CN109136590A - A kind of packet header mixed rare earth concentrate decomposition processing process - Google Patents
A kind of packet header mixed rare earth concentrate decomposition processing process Download PDFInfo
- Publication number
- CN109136590A CN109136590A CN201811102617.9A CN201811102617A CN109136590A CN 109136590 A CN109136590 A CN 109136590A CN 201811102617 A CN201811102617 A CN 201811102617A CN 109136590 A CN109136590 A CN 109136590A
- Authority
- CN
- China
- Prior art keywords
- rare earth
- hydrochloric acid
- activation
- calcination
- 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.)
- Pending
Links
- 238000000034 method Methods 0.000 title claims abstract description 54
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 54
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 31
- 239000012141 concentrate Substances 0.000 title claims abstract description 23
- 238000000354 decomposition reaction Methods 0.000 title claims abstract description 14
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims abstract description 77
- QAOWNCQODCNURD-UHFFFAOYSA-N sulfuric acid Substances OS(O)(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-N 0.000 claims abstract description 65
- 230000004913 activation Effects 0.000 claims abstract description 32
- 238000001354 calcination Methods 0.000 claims abstract description 28
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims abstract description 28
- 238000002386 leaching Methods 0.000 claims abstract description 24
- -1 rare earth sulfate Chemical class 0.000 claims abstract description 23
- 239000002253 acid Substances 0.000 claims abstract description 19
- 238000000605 extraction Methods 0.000 claims abstract description 16
- 239000006210 lotion Substances 0.000 claims abstract description 14
- 229910052684 Cerium Inorganic materials 0.000 claims abstract description 12
- VEXZGXHMUGYJMC-UHFFFAOYSA-M Chloride anion Chemical compound [Cl-] VEXZGXHMUGYJMC-UHFFFAOYSA-M 0.000 claims abstract description 12
- GWXLDORMOJMVQZ-UHFFFAOYSA-N cerium Chemical compound [Ce] GWXLDORMOJMVQZ-UHFFFAOYSA-N 0.000 claims abstract description 12
- 239000012535 impurity Substances 0.000 claims abstract description 10
- 238000004458 analytical method Methods 0.000 claims abstract description 8
- 230000018044 dehydration Effects 0.000 claims abstract description 8
- 238000006297 dehydration reaction Methods 0.000 claims abstract description 8
- 238000005065 mining Methods 0.000 claims abstract description 7
- 230000002411 adverse Effects 0.000 claims abstract description 6
- 238000005457 optimization Methods 0.000 claims abstract description 5
- 239000002893 slag Substances 0.000 claims description 19
- 239000000203 mixture Substances 0.000 claims description 9
- 238000002156 mixing Methods 0.000 claims description 7
- GPRLSGONYQIRFK-UHFFFAOYSA-N hydron Chemical compound [H+] GPRLSGONYQIRFK-UHFFFAOYSA-N 0.000 claims description 3
- 238000000926 separation method Methods 0.000 abstract description 8
- 229910052731 fluorine Inorganic materials 0.000 abstract description 5
- 239000011737 fluorine Substances 0.000 abstract description 4
- PXGOKWXKJXAPGV-UHFFFAOYSA-N Fluorine Chemical compound FF PXGOKWXKJXAPGV-UHFFFAOYSA-N 0.000 abstract 1
- 239000002351 wastewater Substances 0.000 description 7
- 239000007789 gas Substances 0.000 description 6
- 150000003839 salts Chemical class 0.000 description 6
- IKNAJTLCCWPIQD-UHFFFAOYSA-K cerium(3+);lanthanum(3+);neodymium(3+);oxygen(2-);phosphate Chemical compound [O-2].[La+3].[Ce+3].[Nd+3].[O-]P([O-])([O-])=O IKNAJTLCCWPIQD-UHFFFAOYSA-K 0.000 description 5
- 229910052590 monazite Inorganic materials 0.000 description 5
- 238000005406 washing Methods 0.000 description 4
- YCKRFDGAMUMZLT-UHFFFAOYSA-N Fluorine atom Chemical compound [F] YCKRFDGAMUMZLT-UHFFFAOYSA-N 0.000 description 3
- 239000003513 alkali Substances 0.000 description 3
- 238000004519 manufacturing process Methods 0.000 description 3
- 239000002585 base Substances 0.000 description 2
- 239000003518 caustics Substances 0.000 description 2
- 230000029087 digestion Effects 0.000 description 2
- 238000003912 environmental pollution Methods 0.000 description 2
- 238000006386 neutralization reaction Methods 0.000 description 2
- 239000000126 substance Substances 0.000 description 2
- 239000002699 waste material Substances 0.000 description 2
- 229910001122 Mischmetal Inorganic materials 0.000 description 1
- JJEJDZONIFQNHG-UHFFFAOYSA-N [C+4].N Chemical compound [C+4].N JJEJDZONIFQNHG-UHFFFAOYSA-N 0.000 description 1
- 150000001412 amines Chemical class 0.000 description 1
- 230000009286 beneficial effect Effects 0.000 description 1
- 239000003153 chemical reaction reagent Substances 0.000 description 1
- 238000010586 diagram Methods 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 230000007613 environmental effect Effects 0.000 description 1
- 238000003837 high-temperature calcination Methods 0.000 description 1
- 238000009854 hydrometallurgy Methods 0.000 description 1
- 238000009776 industrial production Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 230000000116 mitigating effect Effects 0.000 description 1
- 230000001590 oxidative effect Effects 0.000 description 1
- 238000005507 spraying Methods 0.000 description 1
- 239000001117 sulphuric acid Substances 0.000 description 1
- 235000011149 sulphuric acid Nutrition 0.000 description 1
Classifications
-
- 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
-
- 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
-
- 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
- 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
-
- 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
- C22B3/10—Hydrochloric acid, other halogenated acids or salts thereof
-
- 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
Landscapes
- Chemical & Material Sciences (AREA)
- Engineering & Computer Science (AREA)
- Mechanical Engineering (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Manufacturing & Machinery (AREA)
- Environmental & Geological Engineering (AREA)
- Materials Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geochemistry & Mineralogy (AREA)
- Inorganic Chemistry (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
- Manufacture And Refinement Of Metals (AREA)
Abstract
A kind of packet header mixed rare earth concentrate decomposition processing process, comprising the following steps: packet header mixed rare earth concentrate is carried out calcination for activation by step 1 at a temperature of 350-600 DEG C, and activation time is 1-6 hours, obtains calcination for activation mine；Step 2, calcination for activation are mining, and 3mol/L-8mol/L hydrochloric acid solution carries out the excellent molten leaching of adverse current, obtains the few cerium re chloride and the excellent phase analysis of hydrochloric acid of Low acid；Leached mud and water lotion must be dehydrated after the excellent phase analysis rinse dehydration of step 3, hydrochloric acid；Step 4, dehydration leached mud and the concentrated sulfuric acid are mixed in proportion with quality, are roasted, and obtain sulfuric acid baking mine；Step 5, sulfuric acid baking mine carry out subsequent water logging, neutralize removal of impurities process, obtain rare earth sulfate solution.The method that the present invention uses hydrochloric acid counterflow leaching, earth solution is conducive to subsequent extraction and separation at concentrations up to 250g/L, the leaching for avoiding quadrivalent cerium is leached in hydrochloric acid optimization, it is possible to prevente effectively from the leaching of coordination fluorine, to avoid generating rare earth fluoride three-phase object in extraction process.
Description
Technical field
The present invention relates to field of hydrometallurgy, and in particular to packet header mixed rare earth concentrate decomposition processing process always.
Background technique
China's rare earth resources 80% originate from Inner Mongol packet header, and Baotou rare earth mine is mainly the mixing of bastnaesite and monazite
Mine, since the place of production their relative amount of difference is 9:1-1.1.The chemical formula of bastnaesite is REFCO3, the chemistry of monazite
Formula is REPO4, their chemical property is different, and monazite is more difficult to decompose than bastnaesite.Currently, domestic processing packet header mixed type
The main method of rare earth ore concentrate has concentrated sulfuric acid high-temperature roasting method and concentrated base decomposition method.Concentrated sulfuric acid high-temperature roasting method technique is the concentrated sulfuric acid
Strengthen Roasting Decomposition-water logging-neutralization removal of impurities, obtaining pure mixing rare earth sulfate solution, (mixing sulfuric acid rare earth solubility is low, dense
Highest is spent only to 30-40g/L REO), one rare earth compound of production list is then separated using P507/P204 abstraction and type-reverting, or
Mixed chlorinated rare earth solution is prepared using carbon ammonium precipitation-dissolving with hydrochloric acid, prepares single rare earth compound using extraction and separation.It should
Although method realizes large-scale industrial production, not high to rare earth grade requirement, still, also brings at the same time more serious
Environmental problem.Firstly, waste residue amount is big.Waste residue accounts for about 90% or more of concentrate amount.Secondly, exhaust gas.In concentrated sulfuric acid high-temperature calcination process
It is middle to generate a large amount of gas containing S, F, subsequent recycle using the spraying method and mixed acid solution of the exhaust gas, it is difficult to utilize.
Again, a large amount of waste water (spent shower water, sulfuric acid wastewater containing, amine wastewater of sulphuric acid etc.) of concentrated sulfuric acid high-temperature technology generation seriously pollutes environment.
Concentrated base decomposition method is high (> 55%) to the grade requirement of rare earth ore concentrate；Secondly caustic digestion process is carried out in reactor tank, is operated
Journey is batch operation, limits its large-scale application.
In order to solve above-mentioned industry bottleneck problem, researching and developing that other more environmentally friendly rare earth extraction separation methods become must
It wants.If CN 108165732 discloses a kind of process of two-step method processing Baotou rare earth ore concentrate, specially first by baotite
Oxidizing roasting is leached to obtain the first sulphuric leachate and monazite with sulfuric acid solution, and monazite uses concentrated sulfuric acid low-temperature bake, water again
The second sulphuric leachate is obtained after leaching.This method is whole all to use sulfuric acid leaching, and since sulfuric acid rare earth solubility is low, concentration is only capable of reaching
To 30-40g/LREO, whole be transformed into after high concentration re chloride is needed to carry out extraction and separation again, this process can generate greatly
The sulfuric acid wastewater containing of the low concentration of amount；In addition, the first step uses sulfuric acid leaching, the quadrivalent cerium and fluorine coordination in bastnaesite are leached,
Quadrivalent cerium is needed to add H2O2Reduction reextraction additionally consumes chemical reagent, fluorine element is also needed to be further processed, process
It is relatively complicated.
Summary of the invention
The present invention provides a kind of packet header mixed rare earth concentrate decomposition processing process, individually roasts compared to the concentrated sulfuric acid and alkali
Resolution process, exhaust gas and wastewater flow rate are greatly reduced, and subsequent extraction and separation acid and alkali consumption is much less, and have cost advantage and subtract
Light environmental pollution advantage.
The technical solution adopted in the present invention is as follows:
A kind of packet header mixed rare earth concentrate decomposition processing process, comprising the following steps:
Packet header mixed rare earth concentrate is carried out calcination for activation by step 1 at a temperature of 350-600 DEG C, and activation time is that 1-6 is small
When, obtain calcination for activation mine；
Step 2, calcination for activation are mining, and 3mol/L-8mol/L hydrochloric acid solution carries out the excellent molten leaching of adverse current, obtains few cerium of Low acid
Re chloride and the excellent phase analysis of hydrochloric acid；
Leached mud and water lotion must be dehydrated after the excellent phase analysis rinse dehydration of step 3, hydrochloric acid；
Step 4, dehydration leached mud and the concentrated sulfuric acid are ratio mixing, the roasting of 1:0.8-1.5 with mass ratio, obtain sulfuric acid baking
Mine；
Step 5, sulfuric acid baking mine carry out subsequent water logging, neutralize removal of impurities process, obtain rare earth sulfate solution.
The temperature of calcination for activation is preferably 400-500 DEG C in step 1, and activation time is preferably 2-3 hours.
The concentration of hydrochloric acid solution described in step 2 is preferably 3mol/L-6mol/L.
It is counterflow leaching that hydrochloric acid optimization, which is leached, in step 2, and series is 2-5 grades, and every grade of extraction time is 1-2 hours, few cerium
The concentration of REO is 150-250g/L, pH value 3.5-4.5 in re chloride.
Concentration in step 3 in water lotion containing REO is 10-40g/L, hydrogen ion concentration 0.6-1.0mol/L, the water
Washing lotion will prepare hydrochloric acid solution and continue to leach calcination for activation mine, form closed cycle.
The maturing temperature of slag acid blend is 200-450 DEG C in step 4, calcining time 1-4h.
Concentration in step 5 in obtained rare earth sulfate solution containing REO is 30-40g/L, pH value 1.0-4.5.
The beneficial effects of the present invention are:
The present invention handles packet header mischmetal mine using the excellent molten-concentrated sulfuric acid low-temperature bake of calcination for activation-hydrochloric acid, compared to the concentrated sulfuric acid
Individually roasting and caustic digestion processing, exhaust gas and wastewater flow rate are greatly reduced, and subsequent extraction and separation acid and alkali consumption is much less, and is had
Cost advantage and mitigation environmental pollution advantage.
The present invention uses the concentration of REO in leachate after the excellent molten activation mine of hydrochloric acid adverse current for 150-250g/L, and pH value is
3.5-4.5 saves sulfuric acid rare earth and is transformed into rare earth chloride process, and can save neutralization removal of impurities process, reduces disappearing for lye
Consumption, leachate can be directly entered next procedure and carry out extraction and separation.
The present invention is leached using hydrochloric acid optimization, avoids the leaching of quadrivalent cerium, so that it may the leaching of coordination fluorine is effectively avoided,
To avoid generating rare earth fluoride three-phase object in extraction process.
The present invention is reduced using the excellent molten method of hydrochloric acid adverse current, the consumption of hydrochloric acid, the acidity of excellent solution is lower, is omitted
With removal of impurities process, the consumption of liquid alkaline is reduced.The excellent molten slag of hydrochloric acid is carrying out concentrated sulfuric acid roasting than reducing about 2/3 on ore quality
When, sulfuric acid consumption about reduces 2/3, alleviates the treating capacity of subsequent exhaust gas and waste water significantly.Packet header mixing provided by the invention
The water consume of type Rare Earth Concentrate Decomposition treatment process integrated artistic about reduces 2/3；In addition, since the content of few cerium rare earth chloride is long-range
In the content of sulfuric acid rare earth, the production efficiency of extraction separation process is substantially increased, overall efficiency is significant.
Detailed description of the invention
Fig. 1 is process flow diagram of the invention.
Specific embodiment
A kind of packet header mixed rare earth concentrate decomposition processing process, comprising the following steps:
Packet header mixed rare earth concentrate is carried out calcination for activation by step 1 at a temperature of 350-600 DEG C, and activation time is that 1-6 is small
When, obtain calcination for activation mine；
Step 2, calcination for activation are mining, and 3mol/L-8mol/L hydrochloric acid solution carries out the excellent molten leaching of adverse current, obtains few cerium of Low acid
Re chloride and the excellent phase analysis of hydrochloric acid；
Leached mud and water lotion must be dehydrated after the excellent phase analysis rinse dehydration of step 3, hydrochloric acid；
Step 4, dehydration leached mud and the concentrated sulfuric acid are ratio mixing, the roasting of 1:0.8-1.5 with mass ratio, obtain sulfuric acid baking
Mine；
Step 5, sulfuric acid baking mine carry out subsequent water logging, neutralize removal of impurities process, obtain rare earth sulfate solution.
Further, the temperature of calcination for activation is preferably 400-500 DEG C in step 1, and activation time is preferably 2-3 hours.
Further, the concentration of hydrochloric acid solution described in step 2 is preferably 3mol/L-6mol/L.
Further, it is counterflow leaching that hydrochloric acid optimization, which is leached, in step 2, and series is 2-5 grades, and every grade of extraction time is 1-2
Hour, the concentration of REO is 150-250g/L, pH value 3.5-4.5 in few cerium re chloride.
Further, the concentration in step 3 in water lotion containing REO is 10-40g/L, hydrogen ion concentration 0.6-
1.0mol/L, which, which will prepare hydrochloric acid solution, continues to leach calcination for activation mine, forms closed cycle.
Further, the maturing temperature of slag acid blend is 200-450 DEG C in step 4, calcining time 1-4h.
Further, the concentration in step 5 in obtained rare earth sulfate solution containing REO is 30-40g/L, and pH value is
1.0-4.5。
Present invention be described in more detail combined with specific embodiments below.
Embodiment 1, a kind of packet header mixed rare earth concentrate decomposition processing process, comprising the following steps:
The packet header 300g mixed rare earth concentrates are carried out calcination for activation by step 1, and temperature is 500 DEG C, time 2h, obtain 256g roasting
Burn mine；
Step 2 will roast 3 stage countercurrent leachings of mining hydrochloric acid solution progress, obtain being 170g/L acidity containing REO being that PH is about
3.5 mixed chlorinated rare earth solution and salt acid leaching slag；The concentration of the hydrochloric acid solution is 6mol/L；The re chloride
It is directly entered extracted products technique；
Step 3, salt acid leaching slag are dried after being dehydrated with 200mL water washing, obtain the dry slag of 150g and 200mL water lotion, and water lotion is used
Next group calcination for activation mine is leached in preparing hydrochloric acid solution；
Step 4,150g leach dry slag and the concentrated sulfuric acid and mix in 1:1.2 ratio；Slag acid blend roasts 1.5 under the conditions of 380 DEG C
Hour, obtain sulfuric acid baking mine 245g；
Step 6,245g sulfuric acid baking mine carry out subsequent water logging, neutralize the processes such as removal of impurities, rare earth sulfate solution are obtained, under
One step process.Extraction temperature is 25 DEG C, time 2h, obtains the sulfuric acid rare earth leachate that 2000mL contains REO, the REO's
Concentration is 35g/L.
Embodiment 2
A kind of packet header mixed rare earth concentrate decomposition processing process, comprising the following steps:
The north 300g rare earth ore concentrate is carried out calcination for activation by step 1, and temperature is 450 DEG C, time 2.5h, obtains 261g roasting
Mine；
Step 2 will roast 2 stage countercurrent leachings of mining hydrochloric acid solution progress, obtain being 150g/L acidity containing REO being that PH is about
4.5 mixed chlorinated rare earth solution and salt acid leaching slag；The concentration of the hydrochloric acid solution is 5mol/L；The re chloride
It is directly entered extracted products technique；
Step 3, salt acid leaching slag are dried after being dehydrated with 200mL water washing, obtain the dry slag of 160g and 200mL water lotion, and water lotion is used
Next group calcination for activation mine is leached in preparing hydrochloric acid solution；
Step 4,160g leach dry slag and the concentrated sulfuric acid and mix in 1:1.5 ratio；It is small that slag acid blend roasts 3 under the conditions of 350 DEG C
When, obtain sulfuric acid baking mine 260g；
Step 6,260g sulfuric acid baking mine carry out subsequent water logging, neutralize the processes such as removal of impurities, rare earth sulfate solution are obtained, under
One step process.Extraction temperature is 25 DEG C, time 2h, obtains the sulfuric acid rare earth leachate that 2000mL contains REO, the REO's
Concentration is 40g/L.
Embodiment 3
A kind of packet header mixed rare earth concentrate decomposition processing process, comprising the following steps:
The north 300g rare earth ore concentrate is carried out calcination for activation by step 1, and temperature is 400 DEG C, and time 4h obtains 275g roasted ore；
Step 2 will roast mining hydrochloric acid solution and carry out 5 stage countercurrent leachings, obtain being 250g/L acidity containing REO be PH being about 4
Mixed chlorinated rare earth solution and salt acid leaching slag；The concentration of the hydrochloric acid solution is 8mol/L；The re chloride is straight
It taps into extracted products technique；
Step 3, salt acid leaching slag are dried after being dehydrated with 200mL water washing, obtain the dry slag of 190g and 200mL water lotion, and water lotion is used
Next group calcination for activation mine is leached in preparing hydrochloric acid solution；
Step 4,190g leach dry slag and the concentrated sulfuric acid and mix in 1:1.7 ratio；Slag acid blend roasts 1.5 under the conditions of 450 DEG C
Hour, obtain sulfuric acid baking mine 320g；
Step 6,320g sulfuric acid baking mine carry out subsequent water logging, neutralize the processes such as removal of impurities, rare earth sulfate solution are obtained, under
One step process.Extraction temperature is 25 DEG C, time 2h, obtains the sulfuric acid rare earth leachate that 2900mL contains REO, the REO's
Concentration is 37g/L.
Claims (7)
1. a kind of packet header mixed rare earth concentrate decomposition processing process, it is characterized in that: the following steps are included:
Packet header mixed rare earth concentrate is carried out calcination for activation by step 1 at a temperature of 350-600 DEG C, and activation time is that 1-6 is small
When, obtain calcination for activation mine；
Step 2, calcination for activation are mining, and 3mol/L-8mol/L hydrochloric acid solution carries out the excellent molten leaching of adverse current, obtains few cerium of Low acid
Re chloride and the excellent phase analysis of hydrochloric acid；
Leached mud and water lotion must be dehydrated after the excellent phase analysis rinse dehydration of step 3, hydrochloric acid；
Step 4, dehydration leached mud and the concentrated sulfuric acid are ratio mixing, the roasting of 1:0.8-1.5 with mass ratio, obtain sulfuric acid baking
Mine；
Step 5, sulfuric acid baking mine carry out subsequent water logging, neutralize removal of impurities process, obtain rare earth sulfate solution.
2. process according to claim 1, which is characterized in that the temperature of calcination for activation is preferably 400- in step 1
500 DEG C, activation time is preferably 2-3 hours.
3. process according to claim 1, which is characterized in that the concentration of hydrochloric acid solution described in step 2 is preferably
3mol/L-6mol/L。
4. process according to claim 1, which is characterized in that it is counterflow leaching, grade that hydrochloric acid optimization, which is leached, in step 2
Number is 2-5 grades, and every grade of extraction time is 1-2 hours, and the concentration of REO is 150-250g/L, pH value in few cerium re chloride
For 3.5-4.5.
5. process according to claim 1, which is characterized in that the concentration in step 3 in water lotion containing REO is
10-40g/L, hydrogen ion concentration 0.6-1.0mol/L, which, which will prepare hydrochloric acid solution, continues to leach calcination for activation mine, shape
At closed cycle.
6. process according to claim 1, which is characterized in that the maturing temperature of slag acid blend is in step 4
200-450 DEG C, calcining time 1-4h.
7. process according to claim 1, which is characterized in that contain in obtained rare earth sulfate solution in step 5
The concentration for having REO is 30-40g/L, pH value 1.0-4.5.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811102617.9A CN109136590A (en) | 2018-09-20 | 2018-09-20 | A kind of packet header mixed rare earth concentrate decomposition processing process |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201811102617.9A CN109136590A (en) | 2018-09-20 | 2018-09-20 | A kind of packet header mixed rare earth concentrate decomposition processing process |
Publications (1)
| Publication Number | Publication Date |
|---|---|
| CN109136590A true CN109136590A (en) | 2019-01-04 |
Family
ID=64822963
Family Applications (1)
| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CN201811102617.9A Pending CN109136590A (en) | 2018-09-20 | 2018-09-20 | A kind of packet header mixed rare earth concentrate decomposition processing process |
Country Status (1)
| Country | Link |
|---|---|
| CN (1) | CN109136590A (en) |
Cited By (9)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020030084A1 (en) * | 2018-08-10 | 2020-02-13 | 有研稀土新材料股份有限公司 | Process for smelting and separating rare earth concentrate using combination method |
| CN110923439A (en) * | 2019-12-09 | 2020-03-27 | 四川省冕宁县方兴稀土有限公司 | Method for improving rare earth ore conversion rate in rare earth wet smelting |
| CN111549216A (en) * | 2020-05-22 | 2020-08-18 | 包头稀土研究院 | Decomposition method of rare earth concentrate |
| CN111926181A (en) * | 2020-08-19 | 2020-11-13 | 中国科学院过程工程研究所 | Method for stepwise recovering valuable components in rare earth concentrate |
| CN113621837A (en) * | 2021-08-20 | 2021-11-09 | 湖北省地质实验测试中心(国土资源部武汉矿产资源监督检测中心) | Rare earth extraction method for low-grade fine-fraction rare earth ore |
| 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 |
| CN114314635A (en) * | 2022-01-06 | 2022-04-12 | 四川江铜稀土有限责任公司 | Method for extracting rare earth and recovering fluorine from bastnaesite high-grade leaching residue |
| CN114752788A (en) * | 2022-04-24 | 2022-07-15 | 华卫国 | Roasting method of rare earth ore concentrate added with active agent |
| US12195826B2 (en) | 2022-11-03 | 2025-01-14 | Northeastern University | Mixed rare earth concentrate mineral and suspended mineral phase transformation-clean leaching system and method thereof |
Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61238931A (en) * | 1985-04-13 | 1986-10-24 | Seitetsu Kagaku Co Ltd | Treatment of rare earth concentrate fines |
| CN102146512A (en) * | 2010-02-08 | 2011-08-10 | 北京有色金属研究总院 | Hamartite smelting separation process |
| CN103103349A (en) * | 2013-02-05 | 2013-05-15 | 内蒙古科技大学 | Method for decomposing bayan obo rare earth ore concentrate by acid and alkali combination at low temperature |
| CN103397213A (en) * | 2013-07-22 | 2013-11-20 | 葛新芳 | Method for decomposing and extracting Baotou rare earth ore through mixed alkali roasting process |
| CN104046804A (en) * | 2014-06-25 | 2014-09-17 | 包头华美稀土高科有限公司 | Method for improving concentration of rear earth in lixivium of rear-earth concentrated sulfuric acid roasted ore |
| CN108165732A (en) * | 2017-12-28 | 2018-06-15 | 中国科学院长春应用化学研究所 | A kind of process of two-step method processing Baotou rare earth ore concentrate |
-
2018
- 2018-09-20 CN CN201811102617.9A patent/CN109136590A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JPS61238931A (en) * | 1985-04-13 | 1986-10-24 | Seitetsu Kagaku Co Ltd | Treatment of rare earth concentrate fines |
| CN102146512A (en) * | 2010-02-08 | 2011-08-10 | 北京有色金属研究总院 | Hamartite smelting separation process |
| CN103103349A (en) * | 2013-02-05 | 2013-05-15 | 内蒙古科技大学 | Method for decomposing bayan obo rare earth ore concentrate by acid and alkali combination at low temperature |
| CN103397213A (en) * | 2013-07-22 | 2013-11-20 | 葛新芳 | Method for decomposing and extracting Baotou rare earth ore through mixed alkali roasting process |
| CN104046804A (en) * | 2014-06-25 | 2014-09-17 | 包头华美稀土高科有限公司 | Method for improving concentration of rear earth in lixivium of rear-earth concentrated sulfuric acid roasted ore |
| CN108165732A (en) * | 2017-12-28 | 2018-06-15 | 中国科学院长春应用化学研究所 | A kind of process of two-step method processing Baotou rare earth ore concentrate |
Cited By (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| WO2020030084A1 (en) * | 2018-08-10 | 2020-02-13 | 有研稀土新材料股份有限公司 | Process for smelting and separating rare earth concentrate using combination method |
| CN110923439A (en) * | 2019-12-09 | 2020-03-27 | 四川省冕宁县方兴稀土有限公司 | Method for improving rare earth ore conversion rate in rare earth wet smelting |
| CN111549216A (en) * | 2020-05-22 | 2020-08-18 | 包头稀土研究院 | Decomposition method of rare earth concentrate |
| CN111926181A (en) * | 2020-08-19 | 2020-11-13 | 中国科学院过程工程研究所 | Method for stepwise recovering valuable components in rare earth concentrate |
| CN113621837A (en) * | 2021-08-20 | 2021-11-09 | 湖北省地质实验测试中心(国土资源部武汉矿产资源监督检测中心) | Rare earth extraction method for low-grade fine-fraction rare earth ore |
| 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 |
| 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 |
| CN114314635A (en) * | 2022-01-06 | 2022-04-12 | 四川江铜稀土有限责任公司 | Method for extracting rare earth and recovering fluorine from bastnaesite high-grade leaching residue |
| CN114314635B (en) * | 2022-01-06 | 2023-08-25 | 中稀(凉山)稀土有限公司 | Method for extracting rare earth from bastnaesite optimal leaching slag and recovering fluorine |
| CN114752788A (en) * | 2022-04-24 | 2022-07-15 | 华卫国 | Roasting method of rare earth ore concentrate added with active agent |
| US12195826B2 (en) | 2022-11-03 | 2025-01-14 | Northeastern University | Mixed rare earth concentrate mineral and suspended mineral phase transformation-clean leaching system and method thereof |
Similar Documents
| Publication | Publication Date | Title |
|---|---|---|
| CN109136590A (en) | A kind of packet header mixed rare earth concentrate decomposition processing process | |
| CN107058731B (en) | A kind of technique that platinum palladium product is produced as raw material using Pt Pd concentrate | |
| CN101824554B (en) | Liquid alkali roasting decomposition extraction process of mixed rare earth concentrates | |
| CN101967555B (en) | Method for dipping and decomposing bastnaesite after activation | |
| CN102051477B (en) | Method for chemically separating bastnaesite and urdite from mixed rare earth concentrate | |
| CN101914695B (en) | Method for recovering vanadium from high-silicon high-carbon vanadium ore by wet method | |
| WO2014048385A1 (en) | Method for comprehensively recovering rare earth and fluorine in bastnaesite treatment process | |
| CN102212674A (en) | Process for comprehensively recovering liquid alkali roasting resource of mixed rare earth concentrate | |
| CN109399672B (en) | Method for extracting lithium from spodumene ore and by-producing zeolite or kaliophilite | |
| CN104404243B (en) | A kind of method of soda acid associating low-temperature decomposition low-grade Weishan rare earth ore concentrate | |
| CN103045851A (en) | Technique for decomposing Baotou rare-earth ores | |
| CN108004391A (en) | A kind of method for handling lepidolite extraction metallic element | |
| CN103103349A (en) | Method for decomposing bayan obo rare earth ore concentrate by acid and alkali combination at low temperature | |
| CN103555954A (en) | Method for recovering rare earth elements from waste nickel-metal hydride batteries | |
| CN106337135A (en) | Novel method for producing vanadium pentoxide through ammonium-free vanadium precipitation | |
| CN109811122B (en) | Extraction method of rare earth oxide | |
| CN109811135A (en) | The method and device of selective extraction rare earth oxide from red mud | |
| CN102899488B (en) | Resource transforming method for separating rare earth from fluorine by utilizing rare earth ore concentrate hydrochloric leachate | |
| CN103014316B (en) | Novel method for processing lepidolite material | |
| CN101824531A (en) | Liquid alkali low-temperature roasting decomposition process of caustic soda liquid of mixed rare earth concentrates | |
| CN107746965A (en) | A kind of method of germanium vacuum distillation slag recovery indium germanium | |
| CN106011465A (en) | High-pressure leaching method for Baotou rare-earth ores | |
| CN102732727A (en) | Method for extracting vanadium from high vanadium-sodium-aluminum-silicon slag | |
| CN109022772A (en) | A kind of method that lepidolite ore is leached in sulfuric acid curing | |
| CN108165732A (en) | A kind of process of two-step method processing Baotou rare earth ore concentrate |
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 | ||
| RJ01 | Rejection of invention patent application after publication | ||
| RJ01 | Rejection of invention patent application after publication |
Application publication date: 20190104 |