supernatant, makes ammonium sulfate and ammonium nitrate concn is respectively 2%, as following Ring leaching agent, repeats above-mentioned test, and rare earth extraction rate is 98.66%.
Embodiment 5
S1, leaching weathered superficial leaching rare-earth ore
Leaching agent is the ammonium chloride solution of 200ml 1%, and leaching liquid-solid ratio is 0.8:1, and liquid-solid ratio when pushing up water operation is 0.8:1。
S2, re dip solution is collected in two times
After effluent volume reaches 200mL, stop collecting for the first time.The re dip solution rare earth concentration of collection is for the first time 1.59g/L, impurity aluminum concentration are 0.21g/L.
S3, removal of impurities and settling step
The ammonium bicarbonate soln of 3mL 10% is added in dedoping step, and pH is adjusted to 4.8, stirs 3h, still aging 5h.
The ammonium bicarbonate soln of 4.5mL 10% is added into the leachate after removal of impurities, after stirring 2.5h, still aging 5h, In the carbonated rare earth product, Purity of Rare Earth 94.38%, rare earth yield 96.83%.
Chloride solid is added into supernatant, makes ammonium chloride concentration 1%, as circulation leaching agent, repeats above-mentioned examination It tests, discovery rare earth extraction rate may be up to 96.98%.
Embodiment 6
S1, leaching weathered superficial leaching rare-earth ore
Leaching agent is the mixed solution of 150ml 2% ammonium sulfate and 1% ammonium chloride, and leaching liquid-solid ratio is 0.6:1, and top water is made Liquid-solid ratio when industry is 1:1.
S2, re dip solution is collected in two times
After effluent volume reaches 150mL, stop collecting for the first time.The re dip solution rare earth concentration of collection is for the first time 5.32g/L, impurity aluminum concentration are 0.81g/L.
3, removal of impurities and settling step
The ammonium bicarbonate soln of 5mL 20% is added in dedoping step, and pH is adjusted to 4.5, stirs 1.5h, still aging 4h.
The ammonium bicarbonate soln of 5.5mL 20% is added into the leachate after removal of impurities, after stirring 1.5h, still aging 5h, In the carbonated rare earth product, Purity of Rare Earth 97.72%, rare earth yield 97.63%.
Ammonium sulfate and chloride solid are added into supernatant, makes ammonium sulfate and ammonium chloride concentration is respectively 2% and 1%, As circulation leaching agent, above-mentioned test is repeated, discovery rare earth extraction rate is 98.14%.
Comparative example
A kind of weathering provided in the leaching mine method and embodiment 1 of a kind of weathered superficial leaching rare-earth ore that comparative example provides The leaching mine method basic operation of shell ion adsorption type rare earth ore is consistent, and difference is, Rare Earth Mine leachate disposable collecting, collected dilute Soil leaching liquid measure is big, is 175mL, and rare earth concentration is low, is 1.23g/L, and up to 90.89%, rare earth returns Purity of Rare Earth in rare-earth products Yield is 92.13%.
Fig. 2 is weathered superficial leaching rare-earth ore leaching process elution curve and secondary collection signal in the embodiment of the present invention 1 Figure, as can be seen from Figure 2, the concentration of rare earth, aluminium and ammonium root reduces, most with the increase of elution volume after first increasing to a maximum value After go to zero.100mL, that is, when the leaching agent solution injected is all discharged from ore, leachate are reached in the volume of leachate The instantaneous concentration of middle rare earth and impurity aluminum is lower, respectively 0.32g/L and 0.16g/L, and the concentration of ammonium root is higher, about 0.2mol/L.In the re dip solution collected for the first time, the concentration of rare earth and aluminium is respectively 2.15g/L and 0.34g/L, ammonium root Concentration is 0.089mol/L.In second of leachate collected, the concentration of rare earth and aluminium is respectively 0.0062g/L and 0.0075g/ L, the concentration of ammonium root are 0.019mol/L.
Second of collection of leachate is carried out again, the leachate collected due to second, rare earth and impurity concentration are extremely low, therefore It can be operated without impurity-removing precipitating, direct reuse.Impurity-removing precipitating only is carried out to the re dip solution (100mL) that first time collects Operation, only Zhan always receives the 57% of liquid measure to the partially liq.
The Purity of Rare Earth and rare earth yield of rare-earth products are obtained by the leaching mode in embodiment 1-6 and comparative example It is found that collecting leaching liquid in two times reduces hydrometallurgy working load, the production cycle is shortened.Reduce to removal of impurities pond, sedimentation basin The demand of equal structures, reduces disposable investment.In addition, leachate point two steps collection can be improved and receive liquor for the first time Middle rare earth and concentration impurity ion reduce the consumption to cleaner and precipitating reagent, and increase impurities removing efficiency and rare earth yield, compare In disposable collecting, using the method collected in two times of the invention, rare-earth products purity and rare earth yield are from 90% left side Upper right rises to 95% or more.
The above is only a preferred embodiment of the present invention, is not intended to restrict the invention, for those skilled in the art For member, the invention may be variously modified and varied.All within the spirits and principles of the present invention, it is made it is any modification, Equivalent replacement, improvement etc., should all be included in the protection scope of the present invention.

Claims (10)

1. a kind of leaching mine method of weathered superficial leaching rare-earth ore, which comprises the following steps:
Weathered superficial leaching rare-earth ore is leached with leaching agent, the re dip solution flowed out from mine soil bottom is collected in two times;
After carrying out removal of impurities and precipitating rare earth to the re dip solution that first time collects, the re dip solution collected with second is mixed It closes, adds the leaching agent, mixed liquor is returned into the Rare Earth Mine as fresh leaching agent and carries out leaching operation.
2. a kind of leaching mine method of weathered superficial leaching rare-earth ore according to claim 1, which is characterized in that described It is primary to collect are as follows: to be collected since when the Rare Earth Mine bottom has the re dip solution to flow out, until the rare earth collected When the volume of leachate is identical as the volume of the leaching agent or when the concentration of the re dip solution flowed out is through a maximum value After when being reduced to 0.5g/L or less, stop collecting;Second of collection are as follows: the rare earth flowed out after being collected to first time Leachate is collected, until stopping collecting there is no when re dip solution outflow.
3. a kind of leaching mine method of weathered superficial leaching rare-earth ore according to claim 1, which is characterized in that the leaching Taking agent is ammonium salt solution,
Preferably, the leaching agent includes the mixture of one or more of ammonium sulfate, ammonium chloride, ammonium nitrate solution,
Preferably, the mass concentration of the ammonium salt solution is 1~4%.
4. a kind of leaching mine method of weathered superficial leaching rare-earth ore according to claim 1, which is characterized in that every 1kg The volume that the leaching agent is added in the Rare Earth Mine is 0.2~0.8L.
5. a kind of leaching mine method of weathered superficial leaching rare-earth ore according to claim 1, which is characterized in that further include After the leaching agent all injection Rare Earth Mine, injection top water carries out top water operation.
6. a kind of leaching mine method of weathered superficial leaching rare-earth ore according to claim 5, which is characterized in that the top Water is the mixture of one or more of distilled water, tap water, river water and well water.
7. a kind of leaching mine method of weathered superficial leaching rare-earth ore according to claim 5, which is characterized in that every 1kg The volume that the top water is added in the Rare Earth Mine is 0.8~1.5L.
8. a kind of leaching mine method of weathered superficial leaching rare-earth ore according to claim 1, which is characterized in that described to remove Miscellaneous step are as follows: use the ammonium hydrogen carbonate that mass concentration is 5~20% to clean as cleaner, adjust pH to 4.5~5.0, stirring 1 ~3h, still aging 1~6h;Wherein, the volume ratio of cleaner and the re dip solution of first time collection to be cleaned is 0.004~0.05:1.
9. a kind of leaching mine method of weathered superficial leaching rare-earth ore according to claim 8, which is characterized in that described heavy The step of shallow lake are as follows: it uses the ammonium hydrogen carbonate that mass concentration is 5~20% as precipitating reagent precipitating rare earth, stirs 1~3h, it is still aging 1~6h;Wherein, the volume ratio of the precipitating reagent and the re dip solution after cleaning is 0.01~0.1:1.
10. a kind of rare-earth products, which is characterized in that a kind of its weathered superficial leaching described in -9 any one according to claim 1 The leaching mine method of type Rare Earth Mine leaches to obtain.
CN201910169818.9A 2019-03-06 2019-03-06 Leaching method of weathering crust leaching type rare earth ore and rare earth product Active CN109722532B (en)

Priority Applications (1)

Application Number Priority Date Filing Date Title
CN201910169818.9A CN109722532B (en) 2019-03-06 2019-03-06 Leaching method of weathering crust leaching type rare earth ore and rare earth product

Applications Claiming Priority (1)

Application Number Priority Date Filing Date Title
CN201910169818.9A CN109722532B (en) 2019-03-06 2019-03-06 Leaching method of weathering crust leaching type rare earth ore and rare earth product

Publications (2)

Publication Number Publication Date
CN109722532A true CN109722532A (en) 2019-05-07
CN109722532B CN109722532B (en) 2020-10-30

Family

ID=66301840

Family Applications (1)

Application Number Title Priority Date Filing Date
CN201910169818.9A Active CN109722532B (en) 2019-03-06 2019-03-06 Leaching method of weathering crust leaching type rare earth ore and rare earth product

Country Status (1)

Country Link
CN (1) CN109722532B (en)

Cited By (3)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN112011697A (en) * 2020-09-24 2020-12-01 中国科学院广州地球化学研究所 Method for electrically exploiting rare earth ore and leaching agent for electrically exploiting rare earth ore
CN113699390A (en) * 2020-05-20 2021-11-26 江西理工大学 Impurity removal method for rare earth leaching solution
CN115232992A (en) * 2022-07-27 2022-10-25 中南民族大学 Method for extracting rare earth from weathering crust leaching type rare earth ore by virtue of impurity suppression in stages

Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101476033A (en) * 2008-10-28 2009-07-08 黄日平 Novel method for leaching, impurity removing and precipitating ion type rare earth ore
US20110280778A1 (en) * 2009-02-09 2011-11-17 Xiaowei Huang Method of precipitation of metal ions
CN105803226A (en) * 2016-03-25 2016-07-27 长沙矿冶研究院有限责任公司 Method for extracting rare earth and aluminum from ion adsorption type rare earth ores
CN104328290B (en) * 2013-07-22 2018-06-01 北京有色金属研究总院 A kind of ion type rareearth concentrate acid leaching process
CN108677005A (en) * 2018-06-08 2018-10-19 武汉工程大学 A kind of method of the secondary Situ Leaching recovering rare earth of weathered superficial leaching rare-earth ore
CN108728642A (en) * 2018-06-28 2018-11-02 武汉工程大学 A kind of method of weathered superficial leaching rare-earth ore leachate ammonium bicarbonate precipitation rare earth Mother liquor multiplexing recovering rare earth
CN109055784A (en) * 2018-08-17 2018-12-21 王颖皓 A kind of ion type rareearth ore leaching mother liquor impurity removal process

Patent Citations (7)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101476033A (en) * 2008-10-28 2009-07-08 黄日平 Novel method for leaching, impurity removing and precipitating ion type rare earth ore
US20110280778A1 (en) * 2009-02-09 2011-11-17 Xiaowei Huang Method of precipitation of metal ions
CN104328290B (en) * 2013-07-22 2018-06-01 北京有色金属研究总院 A kind of ion type rareearth concentrate acid leaching process
CN105803226A (en) * 2016-03-25 2016-07-27 长沙矿冶研究院有限责任公司 Method for extracting rare earth and aluminum from ion adsorption type rare earth ores
CN108677005A (en) * 2018-06-08 2018-10-19 武汉工程大学 A kind of method of the secondary Situ Leaching recovering rare earth of weathered superficial leaching rare-earth ore
CN108728642A (en) * 2018-06-28 2018-11-02 武汉工程大学 A kind of method of weathered superficial leaching rare-earth ore leachate ammonium bicarbonate precipitation rare earth Mother liquor multiplexing recovering rare earth
CN109055784A (en) * 2018-08-17 2018-12-21 王颖皓 A kind of ion type rareearth ore leaching mother liquor impurity removal process

Non-Patent Citations (2)

* Cited by examiner, † Cited by third party
Title
丁嘉榆: "对离子型稀土矿原地浸出与堆浸工艺优劣的探讨", 《稀土信息》 *
池汝安: "用碳酸氢铵分离铝和稀土的新工艺研究", 《湖南化工》 *

Cited By (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN113699390A (en) * 2020-05-20 2021-11-26 江西理工大学 Impurity removal method for rare earth leaching solution
CN112011697A (en) * 2020-09-24 2020-12-01 中国科学院广州地球化学研究所 Method for electrically exploiting rare earth ore and leaching agent for electrically exploiting rare earth ore
CN115232992A (en) * 2022-07-27 2022-10-25 中南民族大学 Method for extracting rare earth from weathering crust leaching type rare earth ore by virtue of impurity suppression in stages
CN115232992B (en) * 2022-07-27 2023-07-18 中南民族大学 Method for leaching rare earth in weathered crust leaching type rare earth ore by segmentation and impurity suppression

Also Published As

Publication number Publication date
CN109722532B (en) 2020-10-30

Similar Documents

Publication Publication Date Title
CN101845562B (en) Improved device and method for producing electrolytic manganese metal by two-ore method
CN109722532A (en) A kind of the leaching mine method and rare-earth products of weathered superficial leaching rare-earth ore
CN111926180B (en) Method for extracting ion adsorption type rare earth
CN102191388B (en) Process for extracting vanadium from stone coal through two-section curing with concentrated acid
CN109692715A (en) A kind of method that ground-dipping uranium extraction solves resin poison and blocking
CN107699715B (en) The method of extracting and enriching recovering rare earth from low concentration of rare earth solution
CN101760613B (en) Method for leaching zinc-containing ores
CN101418379B (en) Method for extracting nickel and cobalt by enclosed leaching nickel oxide mine
CN102358645B (en) Fully-closed circulation treatment method for water used by electrolytic manganese metal production
CN102228746A (en) Method for removing fluorine from zinc sulfate solution with active alumina
CN106145164A (en) The method preparing lithium carbonate from lepidolite
CN103184334A (en) Selection-smelting combined technology for treating mixed ore containing molybdenum, oxygen, sulfur and copper
CN109988902B (en) Method for dealkalizing iron-reinforced red mud and separating and recovering iron
US9346934B2 (en) Method for producing nanometer lithopone from electrolytic zinc acid leaching residue
CN105110300B (en) The method that a kind of compound manganese ore of Containing Sulfur manganese extracts manganese and sulphur
CN107012342B (en) A method of the low-grade ion type rareearth raw ore rare earth elements of extraction
Chi et al. Preparation of enriched cerium oxide from bastnasite with hydrochloric acid by two-step leaching
CN105018726B (en) A kind of lead zinc mineral intergrowth processing method
CN106916954B (en) A method of washing lead anode slurry simultaneously recycles lead in lead anode slurry
CN105483399B (en) The manganese carbonate ore leaching method for neutralizing and leaching is leached based on leading portion
CN109321747B (en) Method for leaching manganese concentrate from low-grade calciummanganese ore and regenerating leaching medium
CN106916949A (en) The technique of P204 extractions Extraction of rare earth from southern RE ore
CN106927507A (en) One kind electrolysis MnO2The method for preparing manganese carbonate and ammonium sulfate compound potassium sulfate fertilizer with waste residue containing Mn in electrolysis Mn productions
CN112575205A (en) Device and method for continuously leaching lithium sulfate from spodumene acid clinker
CN102337405B (en) Method for applying baotite mixed carbonate-rare earth precipitation wastewater in precipitation of europium (II) sulfate

Legal Events

Date Code Title Description
PB01 Publication
PB01 Publication
SE01 Entry into force of request for substantive examination
SE01 Entry into force of request for substantive examination
GR01 Patent grant
GR01 Patent grant