CN104229933A - Method for recycling rear earth from rear earth refining industrial wastewater - Google Patents
Method for recycling rear earth from rear earth refining industrial wastewater Download PDFInfo
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- CN104229933A CN104229933A CN201310247058.1A CN201310247058A CN104229933A CN 104229933 A CN104229933 A CN 104229933A CN 201310247058 A CN201310247058 A CN 201310247058A CN 104229933 A CN104229933 A CN 104229933A
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- rare earth
- waste water
- rear earth
- based material
- trade effluent
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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
Abstract
The invention relates to a method for recycling rear earth from rear earth refining industrial wastewater, and belongs to the wet metallurgy field of rear earths. The method is characterized by comprising the following steps: selecting a magnesium-based nano material and recycling rear earth elements from rear earth refining industrial wastewater by virtue of an ion exchange form, wherein the recycling process mainly comprises two stages of pretreatment and displacement precipitation. A recovery rate for rear earth from the wastewater is over 98%, so that trace low-concentration rear earth in the wastewater is sufficiently utilized, and thus, the resource waste is reduced, and precious rear earth resources are recycled to the greatest extent.
Description
Technical field
The present invention relates to a kind of method of refining recovering rare earth trade effluent from rare earth.
Background technology
Rare earth element has the physicalies such as excellent optical, electrical, magnetic, superconduction, catalysis, and type material that can be different, various in style with other materials component property, is referred to as " the industrial monosodium glutamate " in the present age.Rare earth material, in the every field widespread use of national economy and national defense industry, plays an important role in contemporary society's economy and hi-tech numerous areas.But, in recent years along with the further expansion of Rare-earth Industry scale, rare-earth trade is in smelting is separated, and the wastewater flow rate of annual discharge reaches more than 2,000 ten thousand tons, containing a large amount of rare earths in waste water, it is reported, China in recent years rare earth output is 120,000 tons/year, and extraction yield is the highest can only arrive 96 ~ 97%, and the rare earth also namely run off with low dense state with waste water reaches 4000 tons/year, these discharges containing RE waste water cause the loss of valuable rare earth resources on the one hand, also result in environmental pollution on the other hand.
The work of the recovery research of current rare earth is mainly towards used rare-earth products.Such as discard magnetic material for the loss of Rare-Earth Magnetic material in the course of processing or rare earth, many investigators utilize multiple method therefrom to reclaim the rare earths such as Nd, Tb, Dy (M.Itoh, J.Alloys Compd., 2009,477,484-487; T.Saito, Scripta Mater, 2004,51,1069 – 1073.).Mei Guangjun etc. have studied the multiple method (Mei Guangjun, renewable resource research, 2007,6:29-35) extracting Y, Eu rare earth element from luminescent lamp.Because rare earth removal process is very complicated, and have to pass through physics and chemistry process, cause with high costs, up to the present also there is no the rare earth recycling engineering of large-scale application in the middle of magnet material, battery, head light, catalyzer.
Because current China assume responsibility for the production production capacity of global rare earth raw material more than 90%, most Rare Earth Production factories is all in China, and this type of factory of developed country is less, the demand of producing middle-weight rare earths recovery and environmental improvement is little in the demand of developed country, can say, the degree of depth of rare earth metallurgy middle-weight rare earths refine be our national rare-earth industry face have peculiar problem to be solved.So far, some scholars of China are also less for its research carried out.The discharge of rare-earth smelting industry containing RE waste water have the water yield large, containing the low feature of rare earth concentration, conventional adsorbent is as zeolite, clay, flying dust, gac etc., although there is very large loading capacity in some high dense systems, but because it does not possess absorption specificity, therefore and be not suitable for low dense system.
Chinese invention patent application " Rare-earth Mine slag and effluent administers trace rare-earth recovery process " (CN101979335A) adopts lime as precipitation agent, make rare earth ion generate precipitation of hydroxide to be separated with waste water, although the method is simple, but because the water yield is large, need could discharge to neutrality with the anti-pH that adjusts of acid.The efficiency of the method recovering rare earth is undesirable in addition.
The method recovering rare earth that Chinese invention patent application " technique of recovering rare earth from waste water from rare earth mine exploitation by precipitation-extraction " (CN101974690A) adopts calcium hydroxide precipitation and P507 organic extraction to combine, rare earth yield can reach more than 85%, this method extraction agent solution loss is large, cost is high, easy generation secondary pollution, and also to take large-area land resources by settling tank clarification filtration.
Chinese invention patent application " method with recovering rare earth from low-concentration rare earth solution through prussian blue colloidal nanoparticles " (CN102352448A) utilizes Prussian blue colloidal nanoparticles as sorbent material, by dialyzer recovering rare earth, this method rare earth organic efficiency is higher but simultaneously also there is the problem that cost is high, treatment capacity is little.In addition, adopt resin adsorption method also fairly simple, but charge capacity is little, resin cost is high, and rare earth resolves comparatively difficulty.
Summary of the invention
Object of the present invention be exactly, the water yield low for this kind of concentration large containing RE waste water, provide that a kind of technique is simple, rare earth reclaim rare earth abundant, with low cost and refine Rare earth recovery method in trade effluent.
The present invention adopts following technical scheme to realize:
(1) refine a method for recovering rare earth trade effluent from rare earth, it is characterized in that: described method selection mg-based material refines recovering rare earth element trade effluent by ion exchange form from rare earth.
(2) method Gen Ju (1), is characterized in that, described recovering rare earth elementary process comprises pre-treatment and cementation stage.
(3) according to (1) or the method described in (2), it is characterized in that, described mg-based material is selected from magnesium oxychloride, hydromagnesite, causticity magnesite or class brucite stratified material.
(4) according to the method for (3), it is characterized in that, the form of described mg-based material is selected from nanometer materials, and preferred nanometer self-supporting flower-like structure material, more preferably size range is the nano material of 10 ~ 100nm.
(5) method according to any one of (1)-(4), it is characterized in that, described mg-based material is 500mg/g ~ 3g/g to the loading capacity of rare earth, preferred 1g/g-2g/g.
(6) method according to any one of (1)-(5), is characterized in that, described rare earth refines trade effluent and comprises the soap waste water that in rare earth extractive process, saponification rare earth produces, the mother liquor of precipitation of ammonium that precipitating rare earth produces and precipitation wash water.Preferably, the rare earth concentration in described waste water is 0 ~ 500mg/L, and pH value is 0 ~ 7.
(7) method according to any one of (1)-(6), is characterized in that: rare earth refines rare earth element contained in trade effluent and is selected from La, Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm, Sc, Y.
(8) method according to any one of (1)-(7), it is characterized in that, described RE waste water pretreatment stage comprises the steps: to add Wingdale or magnesiumcarbonate in RE waste water, regulates waste water ph to rise to 6 ~ 7.
The object adding these materials utilizes the H in they and waste water
+ionic reaction generates carbonic acid gas and reaches the object regulating wastewater pH, makes the pH value of waste water rise to 6 ~ 7 by regulating.
Adjusting pH by adding calcium hydroxide in prior art, easily making pH too high, final or needs are adjusted with acid is anti-.And the present invention is by adding Wingdale or magnesiumcarbonate adjustment pH, can avoid using the anti-tune of acid.
Consider from cost angle, preferably add Wingdale.Because the acidity in trade effluent is very high, thus use the cost of magnesiumcarbonate can be higher.
Preferably, add Wingdale and wastewater pH is adjusted to neutrality.
(9) according to the method described in any one of (1)-(8), it is characterized in that, the described RE waste water cementation stage comprises the steps: to add mg-based material in the RE waste water regulating pH value.Preferably, also comprise and being uniformly mixed, to make mg-based material fully contact with rare earth ion, while generation ion exchange reaction, displace hydrogen-oxygen rare earth compound.
Causticity magnesite or magnesium oxychloride preferably directly drop in solution and react by the feed postition of described mg-based material.Also preferred hydromagnesite or class brucite stratified material are first calcined 1-2 hours under 500-600 degree after, then drop in solution and react.
(10) according to the method for (9), after cementation 10-30 minute, obtain clarified supernatant and rare earth compound by centrifugation, the rare earth element that final rare earth refines in trade effluent is recycled in the mode forming rare earth compound.
Detect supernatant liquor, the rare earth yield after reaction in solution is up to more than 90%.
The Method And Principle of recovering rare earth from rare earth refinement waste water provided by the invention is as follows:
Containing certain density rare earth ion (Re in original RE waste water
3+), following reaction can be there is when contacting with rare earth ion in the magnesium-base nano material (for causticity magnesite) that the present invention adopts:
2Re
3++3Mg(OH)
2→2Re(OH)
3+3Mg
2+ （1）
Due to the solubility product constant (Ksp=10 of hydrogen-oxygen rare earth compound
-20 ~-35) much smaller than magnesium hydroxide (Ksp=1.8 × 10
-11), therefore when both contact, rare earth ion can carry out cationic exchange with magnesium ion, and the magnesium while producing hydrogen-oxygen rare earth compound in magnesium hydroxide enters into solution in the form of an ion, and the stability constant due to this reaction is comparatively large, and (K is surely=10
7 ~ 27), reaction therefore can be made to carry out thoroughly, finally generate hydrogen-oxygen rare earth compound completely.
The present invention adopts mg-based material to refine the method for recovering rare earth trade effluent from rare earth, the micro-low concentration of rare earth in waste water can be made to be fully recycled in the mode forming rare earth compound, the present invention to the rare earth yield in waste water up to more than 90%, rare earth yield in preferred waste water can reach more than 98%, present method has the features such as technique is simple, with low cost, the material non-secondary pollution of use simultaneously, has higher Social benefit and economic benefit.
Embodiment
The present invention is described in detail to invention by following embodiment, but it will be appreciated by those skilled in the art that following embodiment is not for limiting the scope of the invention.Any improvement made on basis of the present invention, change is all within protection scope of the present invention.
Embodiment 1
Get the rare-earth precipitation mother liquor waste water 500ml(Dy concentration 10mg/L of actual factory), add Wingdale, fully stir, adjust ph to 6.0.In the RE waste water regulating pH value, add the hydromagnesite 10mg after heat modification, continuously stirring 10 minutes, after high speed centrifugation is separated 5 minutes, take out supernatant liquor, the Dy concentration in test supernatant liquor.
Dy concentration after reaction in supernatant liquor is 0.16mg/L, and rare earth yield reaches 98.4%.
Embodiment 2
Get the rare-earth precipitation mother liquor waste water 500ml(Dy concentration 10mg/L of actual factory), add Wingdale, fully stir, adjust ph to 6.5.In the RE waste water regulating pH value, add the hydromagnesite 20mg after heat modification, continuously stirring 30 minutes, after high speed centrifugation is separated 5 minutes, take out supernatant liquor, the Dy concentration in test supernatant liquor.
Dy concentration after reaction in supernatant liquor is 0.05mg/L, and rare earth yield reaches 99.5%.
Embodiment 3
Get the rare-earth precipitation mother liquor waste water 500ml(Ho concentration 10mg/L of actual factory), add Wingdale, fully stir, adjust ph to 7.In the RE waste water regulating pH value, add causticity magnesite 20mg, continuously stirring 10 minutes, after high speed centrifugation is separated 5 minutes, take out supernatant liquor, the Ho concentration in test supernatant liquor.
Ho concentration after reaction in supernatant liquor is 0.10mg/L, and rare earth yield reaches 99.0%.
Embodiment 4
Get the rare-earth precipitation mother liquor waste water 500ml(Ho concentration 30mg/L of actual factory), add Wingdale, fully stir, adjust ph to 6.5.In the RE waste water regulating pH value, add causticity magnesite 40mg, continuously stirring 30 minutes, after high speed centrifugation is separated 5 minutes, take out supernatant liquor, the Ho concentration in test supernatant liquor.
Ho concentration after reaction in supernatant liquor is 0.12mg/L, and rare earth yield reaches 99.6%.
Embodiment 5
Get the rare-earth precipitation mother liquor waste water 500ml(La concentration 50mg/L of actual factory), add magnesiumcarbonate, fully stir, adjust ph to 6.0.In the RE waste water regulating pH value, add causticity magnesite 50mg, continuously stirring 30 minutes, after high speed centrifugation is separated 5 minutes, take out supernatant liquor, the La concentration in test supernatant liquor.
La concentration after reaction in supernatant liquor is 0.25mg/L, and rare earth yield reaches 99.5%.
Embodiment 6
Get the rare-earth precipitation mother liquor waste water 500ml(Eu concentration 10mg/L of actual factory), add magnesiumcarbonate, fully stir, adjust ph to 6.5.In the RE waste water regulating pH value, add magnesium oxychloride 20mg, continuously stirring 20 minutes, after high speed centrifugation is separated 5 minutes, take out supernatant liquor, the Eu concentration in test supernatant liquor.
Eu concentration after reaction in supernatant liquor is 0.04mg/L, and rare earth yield reaches 99.6%.
Embodiment 7
Get the rare-earth precipitation mother liquor waste water 500ml(Y concentration 14mg/L of actual factory), add magnesiumcarbonate, fully stir, adjust ph to 7.0.In the RE waste water regulating pH value, add the class brucite stratified material 30mg after heat modification, continuously stirring 20 minutes, after high speed centrifugation is separated 5 minutes, take out supernatant liquor, the Eu concentration in test supernatant liquor.
Y concentration after reaction in supernatant liquor is 0.03mg/L, and rare earth yield reaches 99.2%.
Claims (10)
1. refine a method for recovering rare earth trade effluent from rare earth, it is characterized in that: described method selection mg-based material refines recovering rare earth element trade effluent by ion exchange form from rare earth.
2. method according to claim 1, is characterized in that, described recovering rare earth elementary process comprises pre-treatment and cementation stage.
3. method according to claim 1 and 2, is characterized in that, it is magnesium oxychloride, hydromagnesite, causticity magnesite or class brucite stratified material that described mg-based material is selected from.Described mg-based material is selected from nanometer materials, and preferred nanometer self-supporting flower-like structure material, more preferably size range is the nano material of 10 ~ 100nm.
4. the method according to any one of claim 1-3, is characterized in that, described mg-based material is 500mg/g ~ 3g/g to the loading capacity of rare earth, preferred 1g/g-2g/g.
5. the method according to any one of claim 1-4, is characterized in that, described trade effluent comprises: the soap waste water that in rare earth extractive process, saponification rare earth produces, the mother liquor of precipitation of ammonium that precipitating rare earth produces and precipitation wash water.Preferably, the rare earth concentration in described waste water is 0 ~ 500mg/L, and pH value is 0 ~ 7.
6. the method according to any one of claim 1-5, is characterized in that: rare earth refines rare earth element contained in trade effluent and is selected from La, Ce, Pr, Nd, Sm, Eu, Tb, Dy, Ho, Er, Tm, Sc, Y.
7. the method according to any one of claim 1-6, is characterized in that, described RE waste water pretreatment stage comprises the steps: to add Wingdale or magnesiumcarbonate in RE waste water, and adjust ph rises to 6 ~ 7.
8. the method according to any one of claim 1-7, is characterized in that, the described RE waste water cementation stage comprises the steps: that in the RE waste water regulating pH value, add mg-based material carries out replacement(metathesis)reaction.Preferably, also comprise and be uniformly mixed step.
9. method according to claim 8, is characterized in that, causticity magnesite or magnesium oxychloride preferably directly drop in solution and react by the feed postition of described mg-based material.Also preferred hydromagnesite or class brucite stratified material are first calcined 1-2 hours under 500-600 degree after, then drop in solution and react.
10. the method for according to Claim 8 or 9, it is characterized in that, after cementation 10-30 minute, obtain clarified supernatant and rare earth compound by centrifugation, the rare earth element that final rare earth refines in trade effluent is recycled in the mode forming rare earth compound.
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Cited By (3)
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| CN110331291A (en) * | 2019-07-19 | 2019-10-15 | 中国科学院福建物质结构研究所 | A method of separation and/or extraction lanthanide series |
| CN113215410A (en) * | 2021-05-31 | 2021-08-06 | 江苏南方永磁科技有限公司 | Method for recovering holmium from soap waste liquid |
| CN117165790A (en) * | 2023-09-04 | 2023-12-05 | 华南理工大学 | TiO (titanium dioxide) 2 P/C electrode material and preparation method and application thereof |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN110331291A (en) * | 2019-07-19 | 2019-10-15 | 中国科学院福建物质结构研究所 | A method of separation and/or extraction lanthanide series |
| CN113215410A (en) * | 2021-05-31 | 2021-08-06 | 江苏南方永磁科技有限公司 | Method for recovering holmium from soap waste liquid |
| CN113215410B (en) * | 2021-05-31 | 2022-04-01 | 江苏南方永磁科技有限公司 | Method for recovering holmium from soap waste liquid |
| CN117165790A (en) * | 2023-09-04 | 2023-12-05 | 华南理工大学 | TiO (titanium dioxide) 2 P/C electrode material and preparation method and application thereof |
| CN117165790B (en) * | 2023-09-04 | 2024-03-08 | 华南理工大学 | TiO (titanium dioxide) 2 P/C electrode material and preparation method and application thereof |
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