CN108950188A - The method of concentrated sulfuric acid low-temperature bake phosphorous rare earth ore concentrate step by step arithmetic phosphorus and rare earth - Google Patents
The method of concentrated sulfuric acid low-temperature bake phosphorous rare earth ore concentrate step by step arithmetic phosphorus and rare earth Download PDFInfo
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- CN108950188A CN108950188A CN201810545487.XA CN201810545487A CN108950188A CN 108950188 A CN108950188 A CN 108950188A CN 201810545487 A CN201810545487 A CN 201810545487A CN 108950188 A CN108950188 A CN 108950188A
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- rare earth
- sulfuric acid
- phosphorous
- phosphorus
- ore concentrate
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B1/00—Preliminary treatment of ores or scrap
- C22B1/02—Roasting processes
- C22B1/06—Sulfating roasting
-
- C—CHEMISTRY; METALLURGY
- C01—INORGANIC CHEMISTRY
- C01B—NON-METALLIC ELEMENTS; COMPOUNDS THEREOF; METALLOIDS OR COMPOUNDS THEREOF NOT COVERED BY SUBCLASS C01C
- C01B25/00—Phosphorus; Compounds thereof
- C01B25/16—Oxyacids of phosphorus; Salts thereof
- C01B25/18—Phosphoric acid
- C01B25/22—Preparation by reacting phosphate-containing material with an acid, e.g. wet process
- C01B25/222—Preparation by reacting phosphate-containing material with an acid, e.g. wet process with sulfuric acid, a mixture of acids mainly consisting of sulfuric acid or a mixture of compounds forming it in situ, e.g. a mixture of sulfur dioxide, water and oxygen
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
-
- Y—GENERAL 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
- Y02—TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
- Y02P10/20—Recycling
Abstract
The invention discloses a kind of methods of concentrated sulfuric acid low-temperature bake phosphorous rare earth ore concentrate step by step arithmetic phosphorus and rare earth, comprising: phosphorous rare earth ore concentrate is mixed in proportion with the concentrated sulfuric acid, and Roasting Decomposition under the conditions of 200-350 DEG C obtains roasted ore;Roasted ore is mixed to size mixing with water and is once leached, leaches and obtains phosphoric acid extracting solution and a phase analysis after terminating filtration washing;Phase analysis carries out secondary leaching with dilution heat of sulfuric acid again, leaches and obtains Extraction of rare eart liquid and water logging slag after terminating filtration washing.The present invention utilizes under acid condition, the principle of the diffusion rate difference of the dissolubilities such as ferric phosphate, phosphoric acid rare earth, thorium phosphate and sulfuric acid rare earth and phosphoric acid, step by step arithmetic phosphoric acid, realizes the method with rare earth initial gross separation, overcomes problem of the existing technology.
Description
Technical field
The present invention relates to a kind of hydrometallurgical technologies, specifically, are related to a kind of phosphorous rare earth ore concentrate of concentrated sulfuric acid low-temperature bake
The method of step by step arithmetic phosphorus and rare earth.
Background technique
The rare-earth mineral in the whole world is broadly divided into three kinds of bastnaesite, monazite and weathered superficial leaching rare-earth ore etc..Wherein
Monazite minerals (REPO4) it is phosphorous rare-earth mineral, wherein further including phosphor resource abundant other than containing rare earth resources.
Currently, mainly using concentrated sulfuric acid decomposition technique Extraction of rare earth from phosphorous rare earth ore concentrate, concentrated sulfuric acid decomposition technique is divided into high temperature again
With two kinds of low temperature.In concentrated sulfuric acid high-temperature roasting technique, the phosphorus in iron and monazite in the concentrate shape in high-temperature calcination process
At the ferric phosphate of slightly solubility, in subsequent water logging (faintly acid), N-process, the phosphate radical dissolved out on a small quantity continues the iron shape with dissolution
It is sunk in water logging slag at ferric phosphate.Due to, there are also ingredients such as radionuclide thorium and calcium sulfate, leading to this part phosphorus in water logging slag
Resource is difficult to recycle.To solve sulfuric acid decomposition in technique, tail gas acid acid measures the problems such as big, roasting energy consumption is high, once using low
Warm decomposition technique processing, since decomposition temperature is lower, sulfuric acid entrainment is big in roasted ore, causes phosphoric acid not tangible with ferric sulfate
At stable phosphoric acid iron precipitate, so the resources such as rare earth, phosphorus, iron, thorium enter infusion after being gone out with water logging.Again because of sulfuric acid
Rare earth solubility is lower, to guarantee rare earth dissolution, is leached using a large amount of water, therefore the very low water logging of phosphorus concentration occur
Liquid, meanwhile, the rare earth ion in infusion seriously affects the recycling of phosphorus, causes reclamation of phosphorus resource difficulty big, at high cost.For into
One step obtains pure earth solution, needs to control iron/phosphorus ratio by iron content in increase infusion, and obtain using alkali neutralization
Into ferrophosphorus thorium and slag and sulfuric acid rare earth leachate.It follows that no matter high-temperature technology or low temperature process, be not carried out mixed
The recycling problem of phosphor resource in mould assembly rare-earth mineral.But from technical process it can be appreciated that during low-temperature bake, in concentrate
Phosphorus is actually to be activated and enter infusion, this just provides condition for the recycling of phosphor resource.But phosphoric acid in infusion
Concentration is lower, the RE of high concentration3+、Fe3+And micro radioactivity Th4+Increase etc. recovery difficult is further resulted in.
Summary of the invention
Technical problem solved by the invention is to provide a kind of phosphorous rare earth ore concentrate step by step arithmetic phosphorus of concentrated sulfuric acid low-temperature bake
With the method for rare earth, using under acid condition, the dissolubilities such as ferric phosphate, phosphoric acid rare earth, thorium phosphate and sulfuric acid rare earth and phosphoric acid
The principle of diffusion rate difference, step by step arithmetic phosphoric acid realize the method with rare earth initial gross separation, overcome difficulty of the existing technology
Topic.
Technical solution is as follows:
A kind of method of concentrated sulfuric acid low-temperature bake phosphorous rare earth ore concentrate step by step arithmetic phosphorus and rare earth, comprising:
Phosphorous rare earth ore concentrate is mixed in proportion with the concentrated sulfuric acid, and Roasting Decomposition under the conditions of 200-350 DEG C is roasted
Mine;
Roasted ore is mixed to size mixing with water and is once leached, leaches and obtains phosphoric acid extracting solution and one after terminating filtration washing
Secondary phase analysis;Phase analysis carries out secondary leaching with dilution heat of sulfuric acid again, leach obtained after terminating filtration washing Extraction of rare eart liquid and
Water logging slag.
Further, the ingredient of Extraction of rare eart liquid is sulfuric acid rare earth, the ingredient of water logging slag is calcium sulfate.
Further, the phosphorous rare earth ore concentrate of mixed type or single that phosphorous rare earth ore concentrate is formed using bastnaesite and monazite
Monazite concentrate.
Further, phosphorous rare earth ore concentrate is that 1:1.2-1.8 is mixed according to weight ratio with the concentrated sulfuric acid.
Further, roasted ore includes calcium sulfate, sulfuric acid rare earth crystal, phosphoric acid and undecomposed sulfuric acid.
Further, in a leaching process, the solid and liquid weight ratio of roasted ore and water is 1:0.4-1:2, time 5-30min,
20-60 DEG C of extraction temperature.
Further, the ingredient of phosphoric acid extracting solution includes phosphoric acid, sulfuric acid, one time phase analysis main component includes calcium sulfate and sulfuric acid
Rare earth crystal.
Further, the dilution heat of sulfuric acid that a phase analysis and pH value are 0.5-2 carries out two according to solid and liquid weight ratio 1:6-1:10
Secondary leaching, extraction time 1-3h, extraction temperature are 20-60 DEG C.
The technology of the present invention effect includes:
The present invention overcomes problem of the existing technology, using under acid condition, ferric phosphate, phosphoric acid rare earth, thorium phosphate etc.
The principle of dissolubility and the diffusion rate difference of sulfuric acid rare earth and phosphoric acid, step by step arithmetic phosphoric acid are realized and rare earth initial gross separation
Method.Meanwhile low-temperature bake ring formation frequency is reduced to a certain extent, reach reduction and neutralizes alkali consumption and emissive industrial waste residue
The purpose of minimizing.
(1) rare earth of phosphorous rare earth ore concentrate and phosphor resource extraction are integrated into same smelting process, without individually processing
Rare-earth smelting waste residue recycles phosphor resource.
(2) phosphorous rare-earth mineral resolution ratio is improved using peracid mine ratio, solves the problems, such as engineering ring formation, while providing for phosphorus
It extracts and lays the foundation in source.
(3) extraction raffinate of the high concentration phosphorus acid solution after recycling phosphoric acid can merge with the sulfuric acid rare earth leachate of secondary leaching
Carry out subsequent disposition.
(4) since phosphor resource is extracted, the iron resource introduced for precipitating phosphorus is reduced, while reducing emissive industrial waste residue
The quantity of slag.
Detailed description of the invention
The drawings herein are incorporated into the specification and forms part of this specification, and shows and meets implementation of the invention
Example, and be used to explain the principle of the present invention together with specification.
Fig. 1 is the technique stream of the method for the phosphorous rare earth ore concentrate step by step arithmetic phosphorus of concentrated sulfuric acid low-temperature bake and rare earth in the present invention
Cheng Tu.
Specific embodiment
Be described below and specific embodiments of the present invention be fully shown, with enable those skilled in the art to practice and
It reproduces.
Present invention is mainly used for mixed type rare-earth mineral concentrated sulfuric acid low-temperature bake phosphor resource extraction process.Broad sense is said, is fitted
For in other phosphorus ore containing acid decomposable processes, process to be separately recovered in phosphor resource and metal resource.
As shown in Figure 1, being the method for concentrated sulfuric acid low-temperature bake phosphorous rare earth ore concentrate step by step arithmetic phosphorus and rare earth in the present invention
Process flow chart.
The method of concentrated sulfuric acid low-temperature bake phosphorous rare earth ore concentrate step by step arithmetic phosphorus and rare earth, specifically includes the following steps:
Step 1: by phosphorous rare earth ore concentrate (the phosphorous rare earth ore concentrate of mixed type that bastnaesite and monazite are formed or it is single solely
Occupy stone concentrate) with the concentrated sulfuric acid (concentration 92%-98%) according to weight ratio be 1:1.2-1.8 mix, under the conditions of 200-300 DEG C
Roasting Decomposition obtains roasted ore;
The main component of roasted ore is calcium sulfate, sulfuric acid rare earth crystal, phosphoric acid and undecomposed sulfuric acid.
Sour mine ratio during raising low-temperature bake between sulfuric acid and phosphorous rare earth ore concentrate, excess sulfuric acid will mention for substep
It takes, recycle phosphoric acid and create conditions, while significantly reducing the ring formation frequency during low-temperature bake, improve rare-earth mineral decomposition
Rate.
Step 2: roasted ore is mixed to size mixing with water and is once leached, solid and liquid weight ratio 1:0.4-1:2, time 5-
30min, obtains phosphoric acid extracting solution and a phase analysis after filtration washing by 20-60 DEG C of extraction temperature;
The main component of phosphoric acid extracting solution is phosphoric acid, sulfuric acid, and one time phase analysis main component includes calcium sulfate and sulfuric acid rare earth
Crystal.
During low-temperature bake, since maturing temperature is low, the phosphoric acid of sulfuric acid and generation is undecomposed, and iron ion can not be sent out
The fixed function to phosphate radical is waved, therefore, the phosphate radical in roasted ore is existed with phosphoric acid.And roasting causes to roast mineral water
Totally, calcium sulphate dihydrate and sulfuric acid rare earth crystal wrap up presence in the form of state mix in roasted ore for point evaporation.So in water logging
In the process, phosphoric acid rate of dissolution is exceedingly fast, and sulfuric acid rare earth crystal is influenced to cause rate of dissolution slower by external diffusion mechanism.Cause
This, can use the two rate of dissolution difference and realize initial gross separation.It is obtained in phosphoric acid extracting solution in step by step arithmetic, and because height
The phosphate anion of enrichment controls suitable molten the inhibiting effect of the indissolubles object dissolution equilibrium such as phosphoric acid rare earth, ferric phosphate, thorium phosphate
Solution condition can achieve the target for reducing rare earth, iron, thorium concentration of element in phosphoric acid solution.To be synthetical recovery phosphor resource, subtract
Alkali consumption is neutralized less, reduces the emissive industrial waste residue quantity of slag, and reclamation of phosphorus resource involvement acid technological process system is created conditions.
Step 3: a phase analysis and the dilution heat of sulfuric acid that pH value is 0.5-2 are secondary according to solid and liquid weight ratio 1:6-1:10 progress
It leaches, extraction time 1-3h, extraction temperature is 20-60 DEG C, obtains Extraction of rare eart liquid and water logging slag after filtering rare earth.
The main component of Extraction of rare eart liquid is sulfuric acid rare earth, the main component calcium sulfate of water logging slag.
Embodiment 1
The mixed rare earth concentrate and the concentrated sulfuric acid that rare earth grade is 60% are that 1:1.8 is mixed according to weight ratio, in 350 DEG C of items
Roasting Decomposition under part, obtains roasted ore.Roasted ore is mixed to size mixing with water and is once leached, solid and liquid weight ratio 1:1, when leaching
Between 10min, 30 DEG C of extraction temperature, P is obtained after filtration washing2O5Content is that the phosphoric acid extracting solution of 40g/L and a phase analysis, phosphorus mention
Taking rate is 92%.The dilution heat of sulfuric acid that phase analysis is again 0.5 with pH value carries out secondary leaching according to solid and liquid weight ratio 1:6,
Extraction time 3h, extraction temperature are 40 DEG C, and it is 38g/L, the Extraction of rare eart liquid and water logging slag that pH value is 0.4 that REO is obtained after filtering.
Embodiment 2
The mengite rare-earth concentrate and the concentrated sulfuric acid that rare earth grade is 60% are that 1:1.7 is mixed according to weight ratio, in 350 DEG C of items
Roasting Decomposition 1 hour, obtains roasted ore under part.Roasted ore is mixed to size mixing with water and is once leached, solid and liquid weight ratio 1:2,
Extraction time 10min, obtains P by 40 DEG C of extraction temperature after filtration washing2O5The phosphoric acid extracting solution and primary leaching that content is 21g/L
Slag, phosphorus recovery rate are 95%.The dilution heat of sulfuric acid that phase analysis is again 1 with pH value carries out secondary according to solid and liquid weight ratio 1:6
It leaches, extraction time 3h, extraction temperature is 50 DEG C, and it is 35g/L, the Extraction of rare eart liquid and water that pH value is 0.8 that REO is obtained after filtering
Phase analysis.
Embodiment 3
The mixed rare earth concentrate and the concentrated sulfuric acid that rare earth grade is 60% are that 1:1.6 is mixed according to weight ratio, in 300 DEG C of items
Roasting Decomposition 1 hour, obtains roasted ore under part.Roasted ore is mixed to size mixing with water and is once leached, solid and liquid weight is than 1:
0.4, extraction time 30min, obtain P by 20 DEG C of extraction temperature after filtration washing2O5Phosphoric acid extracting solution that content is 91g/L and primary
Phase analysis, phosphorus recovery rate are 85%.The dilution heat of sulfuric acid that phase analysis is again 2 with pH value carries out two according to solid and liquid weight ratio 1:10
Secondary leaching, extraction time 1h, extraction temperature be 60 DEG C, obtained after filtering REO be 24g/L, pH value be 0.3 Extraction of rare eart liquid and
Water logging slag.
Embodiment 4
The mixed rare earth concentrate and the concentrated sulfuric acid that rare earth grade is 65% are that 1:1.2 is mixed according to weight ratio, in 200 DEG C of items
Roasting Decomposition 2 hours, obtain roasted ore under part.Roasted ore is mixed to size mixing with water and is once leached, solid and liquid weight ratio 1:1,
Extraction time 20min, obtains P by 40 DEG C of extraction temperature after filtration washing2O5The phosphoric acid extracting solution and primary leaching that content is 33g/L
Slag, phosphorus recovery rate are 80%.The dilution heat of sulfuric acid that phase analysis is again 1.5 with pH value carries out two according to solid and liquid weight ratio 1:8
Secondary leaching, extraction time 2h, extraction temperature are 20 DEG C, and it is 41.6g/L, the Extraction of rare eart liquid that pH value is 0.3 that REO is obtained after filtering
And water logging slag.
Embodiment 5
The mengite rare-earth concentrate and the concentrated sulfuric acid that rare earth grade is 50% are that 1:1.5 is mixed according to weight ratio, in 250 DEG C of items
Roasting Decomposition 3 hours, obtain roasted ore under part.Roasted ore is mixed to size mixing with water and is once leached, solid and liquid weight is than 1:
0.7, extraction time 5min, obtain P by 60 DEG C of extraction temperature after filtration washing2O5Phosphoric acid extracting solution that content is 44g/L and primary
Phase analysis, phosphorus recovery rate are 75%.The dilution heat of sulfuric acid that phase analysis is again 1 with pH value carries out two according to solid and liquid weight ratio 1:8
Secondary leaching, extraction time 2h, extraction temperature be 30 DEG C, obtained after filtering REO be 29g/L, pH value be 0.2 Extraction of rare eart liquid and
Water logging slag.
It should be understood that above description be only it is exemplary and explanatory, the present invention can not be limited, the present invention is simultaneously
Be not limited to the process and structure that are described above and are shown in the accompanying drawings, and can carry out without departing from the scope it is various
Modifications and changes.The scope of the present invention is limited only by the attached claims.
Claims (8)
1. a kind of method of concentrated sulfuric acid low-temperature bake phosphorous rare earth ore concentrate step by step arithmetic phosphorus and rare earth, comprising:
Phosphorous rare earth ore concentrate is mixed in proportion with the concentrated sulfuric acid, and Roasting Decomposition under the conditions of 200-350 DEG C obtains roasted ore;
Roasted ore is mixed to size mixing with water and is once leached, leaches and obtains phosphoric acid extracting solution and primary leaching after terminating filtration washing
Slag;Phase analysis carries out secondary leaching with dilution heat of sulfuric acid again, leaches and obtains Extraction of rare eart liquid and water logging after terminating filtration washing
Slag.
2. the method for concentrated sulfuric acid low-temperature bake phosphorous rare earth ore concentrate step by step arithmetic phosphorus and rare earth as described in claim 1, feature
Be: the ingredient of Extraction of rare eart liquid is sulfuric acid rare earth, and the ingredient of water logging slag is calcium sulfate.
3. the method for concentrated sulfuric acid low-temperature bake phosphorous rare earth ore concentrate step by step arithmetic phosphorus and rare earth as described in claim 1, feature
Be: phosphorous rare earth ore concentrate is smart using the phosphorous rare earth ore concentrate of mixed type or single monazite of bastnaesite and monazite formation
Mine.
4. the method for concentrated sulfuric acid low-temperature bake phosphorous rare earth ore concentrate step by step arithmetic phosphorus and rare earth as described in claim 1, feature
Be: phosphorous rare earth ore concentrate is that 1:1.2-1.8 is mixed according to weight ratio with the concentrated sulfuric acid.
5. the method for concentrated sulfuric acid low-temperature bake phosphorous rare earth ore concentrate step by step arithmetic phosphorus and rare earth as described in claim 1, feature
Be: roasted ore includes calcium sulfate, sulfuric acid rare earth crystal, phosphoric acid and undecomposed sulfuric acid.
6. the method for concentrated sulfuric acid low-temperature bake phosphorous rare earth ore concentrate step by step arithmetic phosphorus and rare earth as described in claim 1, feature
Be: in a leaching process, the solid and liquid weight ratio of roasted ore and water is 1:0.4-1:2, time 5-30min, extraction temperature 20-
60℃。
7. the method for concentrated sulfuric acid low-temperature bake phosphorous rare earth ore concentrate step by step arithmetic phosphorus and rare earth as described in claim 1, feature
Be: the ingredient of phosphoric acid extracting solution includes phosphoric acid, sulfuric acid, and a phase analysis main component includes calcium sulfate and sulfuric acid rare earth crystal.
8. the method for concentrated sulfuric acid low-temperature bake phosphorous rare earth ore concentrate step by step arithmetic phosphorus and rare earth as described in claim 1, feature
Be: the dilution heat of sulfuric acid that a phase analysis and pH value are 0.5-2 carries out secondary leaching according to solid and liquid weight ratio 1:6-1:10, leaches
Time 1-3h, extraction temperature are 20-60 DEG C.
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Cited By (6)
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CN113373326A (en) * | 2020-03-09 | 2021-09-10 | 有研稀土新材料股份有限公司 | Method for preparing pure rare earth sulfate solution |
CN113387381A (en) * | 2021-05-10 | 2021-09-14 | 江西铜业技术研究院有限公司 | Process for producing industrial precipitated barium sulfate by taking barite concentrate as raw material |
CN114249308A (en) * | 2021-11-19 | 2022-03-29 | 四川大学 | Method for extracting phosphorus resource and rare earth resource in phosphorus-containing mixed rare earth concentrate |
CN114737049A (en) * | 2021-12-27 | 2022-07-12 | 包头华美稀土高科有限公司 | Method for removing phosphorus in rare earth leaching solution |
CN115029546A (en) * | 2022-05-07 | 2022-09-09 | 包头稀土研究院 | Method for treating mixed rare earth ore |
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 |
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CN113373326A (en) * | 2020-03-09 | 2021-09-10 | 有研稀土新材料股份有限公司 | Method for preparing pure rare earth sulfate solution |
CN113387381A (en) * | 2021-05-10 | 2021-09-14 | 江西铜业技术研究院有限公司 | Process for producing industrial precipitated barium sulfate by taking barite concentrate as raw material |
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CN114249308B (en) * | 2021-11-19 | 2023-09-08 | 四川大学 | Method for extracting phosphorus resources and rare earth resources in phosphorus-containing mixed rare earth concentrate |
CN114737049A (en) * | 2021-12-27 | 2022-07-12 | 包头华美稀土高科有限公司 | Method for removing phosphorus in rare earth leaching solution |
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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 |
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