CN103343245B - Method for removing impurity aluminum in rare earth solution by neutralization-magnetic flocculation-magnetic separation - Google Patents
Method for removing impurity aluminum in rare earth solution by neutralization-magnetic flocculation-magnetic separation Download PDFInfo
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- CN103343245B CN103343245B CN201310295016.5A CN201310295016A CN103343245B CN 103343245 B CN103343245 B CN 103343245B CN 201310295016 A CN201310295016 A CN 201310295016A CN 103343245 B CN103343245 B CN 103343245B
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- 229910052782 aluminium Inorganic materials 0.000 title claims abstract description 32
- 229910052761 rare earth metal Inorganic materials 0.000 title claims abstract description 32
- 150000002910 rare earth metals Chemical class 0.000 title claims abstract description 32
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 title claims abstract description 27
- 238000000034 method Methods 0.000 title claims abstract description 25
- 239000012535 impurity Substances 0.000 title claims abstract description 11
- 238000007885 magnetic separation Methods 0.000 title claims abstract description 11
- 239000007788 liquid Substances 0.000 claims abstract description 53
- 238000003756 stirring Methods 0.000 claims abstract description 21
- 239000012141 concentrate Substances 0.000 claims abstract description 19
- 239000002253 acid Substances 0.000 claims abstract description 17
- 238000005189 flocculation Methods 0.000 claims abstract description 12
- 230000016615 flocculation Effects 0.000 claims abstract description 12
- 239000000463 material Substances 0.000 claims abstract description 11
- HEMHJVSKTPXQMS-UHFFFAOYSA-M Sodium hydroxide Chemical compound [OH-].[Na+] HEMHJVSKTPXQMS-UHFFFAOYSA-M 0.000 claims description 15
- VEXZGXHMUGYJMC-UHFFFAOYSA-N Hydrochloric acid Chemical compound Cl VEXZGXHMUGYJMC-UHFFFAOYSA-N 0.000 claims description 10
- 238000013019 agitation Methods 0.000 claims description 10
- 125000002091 cationic group Chemical group 0.000 claims description 10
- 239000006148 magnetic separator Substances 0.000 claims description 10
- 229920002401 polyacrylamide Polymers 0.000 claims description 10
- 229920000642 polymer Polymers 0.000 claims description 10
- 239000003795 chemical substances by application Substances 0.000 claims description 6
- 239000000701 coagulant Substances 0.000 claims description 6
- NIXOWILDQLNWCW-UHFFFAOYSA-N Acrylic acid Chemical compound OC(=O)C=C NIXOWILDQLNWCW-UHFFFAOYSA-N 0.000 claims description 5
- QAOWNCQODCNURD-UHFFFAOYSA-L Sulfate Chemical compound [O-]S([O-])(=O)=O QAOWNCQODCNURD-UHFFFAOYSA-L 0.000 claims description 5
- 230000002378 acidificating effect Effects 0.000 claims description 5
- 235000011114 ammonium hydroxide Nutrition 0.000 claims description 5
- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 claims description 5
- 239000002105 nanoparticle Substances 0.000 claims description 5
- 239000007787 solid Substances 0.000 claims description 5
- 239000002562 thickening agent Substances 0.000 claims description 5
- HIZCIEIDIFGZSS-UHFFFAOYSA-L trithiocarbonate Chemical compound [S-]C([S-])=S HIZCIEIDIFGZSS-UHFFFAOYSA-L 0.000 claims description 5
- 239000012989 trithiocarbonate Substances 0.000 claims description 5
- 239000002699 waste material Substances 0.000 claims description 5
- 238000002360 preparation method Methods 0.000 claims 1
- 238000000926 separation method Methods 0.000 abstract description 6
- -1 aluminum ions Chemical class 0.000 abstract description 5
- 238000001914 filtration Methods 0.000 abstract description 4
- 230000007062 hydrolysis Effects 0.000 abstract description 3
- 238000006460 hydrolysis reaction Methods 0.000 abstract description 3
- 238000006386 neutralization reaction Methods 0.000 abstract description 2
- 238000004090 dissolution Methods 0.000 abstract 2
- 238000002156 mixing Methods 0.000 abstract 1
- 230000035515 penetration Effects 0.000 abstract 1
- 239000004411 aluminium Substances 0.000 description 14
- REDXJYDRNCIFBQ-UHFFFAOYSA-N aluminium(3+) Chemical compound [Al+3] REDXJYDRNCIFBQ-UHFFFAOYSA-N 0.000 description 4
- 238000001556 precipitation Methods 0.000 description 3
- PNEYBMLMFCGWSK-UHFFFAOYSA-N aluminium oxide Inorganic materials [O-2].[O-2].[O-2].[Al+3].[Al+3] PNEYBMLMFCGWSK-UHFFFAOYSA-N 0.000 description 2
- 230000004888 barrier function Effects 0.000 description 2
- 239000003513 alkali Substances 0.000 description 1
- 238000005516 engineering process Methods 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 238000004519 manufacturing process Methods 0.000 description 1
- 239000000203 mixture Substances 0.000 description 1
- 239000002245 particle Substances 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000002002 slurry Substances 0.000 description 1
Classifications
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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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- Manufacture And Refinement Of Metals (AREA)
- Separation Of Suspended Particles By Flocculating Agents (AREA)
Abstract
The invention discloses a method for removing impurity aluminum in a rare earth solution by neutralization-magnetic flocculation-magnetic separation. The method comprises the following steps of: acid dissolution, concentration, neutralization, stirring and mixing, magnetic flocculation and magnetic separation. According to the process, the concentration of aluminum ions in a rare earth acid dissolution material solution can be reduced from more than 1g/L to 200mg/L; the investment is low, the flow process is simple, the treatment quantity is large, and the problems of filtration missing and penetration caused by filtration of a hydrolysis method are avoided; the method is mainly applied to rare earth concentrates with high aluminum content; and by adopting the method, the two major difficult problems of difficulty in solid-liquid separation and over-standard aluminum of the material solution can be simultaneously solved.
Description
Technical field
The invention belongs to rare earth metal separating-purifying field, be specifically related to the separated method of removing impurity aluminum in earth solution of a kind of neutralization-magnetic flocculation-magnetic.
Background technology
At present, generally adopt " sour molten-precipitation " art breading rare earth ore concentrate before rare earth metal separating-purifying, the impurity aluminum in rare earth ore concentrate enters the molten feed liquid of rare earth acid thus, and becomes the main source of aluminium in rare earth metal.The rare earth ore concentrate that aluminium content is high will cause that in sour molten feed liquid, aluminium ion concentration is too high, and then affects Rare Earth Separation operation, even final rare-earth products quality.Therefore, obtain qualified rare-earth products, first should solve the high problem of aluminium content in rare earth ore concentrate.
Chinese scholars to lower concentration in solution aluminum ions removal carried out a large amount of research, document is also abundanter, but the research of removing for the molten feed liquid middle and high concentration aluminum ion of rare earth ore concentrate acid is rare.Zan laughs at big passing through Al in high concentrated acid alkali wasteliquid
3+exist the research of form and feature to find, as Al (OH)
3when concentration reaches 3.6g/L, the feed liquid after employing neutralisation is processed is the starchiness slurry of " plastic fluid " feature, Al wherein (OH)
3be not to exist with flco, but exist with particle state, solid-liquid separation is extremely difficult, and easily wears filter.Can draw thus, when aluminium ion concentration is greater than 3.6g/L in the molten feed liquid of rare earth acid, adopts and first regulate pH value, make aluminum ion generate Al (OH)
3the method of carrying out again solid-liquid separation is difficult to realize industrialization.Therefore the deep processing that, how effectively to remove aluminum ion in the molten feed liquid of high alumina type rare earth ore concentrate acid, realizes Rare-earth Industry is technical barrier urgently to be resolved hurrily at present.
Domestic many enterprises rare earth ore concentrate used belongs to high alumina type, causes thus sour molten feed liquid aluminium composition height and solid-liquid separation difficult.Become a large technical barrier of enterprise.At present, a lot of enterprises adopt repeatedly the method for press filtration+multi stage precipitation to make the aluminium content in feed liquid drop to 1g/L by 6g/L, and adopt repeatedly press filtration+multi stage precipitation operation not only floor space be large, the production cost of intermittent operation, unit material is high, the more important thing is that in rare earth feed liquid, aluminium content still fails to reach below 0.5g/L.
Summary of the invention
The object of the present invention is to provide the separated method of removing impurity aluminum in earth solution of a kind of neutralization-magnetic flocculation-magnetic, this technique can make aluminium ion concentration in the molten feed liquid of rare earth acid once drop to 200mg/L by > 1g/L; Invest littlely, flow process is simple, and treatment capacity is large, the leakage filter of having avoided adopting hydrolysis method to occur, wears filter problem.
For achieving the above object, the present invention adopts following technical scheme:
The separated method of removing impurity aluminum in earth solution of neutralization-magnetic flocculation-magnetic comprises the following steps: acid is molten, concentrate, neutralize, be uniformly mixed, magnetic flocculation, magnetic are separated.Concrete steps are as follows: adopt concentrated hydrochloric acid to dissolve rare earth ore concentrate, the earth solution pH value of adjusting after dissolving is 3.5 ~ 4.0, temperature is 40 ~ 90 ℃, then adopts Hhigh-efficient thickener concentrated, and the solid after concentrating returns to sour molten operation, it is 5.20 ~ 5.30 that concentrated solution first adds NaOH adjustment pH value, feed temperature is adjusted to below 15 ~ 35 ℃, and adding ammoniacal liquor adjustment pH value is 5.43, in agitation vat, with 400 ~ 800 revs/min of speed, stirs, (Polyferric Sulfate, consumption is 0.03 ~ 0.09kg/m to add coagulant aids
3feed liquid), 2 ~ 5 minutes used times, with the speed of 80 ~ 200 revs/min, stir, add simultaneously flocculation agent (cationic polyacrylamide, cationic degree is 50 ~ 60, molecular weight is 300 ~ 8,000,000, consumption is 0.02 ~ 0.06kg/m
3feed liquid) and the modified Nano Z 250 (block polymer of preparing vinylformic acid and polyacrylamide with S-butyl-S '-isopropyl acidic group trithiocarbonate, the pH value of telomerized polymer solution is 5, then itself and ferriferrous oxide nano-particle is mixed in to violent stirring 1.5 ~ 2.5h under room temperature; Consumption is 0.5 ~ 3kg/m
3feed liquid), 1 ~ 5 minute used time, with the speed of 80 ~ 200 revs/min, stir 5 ~ 10 minutes, mixed liquor enters in low intensity magnetic separator and carries out magnetic separation, and feed liquid is qualified feed liquid; Throw out enters connecting material in case of magnetic separator together with magnetic, and by wash agitation groove, rotating speed is 400 ~ 800 revs/min, adjusting pH value is 5 ~ 8, is uniformly mixed 1 ~ 5min, then enters secondary magnetic separated, nano ferriferrous oxide is reclaimed, and recycles, waste liquid individual curing.
Remarkable advantage of the present invention is:
(1) this technique can make aluminium ion concentration in the molten feed liquid of rare earth acid once drop to 200mg/L by > 1g/L; Invest littlely, flow process is simple, and treatment capacity is large, the leakage filter of having avoided adopting hydrolysis method to occur, wears filter problem.
(2) be mainly used in the rare earth ore concentrate of high aluminium content.Can solve the difficult and aluminium of feed liquid solid-liquid separation two hang-ups that exceed standard simultaneously.
Accompanying drawing explanation
Fig. 1 is process flow sheet of the present invention.
Embodiment
embodiment 1
Adopt the separated method of removing impurity aluminum in earth solution of neutralization-magnetic flocculation-magnetic to comprise the following steps: acid is molten, concentrate, neutralize, be uniformly mixed, magnetic flocculation, magnetic separation.Concrete steps are as follows: adopt concentrated hydrochloric acid to dissolve rare earth ore concentrate, the earth solution pH value of adjusting after dissolving is 4.0, temperature is 90 ℃, then adopts Hhigh-efficient thickener concentrated, and the solid after concentrating returns to sour molten operation, it is 5.30 that concentrated solution first adds NaOH adjustment pH value, feed temperature is adjusted to below 35 ℃, and adding ammoniacal liquor adjustment pH value is 5.43, in agitation vat, with 800 revs/min of speed, stirs, (Polyferric Sulfate, consumption is 0.09kg/m to add coagulant aids
3feed liquid), 5 minutes used times, with the speed of 200 revs/min, stir, add simultaneously flocculation agent (cationic polyacrylamide, cationic degree is 50 ~ 60, molecular weight is 300 ~ 8,000,000, consumption is 0.06kg/m
3feed liquid) and the modified Nano Z 250 (block polymer of preparing vinylformic acid and polyacrylamide with S-butyl-S '-isopropyl acidic group trithiocarbonate, the pH value of telomerized polymer solution is 5, then itself and ferriferrous oxide nano-particle is mixed in to violent stirring 2.5h under room temperature; Consumption is 3kg/m
3feed liquid), 5 minutes used times, with the speed of 200 revs/min, stir 10 minutes, mixed liquor enters in low intensity magnetic separator and carries out magnetic separation, and feed liquid is qualified feed liquid; Throw out enters connecting material in case of magnetic separator together with magnetic, and by wash agitation groove, rotating speed is 800 revs/min, adjusting pH value is 8, is uniformly mixed 5min, then enters secondary magnetic separated, nano ferriferrous oxide is reclaimed, and recycles, waste liquid individual curing.
In the molten feed liquid of rare earth acid, aluminium content is 2.92g/L, and material liquid aluminium content is after treatment 153mg/L.
embodiment 2
Adopt the separated method of removing impurity aluminum in earth solution of neutralization-magnetic flocculation-magnetic to comprise the following steps: acid is molten, concentrate, neutralize, be uniformly mixed, magnetic flocculation, magnetic separation.Concrete steps are as follows: adopt concentrated hydrochloric acid to dissolve rare earth ore concentrate, the earth solution pH value of adjusting after dissolving is 3.5, temperature is 40 ℃, then adopts Hhigh-efficient thickener concentrated, and the solid after concentrating returns to sour molten operation, it is 5.20 that concentrated solution first adds NaOH adjustment pH value, feed temperature is adjusted to below 15 ℃, and adding ammoniacal liquor adjustment pH value is 5.43, in agitation vat, with 400 revs/min of speed, stirs, (Polyferric Sulfate, consumption is 0.03kg/m to add coagulant aids
3feed liquid), 2 minutes used times, with the speed of 80 revs/min, stir, add simultaneously flocculation agent (cationic polyacrylamide, cationic degree is 50 ~ 60, molecular weight is 300 ~ 8,000,000, consumption is 0.02kg/m
3feed liquid) and the modified Nano Z 250 (block polymer of preparing vinylformic acid and polyacrylamide with S-butyl-S '-isopropyl acidic group trithiocarbonate, the pH value of telomerized polymer solution is 5, then itself and ferriferrous oxide nano-particle is mixed in to violent stirring 1.5h under room temperature; Consumption is 0.5kg/m
3feed liquid), 1 minute used time, with the speed of 80 revs/min, stir 5 minutes, mixed liquor enters in low intensity magnetic separator and carries out magnetic separation, and feed liquid is qualified feed liquid; Throw out enters connecting material in case of magnetic separator together with magnetic, and by wash agitation groove, rotating speed is 400 revs/min, adjusting pH value is 5, is uniformly mixed 1min, then enters secondary magnetic separated, nano ferriferrous oxide is reclaimed, and recycles, waste liquid individual curing.
In the molten feed liquid of rare earth acid, aluminium content is 2.08g/L, and material liquid aluminium content is after treatment 143mg/L.
embodiment 3
Adopt the separated method of removing impurity aluminum in earth solution of neutralization-magnetic flocculation-magnetic to comprise the following steps: acid is molten, concentrate, neutralize, be uniformly mixed, magnetic flocculation, magnetic separation.Concrete steps are as follows: adopt concentrated hydrochloric acid to dissolve rare earth ore concentrate, the earth solution pH value of adjusting after dissolving is 3.8, temperature is 70 ℃, then adopts Hhigh-efficient thickener concentrated, and the solid after concentrating returns to sour molten operation, it is 5.25 that concentrated solution first adds NaOH adjustment pH value, feed temperature is adjusted to below 30 ℃, and adding ammoniacal liquor adjustment pH value is 5.43, in agitation vat, with 600 revs/min of speed, stirs, (Polyferric Sulfate, consumption is 0.06kg/m to add coagulant aids
3feed liquid), 3 minutes used times, with the speed of 100 revs/min, stir, add simultaneously flocculation agent (cationic polyacrylamide, cationic degree is 50 ~ 60, molecular weight is 300 ~ 8,000,000, consumption is 0.02kg/m
3feed liquid) and the modified Nano Z 250 (block polymer of preparing vinylformic acid and polyacrylamide with S-butyl-S '-isopropyl acidic group trithiocarbonate, the pH value of telomerized polymer solution is 5, then itself and ferriferrous oxide nano-particle is mixed in to violent stirring 2h under room temperature; Consumption is 1.5kg/m
3feed liquid), 3 minutes used times, with the speed of 100 revs/min, stir 8 minutes, mixed liquor enters in low intensity magnetic separator and carries out magnetic separation, and feed liquid is qualified feed liquid; Throw out enters connecting material in case of magnetic separator together with magnetic, and by wash agitation groove, rotating speed is 600 revs/min, adjusting pH value is 6, is uniformly mixed 3min, then enters secondary magnetic separated, nano ferriferrous oxide is reclaimed, and recycles, waste liquid individual curing.
In the molten feed liquid of rare earth acid, aluminium content is 2.31g/L, and material liquid aluminium content is after treatment 177mg/L.
The foregoing is only preferred embodiment of the present invention, all equalizations of doing according to the present patent application the scope of the claims change and modify, and all should belong to covering scope of the present invention.
Claims (1)
1. the separated method of removing impurity aluminum in earth solution of neutralization-magnetic flocculation-magnetic, is characterized in that: comprise the following steps: acid is molten, concentrate, neutralize, be uniformly mixed, magnetic flocculation, magnetic are separated;
Concrete steps are as follows: adopt concentrated hydrochloric acid to dissolve rare earth ore concentrate, the earth solution pH value of adjusting after dissolving is 3.5 ~ 4.0, temperature is 40 ~ 90 ℃, then adopt Hhigh-efficient thickener concentrated, solid after concentrated returns to sour molten operation, it is 5.20 ~ 5.30 that concentrated solution first adds NaOH adjustment pH value, feed temperature is adjusted to 15 ~ 35 ℃, adding ammoniacal liquor adjustment pH value is 5.43, in agitation vat, with 400 ~ 800 revs/min of speed, stir, add coagulant aids, 2 ~ 5 minutes used times, with the speed of 80 ~ 200 revs/min, stir, add flocculation agent and modified Nano Z 250 simultaneously, 1 ~ 5 minute used time, with the speed of 80 ~ 200 revs/min, stir 5 ~ 10 minutes, mixed liquor enters and in low intensity magnetic separator, carries out magnetic separation, feed liquid is qualified feed liquid, throw out enters connecting material in case of magnetic separator together with magnetic, and by wash agitation groove, rotating speed is 400 ~ 800 revs/min, adjusting pH value is 5 ~ 8, is uniformly mixed 1 ~ 5min, then enters secondary magnetic separated, nano ferriferrous oxide is reclaimed, and recycles, waste liquid individual curing,
Described coagulant aids is Polyferric Sulfate, and consumption is 0.03 ~ 0.09kg/m
3feed liquid;
Described flocculation agent is cationic polyacrylamide, and cationic degree is 50 ~ 60, and molecular weight is 300 ~ 8,000,000, and consumption is 0.02 ~ 0.06kg/m
3feed liquid;
The preparation process of described modified Nano Z 250: the block polymer of preparing vinylformic acid and polyacrylamide with S-butyl-S '-isopropyl acidic group trithiocarbonate, the pH value of telomerized polymer solution is 5, then itself and ferriferrous oxide nano-particle is mixed in to violent stirring 1.5 ~ 2.5h under room temperature;
The consumption of described modified Nano Z 250 is 0.5 ~ 3kg/m
3feed liquid.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310295016.5A CN103343245B (en) | 2013-07-15 | 2013-07-15 | Method for removing impurity aluminum in rare earth solution by neutralization-magnetic flocculation-magnetic separation |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201310295016.5A CN103343245B (en) | 2013-07-15 | 2013-07-15 | Method for removing impurity aluminum in rare earth solution by neutralization-magnetic flocculation-magnetic separation |
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| CN103343245A CN103343245A (en) | 2013-10-09 |
| CN103343245B true CN103343245B (en) | 2014-05-07 |
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| CN110079672B (en) * | 2019-04-23 | 2021-03-05 | 南昌大学 | Rare earth extraction method based on magnetic control flocculation silica gel |
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| CN101979680B (en) * | 2010-11-17 | 2012-08-15 | 广东富远稀土新材料股份有限公司 | Method for removing aluminum from rare-earth feed liquid |
| CN102328942A (en) * | 2011-08-08 | 2012-01-25 | 山西同华科技有限公司 | Method for preparing sodium aluminate from alumina red mud |
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