CN105463190A - Method for ultrasonic leaching of acid-process rare earth roasted ore - Google Patents
Method for ultrasonic leaching of acid-process rare earth roasted ore Download PDFInfo
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- CN105463190A CN105463190A CN201511015061.6A CN201511015061A CN105463190A CN 105463190 A CN105463190 A CN 105463190A CN 201511015061 A CN201511015061 A CN 201511015061A CN 105463190 A CN105463190 A CN 105463190A
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- rare earth
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- roasted ore
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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
- 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
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- 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
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- Mechanical Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
The invention relates to a method for ultrasonic leaching of acid-process rare earth roasted ore. The method is characterized in that acid-process rare earth roasted ore, water and an impurity restraining solvent are mixed for size mixing, size is extracted in an ultrasonic extraction device with the work frequency of (20+/-5) kHz-(30+/-5) kHz and the ultrasonic power of 60 w-600 w for 5-30 min, and sulfuric acid rare earth feed liquid and primary leaching residues are obtained through solid-liquid separation. The primary leaching residues are subjected to ultrasonic washing through dilute sulfuric acid for 5-20 min, and washing fluid and discharge residues are obtained through solid-liquid separation. The washing fluid is reutilized till size mixing leaching. The method has the advantages that the leaching efficiency of rare earth in acid-process rare earth roasted ore can be greatly improved, solid-liquid separation time is shortened, the technological process is simplified, and equipment, energy consumption, labor cost and the occupied area are reduced.
Description
Technical field
The present invention relates to a kind of technique utilizing ultrasonic technology to extract sulfuric acid rare earth in acid system rare earth roasted ore, the method for specifically a kind of acid system rare earth roasted ore ultrasonic wave leaching, belongs to technical field of wet metallurgy.
Background technology
At present, the Bayan Obo mixed rare earth concentrates of more than 90% adopts vitriol oil strengthening Roasting Decomposition art breading.The roasted ore formed through roasting is still using traditional stirring drill traverse treatment process.Roasted ore and water extraction time are greater than 4h, and each washing time, all at more than 40min, adds 3 ~ 4 solid-liquid separation times, and more than 5 hours consuming time of whole technique, efficiency is extremely low.Once leach a large amount of leached muds of formation, still adopt simple agitator treating, make slag middle-weight rare earths can not fully stripping, thus cause REO total recovery to only have about 94%.By analyzing above and can drawing, this technique and equipment also exist length consuming time, and energy consumption is large, the defects such as equipment volume is large, quantity is many, and rare-earth yield is low.
Summary of the invention
The object of this invention is to provide one and utilize ultrasonic extraction mode, the leaching efficiency of sulfuric acid rare earth in rare earth roasted ore is improved, impurity leaching yield reduces, technical process is shortened, and final raising rare earth leaching yield, the method that saving equipment, kind acid system rare earth roasted ore ultrasonic wave that is artificial, energy consumption cost leach.
Concrete technology step of the present invention is:
(1) to be mixed with water by acid system rare earth roasted ore according to solid-liquid weight ratio 1:6 ~ 1:8 and size mixing, the process of sizing mixing adds impurity and presses down solvent, makes mixed serum pH value control 2.0 ~ 4.0; Mixed serum is placed in ultrosonic extractor, controls extraction temperature≤45 DEG C, ultrasound working frequency (20 ± 5) kHz ~ (30 ± 5) kHz, ultrasonic power 60w ~ 600w, extraction time 5min ~ 30min, then solid-liquid separation, obtain a leached mud and sulfuric acid rare earth infusion;
(2) be the dilute sulphuric acid of 0.1mol/L ~ 1mol/L by acidity, with a leached mud according to solid-liquid weight ratio 1:5 ~ 1:10 supersound washing 5 ~ 20min, ultrasound working frequency (20 ± 5) kHz ~ (30 ± 5) kHz, ultrasonic power 60w ~ 600w, solid-liquid separation obtains washings and outer deslagging, and washings reuse is to leaching process of sizing mixing.
Described acid system rare earth roasted ore to be temperature the be cooled or hot acid system rare earth roasted ore of 20 DEG C ~ 450 DEG C;
It is one in magnesium oxide, calcium oxide or ammoniacal liquor that described impurity presses down solvent;
Described dilute sulphuric acid is the acid of eo-acid or the configuration of acid system tail gas treatment process reclaim(ed) sulfuric acid.
Compared with prior art beneficial effect of the present invention is as follows:
The present invention have studied processing condition and the technical parameter of sulfuric acid rare earth in ultrasonic extraction roasted ore, found by research, compared with current technology, roasted ore is after the leaching of 5min ~ 30min, and its REO leaching yield far exceedes current technology 4h and stirs drill traverse result.Further, in ultrasonic wave leaching process, add impurity press down solvent, can a leaching yield of effective inhibition of impurities, selectivity stripping rare earth composition, alleviates impurity treatment amount and REO loss amount in N-process.Because ultrasonic leaching efficiency is higher, so the particle diameter of leached mud is comparatively large, effectively raises the efficiency of solid-liquid separation link.
After a ultrasonic leaching, solid phase particles granularity is very large.Leaching slurry is leached by slush pump shearing-crushing, high speed, is delivered to sheet frame.On sheet frame, loose particle is extruded fragmentation again, and grain graininess significantly reduces, and by the washing of 5min ~ 20min ultrasonic acid, can complete the leaching of residue rare earth.
In traditional technology, one time leached mud adopts mild acid wash, and weak acid pH value is 1.0 ~ 1.5.By the impact of a leached mud middle-weight rare earths salinity character and mode of washing, the total stripping quantity of acid elution process REO is lower.Adopt 0.1 ~ 1.0mol/L dilute sulphuric acid, and in addition intensified by ultrasonic wave leaches, can make in slag remaining can dissolved rare earth fast, all strippings.Therefore, acid system rare earth roasted ore ultrasonic wave leaching-out technique is in advance a kind of, has the processing method of huge economic value.
In general, the present invention greatly can improve the leaching efficiency of acid system rare earth roasted ore middle-weight rare earths, shortens the solid-liquid separation time, simplification of flowsheet, and saves equipment, energy consumption, labour cost and floor space.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
Embodiment 1: according to the solid-liquid weight ratio of 1:7.5, the roasted ore of cooling is mixed with water and sizes mixing, adding small amounts calcium makes mixed serum pH value be 2.0, be placed in ultrosonic extractor, extraction temperature is 28 DEG C, and ultrasonic frequency is 40KHz, ultrasonic power 360w, extraction time is 30min, solid-liquid separation, and in infusion, REO content reaches 41.54g/l.The sulfuric acid of tail gas absorption is diluted to the dilute sulphuric acid of 0.6mol/L, according to solid-liquid weight ratio 1:8 by a leached mud and dilute sulphuric acid ultrasonic leaching 10min, ultrasonic frequency is 40KHz, ultrasonic power 360w, after solid-liquid separation, in washings, REO is that the total leaching yield of 3.98g/l, REO reaches 95.8%.
Embodiment 2: according to the solid-liquid weight ratio of 1:6, the roasted ore of cooling is mixed with water and sizes mixing, adding small amounts magnesium makes mixed serum pH value be 3.0, be placed in ultrosonic extractor, extraction temperature is 28 DEG C, and ultrasonic frequency is 20KHz, ultrasonic power 600w, extraction time is 20min, solid-liquid separation, and in infusion, REO content reaches 51.08g/l.The sulfuric acid of tail gas absorption is diluted to the dilute sulphuric acid of 0.8mol/L, according to solid-liquid weight ratio 1:10 by a leached mud and dilute sulphuric acid ultrasonic leaching 15min, ultrasonic frequency is 20KHz, ultrasonic power 480w, after solid-liquid separation, in washings, REO is that the total leaching yield of 3.18g/l, REO reaches 95.3%.
Embodiment 3: according to the solid-liquid weight ratio of 1:8, hot calcine is mixed with water and sizes mixing, adding a small amount of ammoniacal liquor makes mixed serum pH value be 4.0, be placed in ultrosonic extractor, extraction temperature is 36 ~ 38 DEG C, and ultrasonic frequency is 40KHz, ultrasonic power 360w, extraction time is 10min, solid-liquid separation, and in infusion, REO content reaches 36.85g/l.With the dilute sulphuric acid of vitriol oil configuration 0.5mol/L, according to solid-liquid weight ratio 1:8 by a leached mud and dilute sulphuric acid ultrasonic leaching 20min, ultrasonic frequency is 40KHz, ultrasonic power 360w, after solid-liquid separation, in washings, REO is that the total leaching yield of 6.2g/l, REO reaches 95.4%.
Embodiment 4: according to the solid-liquid weight ratio of 1:7, mixes hot calcine with water and sizes mixing; Be placed in ultrosonic extractor, add small amounts magnesium and make mixed serum pH value be 3.0, extraction temperature is 38 DEG C, and ultrasonic frequency is 20KHz, ultrasonic power 600w, and extraction time is 20min, solid-liquid separation, and in infusion, REO content reaches 44.7g/l.With the dilute sulphuric acid of industrial sulphuric acid configuration 0.1mol/L, according to solid-liquid weight ratio 1:5 by a leached mud and dilute sulphuric acid ultrasonic leaching 10min, ultrasonic frequency is 40KHz, ultrasonic power 360w, after solid-liquid separation, in washings, REO is that the total leaching yield of 2.35g/l, REO reaches 94.8%.
Embodiment 5: according to the solid-liquid weight ratio of 1:8, mixes the roasted ore of cooling with water and sizes mixing; Be placed in ultrosonic extractor, extraction temperature is 28 DEG C, and ultrasonic frequency is 40KHz, ultrasonic power 60w, and extraction time is 30min, solid-liquid separation, and in infusion, REO content reaches 39.44g/l.With the dilute sulphuric acid of industrial sulphuric acid configuration 1mol/L, according to solid-liquid weight ratio 1:8 by a leached mud and dilute sulphuric acid ultrasonic leaching 5min, ultrasonic frequency is 40KHz, ultrasonic power 60w, after solid-liquid separation, in washings, REO is that the total leaching yield of 1.25g/l, REO reaches 95.7%.
Claims (3)
1. a method for acid system rare earth roasted ore ultrasonic wave leaching, is characterized in that: concrete technology step is:
(1) to be mixed with water by acid system rare earth roasted ore according to solid-liquid weight ratio 1:6 ~ 1:8 and size mixing, the process of sizing mixing adds impurity and presses down solvent, makes mixed serum pH value control 2.0 ~ 4.0; Mixed serum is placed in ultrosonic extractor, controls extraction temperature≤45 DEG C, ultrasound working frequency (20 ± 5) kHz ~ (30 ± 5) kHz, ultrasonic power 60w ~ 600w, extraction time 5min ~ 30min, then solid-liquid separation, obtain a leached mud and sulfuric acid rare earth infusion;
(2) be the dilute sulphuric acid of 0.1mol/L ~ 1mol/L by acidity, with a leached mud according to solid-liquid weight ratio 1:5 ~ 1:10 supersound washing 5 ~ 20min, ultrasound working frequency (20 ± 5) kHz ~ (30 ± 5) kHz, ultrasonic power 60w ~ 600w, solid-liquid separation obtains washings and outer deslagging, and washings reuse is to leaching process of sizing mixing.
2. the method that leaches of acid system rare earth roasted ore ultrasonic wave according to claim 1, is characterized in that: acid system rare earth roasted ore to be temperature the be cooled or hot acid system rare earth roasted ore of 20 DEG C ~ 450 DEG C.
3. the method that leaches of acid system rare earth roasted ore ultrasonic wave according to claim 1, is characterized in that: it is one in magnesium oxide, calcium oxide or ammoniacal liquor that impurity presses down solvent.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201511015061.6A CN105463190A (en) | 2015-12-31 | 2015-12-31 | Method for ultrasonic leaching of acid-process rare earth roasted ore |
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| CN201511015061.6A CN105463190A (en) | 2015-12-31 | 2015-12-31 | Method for ultrasonic leaching of acid-process rare earth roasted ore |
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| CN105463190A true CN105463190A (en) | 2016-04-06 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108342598A (en) * | 2017-01-25 | 2018-07-31 | 连云港市丽港稀土实业有限公司 | The separation method of concomitant radioactivity nucleic in a kind of rare earth waste leachate |
Citations (4)
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| CN1920068A (en) * | 2006-08-22 | 2007-02-28 | 扬州大学 | Ultrasound leaching technique of concentrated sulfuric acid roasting rare earth concentrate |
| CN101012499A (en) * | 2007-02-05 | 2007-08-08 | 扬州大学 | Method for separating highly-pure rare-earth oxide from sulphating roasting rare earth mine |
| CN101012510A (en) * | 2007-02-05 | 2007-08-08 | 扬州大学 | Method for hypersonic rare earth leaching |
| CN103924073A (en) * | 2014-04-28 | 2014-07-16 | 包头稀土研究院 | Method for decomposing rare earth ore concentrate through roasting by liquid caustic soda and acid-leaching rare earth through intensifying by ultrasonic |
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2015
- 2015-12-31 CN CN201511015061.6A patent/CN105463190A/en active Pending
Patent Citations (4)
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|---|---|---|---|---|
| CN1920068A (en) * | 2006-08-22 | 2007-02-28 | 扬州大学 | Ultrasound leaching technique of concentrated sulfuric acid roasting rare earth concentrate |
| CN101012499A (en) * | 2007-02-05 | 2007-08-08 | 扬州大学 | Method for separating highly-pure rare-earth oxide from sulphating roasting rare earth mine |
| CN101012510A (en) * | 2007-02-05 | 2007-08-08 | 扬州大学 | Method for hypersonic rare earth leaching |
| CN103924073A (en) * | 2014-04-28 | 2014-07-16 | 包头稀土研究院 | Method for decomposing rare earth ore concentrate through roasting by liquid caustic soda and acid-leaching rare earth through intensifying by ultrasonic |
Non-Patent Citations (1)
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| 王翠珍等: ""超声振荡条件下赤泥盐酸介质浸提钪的研究"", 《无机盐工业》 * |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108342598A (en) * | 2017-01-25 | 2018-07-31 | 连云港市丽港稀土实业有限公司 | The separation method of concomitant radioactivity nucleic in a kind of rare earth waste leachate |
| CN108342598B (en) * | 2017-01-25 | 2020-05-22 | 连云港市丽港稀土实业有限公司 | Method for separating associated radionuclides in rare earth waste residue leachate |
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Application publication date: 20160406 |