CN105087964B - It is a kind of to remove lead from rare earth extraction saponification waste-water while the technique of recovering rare earth - Google Patents
It is a kind of to remove lead from rare earth extraction saponification waste-water while the technique of recovering rare earth Download PDFInfo
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- CN105087964B CN105087964B CN201410196597.1A CN201410196597A CN105087964B CN 105087964 B CN105087964 B CN 105087964B CN 201410196597 A CN201410196597 A CN 201410196597A CN 105087964 B CN105087964 B CN 105087964B
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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
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Abstract
The invention discloses a kind of remove lead while the technique of recovering rare earth, comprises the steps from rare earth extraction saponification waste-water：a）Rare earth extraction saponification waste-water is carried out into oil removing via oil interceptor；b）NaOH solution is added, pH to 10.5 ~ 13 is adjusted, solid-liquid separation obtains leaded supernatant and rare-earth precipitation slag；c）To precipitation slag or filter press is carried out, obtain pressing filtering liquid and filter-press residues；Or directly processed and obtain re chloride, into extraction process rare-earth separating with hydrochloric acid or the acidic leach of extractant；d）By supernatant and/or pressing filtering liquid, Na is added3PO4Solution, obtains the supernatant of lead phosphate precipitate and total Pb≤0.2mg/L；e）Precipitate filter pressing is stacked, transfers to dangerous solid waste qualification to dispose processed in units；Supernatant is acidified, plus lime cream is processed and removes excessive PO4 3‑After discharge；Total Pb≤the 0.2mg/L of rare earth extraction saponification waste-water after process, meets《Rare-earth trade pollutant emission standard》Require, and effectively realize the recycling of waste water middle rare earth.
Description
Technical field
The present invention relates to a kind of substep from rare earth extraction saponification waste-water is deep to remove lead while the technique of recovering rare earth.
Background technology
Rare Earth Mine contains the elements such as micro lead, arsenic, aluminum, uranium, thorium, and the process for smelting rare-earth separating is extracted in acid system
In, using extractants such as P507, P204 and aphthenic acids（Organic faciess）Jing alkaline matters（The alkali compoundss such as sodium, calcium, magnesium, ammonia）It is fixed
After amount saponification, then mix and carry out rare-earth sodium saponification for 1 ~ 4 acid earth solution with pH（Extractant supported rare earth ion）, it is quantitative to extract
Rare earth element is taken, the rare earth extraction saponification waste-water of the heavy metal ion being extracted containing trace rare-earth ion and hardly possible is produced（pH=
3.5~5）, after the wastewater collection, use alkaline matter（Lime cream, magnesium oxide, sodium hydroxide, sodium carbonate etc.）Process, neutralize PH to 6
Clarify after ~ 9, supernatant discharge after solid-liquid separation.
Typically contain 10 ~ 800 mg/litre of rare earth in the detached rare earth soap waste water of rare earth extraction, 2 ~ 100 mg/litre of lead,
The elements such as arsenic, nickel, cadmium are micro, and conventional processes are alkaline matter（Conventional industrial soda or lime cream etc.）Neutralization precipitation method.Plus
Enter alkaline matter（OH-）Afterwards, in the waste water rare earth and heavy metal element generates insoluble metal compound, can remove after sedimentation.
But there is difference as different metal element starts the pH for generating and precipitating completely, meeting Sewage Water Emissions limit value pH=6 ~ 9
Under conditions of, part heavy metal element can not precipitate removal completely, can not particularly meet rare-earth industry pollutant emission standard
（GB2645-2011 tables 2）, there is the hidden danger of not qualified discharge in the requirement of total Pb≤0.2 mg/litre.Meanwhile, the weight such as rare earth and lead
The precipitate that metal is generated（Inorganic sludge）After solid-liquid separation filter pressing, the hydroxide containing rare earth and heavy metal for obtaining
It is dissolved in acid, it is impossible to directly recycle the rare earth in waste water, waste rare earth resources, reduce the rare earth yield of production process.
PO4 is used3-Or S2-Removal rare earth and lead element, but RE phosphate and sulfide can be processed insoluble in acid Deng material,
Can not be directly from rare earth extraction saponification waste-water by the method separating beavy metal and recycling rare earth of resolution of precipitate.
The content of the invention
It is contemplated that being alkaline insoluble matters by using rare earth hydrate, Lead oxide hydrate is amphoteric compound and phosphoric acid
Characteristic of the lead insoluble in bronsted lowry acids and bases bronsted lowry, there is provided a kind of to remove lead from rare earth extraction saponification waste-water while the technique of recovering rare earth.Place
Total Pb≤the 0.2mg/L of rare earth extraction saponification waste-water after reason, meets《Rare-earth industry pollutant emission standard》Requirement, and can be straight
Connect the recycling for being effectively realized rare earth extraction saponification waste-water middle rare earth.
It is a kind of to remove lead from rare earth extraction saponification waste-water while the technique of recovering rare earth, comprises the steps：
a）Rare earth extraction saponification waste-water is carried out into clarification oil removing via oil interceptor, obtains removing organic oiliness things such as extractant
The rare earth extraction saponification waste-water of matter；
b）The NaOH solution of 1 ~ 10mol/L is added, pH is adjusted to 8 ~ 10, obtain rare earth hydrate precipitation and Lead oxide hydrate sinks
Forming sediment, continuously adding the NaOH solution of 1 ~ 10mol/L, pH value is adjusted to 10.5 ~ 13, Lead oxide hydrate precipitation all dissolves, and obtains molten
The lead ion of solution；Add wadding, coagulant to carry out solid-liquid separation, obtain the supernatant containing lead ion and sinking containing rare earth hydrate
Mud；
c）For the precipitation slag containing rare earth hydrate is carried out after sedimentation concentration, or filter press process is carried out, solid-liquid point
From obtaining the pressing filtering liquid containing lead ion and the filter-press residues containing rare earth hydrate precipitate, filter-press residues dissolving with hydrochloric acid obtained
To re chloride, rare earth is separated and recovered into extraction process；Or do not carry out filter press process, directly use dissolving with hydrochloric acid or
Extractant saponification is dissolved, and obtains re chloride or extraction organic faciess supported rare earth, separates and recovers rare earth into extraction process；
d）By the supernatant containing dissolved state lead ion and step c）Process what the precipitation slag containing rare earth hydrate was obtained
Recovered liquid, adds the Na of 10 ~ 100g/L under agitation3PO4Solution, until not producing white precipitate for terminal, solid-liquid point
From obtaining the supernatant of the precipitate containing lead phosphate and total Pb≤0.2mg/L；
e）Precipitate filter pressing containing Lead oxide hydrate is stacked, transfers to dangerous solid waste to dispose processed in units；By total Pb≤
The supernatant collection of 0.2mg/L, Jing after the acidifying of composite wastewater treating stations, plus lime cream is processed and removes excessive PO4 3-After discharge.
Wherein, the pH of the rare earth extraction saponification waste-water is 3.5 ~ 5.0, and content of rare earth is 10 ~ 800mg/L, and Pb contents are 2
~100mg/L。
Preferably, the flocculant is 5g/L polyacrylamide solutions, and coagulant is polyaluminium chloride 50g/L aqueous solutions.
Preferably, the concentration >=2mol/L of the hydrochloric acid.
Preferably, the extractant is P204 or P507, the concentration >=0.8mol/L of extractant.
Saponification dissolve when, saponifier used be reclaim rare earth hydrate condensed slag, content of rare earth（TREO total rare earth (TRE)s）
For≤20%.
Step d）Add Na3PO4The lead phosphate insoluble in bronsted lowry acids and bases bronsted lowry is generated, lead ion is removed；Supernatant and pressing filtering liquid
Lime cream is added to remove excessive PO after acidifying4 3-。
It is contemplated that being alkaline insoluble compound by using rare earth hydrate, Lead oxide hydrate is amphoteric compound and phosphorus
Characteristic of the lead plumbate insoluble in bronsted lowry acids and bases bronsted lowry, there is provided a kind of to remove lead from rare earth extraction saponification waste-water while the technique of recovering rare earth.
When rare earth extraction saponification waste-water to be added under conditions of stirring the NaOH solution of 1 ~ 10mol/L, when adjusting pH to 7.5 ~ 10,
Obtain Lead oxide hydrate and rare earth hydrate precipitation；The NaOH solution of 1 ~ 10mol/L is continuously added, when adjusting pH >=10, hydroxide
Lead precipitation starts dissolving, and it is 10.5 ~ 13 to continue to adjust pH value, and Lead oxide hydrate precipitation all dissolves under agitation, and hydrogen-oxygen
Change rare earth then not dissolving, add flocculant to carry out solid-liquid separation, the lead ion supernatant containing dissolved state can be obtained and contained
There is the precipitation slag of rare earth hydrate precipitate；Then respectively by the supernatant containing dissolved state lead ion and containing hydroxide it is dilute
The precipitation slag of native precipitate carries out phosphate radical respectively except lead and recovering rare earth are processed.
The technique that the present invention is adopted can effectively remove the heavy metal Pb in rare-earth sodium saponification waste water so that the rare earth after process
Total Pb≤0.2mg/L of extraction saponification waste-water, meets《Rare-earth industry pollutant emission standard》（GB26451-2011）Environmental protection
Limit value emission request, so as to improve environmental pollution improvement's level of Rare Earth Enterprises, while being directly effectively realized rare earth extraction
The recovery of saponification waste-water middle rare earth, improves total rare earth recovery rate 0.5-1.0% of production process, and comprehensive utilization of resources is profitable.
Description of the drawings
Fig. 1 is that lead is removed from rare earth extraction saponification waste-water while the process chart of recovering rare earth.
Specific embodiment
Embodiment 1
It is a kind of to remove lead from rare earth extraction saponification waste-water while the technique of recovering rare earth, comprises the steps：By pH=
3.5th, content of rare earth is that 459mg/L, Pb content carries out clarification oil removing via oil interceptor for the rare earth extraction saponification waste-water of 38mg/L,
Obtain removing the rare earth extraction saponification waste-water of organic oily matters such as extractant；Add the NaOH of 5mol/L molten under stirring
Liquid, adjusts pH value to 9, obtains rare earth hydrate precipitation and Lead oxide hydrate precipitation, continuously adds the NaOH solution of 5mol/L, due to
Lead oxide hydrate is deposited in after base excess is added and will dissolve again, adjusts pH value to 12, and Lead oxide hydrate precipitation all dissolves, and is dissolved
Lead ion；Polyaluminium chloride solution 50ppm of 50g/L is added, the polyacrylamide 5ppm of 5g/L is subsequently added into, stirring is mixed
After solidifying and flocculation, Jing tube settlers pond carries out solid-liquid separation process, obtains the supernatant containing dissolved state lead ion and contains
The precipitation slag of rare earth hydrate precipitate.Wherein rare earth hydrate precipitate is discharged from tube settler bottom of pond, Jing sludge thickening ponds
Extraction process is directly entered after concentration, using the acid Directly saponification dissolving of the P507 extractants of 1.5mol/L, rare earth is saponified
Extraction is separated into organic faciess；Tube settler pond is contained within into the supernatant of dissolved state lead ion, under agitation
Add the Na of 100g/L3PO4Solution, until not producing white precipitate for terminal, solid-liquid separation can obtain heavy containing lead phosphate
The supernatant of starch and total Pb≤0.2mg/L；Precipitate filter pressing containing lead phosphate is stacked, hands over dangerous solid waste to dispose unit
Process；By the supernatant collection acidification of total Pb≤0.2mg/L, Jing composite wastewaters treating stations add lime cream to remove excess
PO4 3-Discharge after ion.Waste water Jing monitorings after process, total Pb≤0.2mg/L meet《Rare-earth industry pollutant emission standard》
Emission limit require.According to production measuring and calculating, 7 tons of mixed rare-earth oxides are processed daily, about 100 tons of rare-earth sodium saponification waste water is produced,
459 mg/litre of waste water middle rare earth concentration, 45.9 kilograms of recyclable rare earth after process improve rare earth total recovery 0.66%.
Embodiment 2
It is a kind of to remove lead from rare earth extraction saponification waste-water while the technique of recovering rare earth, comprises the steps：By pH=
4.0, content of rare earth is 500mg/L, and Pb contents are that the rare earth extraction saponification waste-water of 56mg/L carries out clarification oil removing via oil interceptor,
Obtain removing the rare earth extraction saponification waste-water of organic oily matters such as extractant；Add the NaOH of 5mol/L molten under stirring
Liquid, adjusts pH value to 9, obtains rare earth hydrate precipitation and Lead oxide hydrate precipitation, continuously adds the NaOH solution of 5mol/L, due to
Lead oxide hydrate is deposited in after base excess is added and will dissolve again, adjusts pH value to 12, and Lead oxide hydrate precipitation all dissolves, and is dissolved
Lead ion；Polyaluminium chloride solution 50ppm of 50g/L is added, the polyacrylamide 5ppm of 5g/L is subsequently added into, stirring is mixed
After solidifying and flocculation, Jing tube settlers pond carries out solid-liquid separation process, obtains the supernatant containing dissolved state lead ion and contains
The precipitation slag of rare earth hydrate precipitate.Wherein rare earth hydrate precipitate is discharged from tube settler bottom of pond, after thickening pond concentration,
Carry out filter press process, solid-liquid separation obtains the pressing filtering liquid containing dissolved state lead ion and rare earth hydrate precipitate
Filter-press residues；By the filter-press residues dissolving with hydrochloric acid of rare earth hydrate, re chloride is obtained, separated and recovered into extraction process dilute
Soil；Tube settler pond is contained within into the filter pressing clear liquid that the supernatant of dissolved state lead ion and filter pressing are reclaimed, in stirring condition
The Na of lower addition 100g/L3PO4Solution, until not producing white precipitate for terminal, solid-liquid separation obtains heavy containing lead phosphate
The supernatant of starch and total Pb≤0.2mg/L；Precipitate filter pressing containing lead phosphate is stacked, hands over dangerous solid waste to dispose unit
Process；By the supernatant collection acidification of total Pb≤0.2mg/L, Jing composite wastewaters treating stations add lime cream to remove excess
PO4 3-Discharge after ion.Waste water Jing monitorings after process, total Pb≤0.2mg/L meet《Rare-earth industry pollutant emission standard》
Emission limit require.According to production measuring and calculating, 7 tons of mixed rare-earth oxides are processed daily, about 100 tons of rare-earth sodium saponification waste water is produced,
500 mg/litre of waste water middle rare earth concentration, 50 kilograms of recyclable rare earth after process improve rare earth total recovery 0.71%.
Claims (4)
1. it is a kind of to remove lead from rare earth extraction saponification waste-water while the technique of recovering rare earth, comprises the steps：
a）Rare earth extraction saponification waste-water is carried out into clarification oil removing via oil interceptor, obtains removing the dilute of the organic oily matter of extractant
Native extraction saponification waste-water；
b）The NaOH solution of 1 ~ 10mol/L is added, pH is adjusted to 8 ~ 10, obtain rare earth hydrate precipitation and Lead oxide hydrate precipitation,
The NaOH solution of 1 ~ 10mol/L being continuously added, pH value being adjusted to 10.5 ~ 13, Lead oxide hydrate precipitation all dissolves, and obtains what is dissolved
Lead ion；Add wadding, coagulant to carry out solid-liquid separation, obtain the supernatant containing lead ion and the precipitation containing rare earth hydrate
Slag；
c）For the precipitation slag containing rare earth hydrate is carried out after sedimentation concentration, or filter press process is carried out, solid-liquid separation is obtained
Pressing filtering liquid containing lead ion and the filter-press residues containing rare earth hydrate precipitate, by filter-press residues dissolving with hydrochloric acid, obtain chlorination
Earth solution, separates and recovers rare earth into extraction process；Or filter press process is not carried out, directly use dissolving with hydrochloric acid or extractant
Saponification is dissolved, and obtains re chloride or extraction organic faciess supported rare earth, separates and recovers rare earth into extraction process；
d）By the supernatant containing dissolved state lead ion and step c）Process the recovery that the precipitation slag containing rare earth hydrate is obtained
Liquid, adds the Na of 10 ~ 100g/L under agitation3PO4Solution, until not producing white precipitate for terminal, solid-liquid separation is obtained
To the precipitate containing lead phosphate and the supernatant of total Pb≤0.2mg/L；
e）Precipitate filter pressing containing lead phosphate is stacked, transfers to dangerous solid waste to dispose processed in units；By total Pb≤0.2mg/L
Supernatant collection, Jing after the acidifying of composite wastewater treating stations, plus lime cream is processed and removes unnecessary PO4 3-After discharge.
2. it is according to claim 1 to remove lead from rare earth extraction saponification waste-water while the technique of recovering rare earth, its feature
It is that the pH of the rare earth extraction saponification waste-water is 3.5 ~ 5.0, content of rare earth is 10 ~ 800mg/L, and Pb contents are 2 ~ 100mg/
L。
3. it is according to claim 1 to remove lead from rare earth extraction saponification waste-water while the technique of recovering rare earth, its feature
It is, step b）The flocculant is 5g/L polyacrylamide solutions, and coagulant is polyaluminium chloride 50g/L aqueous solutions.
4. it is according to claim 1 to remove lead from rare earth extraction saponification waste-water while the technique of recovering rare earth, its feature
It is, step c）Concentration >=the 2mol/L of the hydrochloric acid, the extractant be P204 or P507, concentration >=0.8mol/L.
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| CN108130434A (en) * | 2017-11-29 | 2018-06-08 | 中铝广西国盛稀土开发有限公司 | A kind of wastewater application using Rare Earth Separation is in the process of rare earth in_situ leaching |
| CN109097566A (en) * | 2018-09-17 | 2018-12-28 | 江西理工大学 | A method of the recovering rare earth from weathered superficial leaching rare-earth ore |
| CN109554557A (en) * | 2018-12-28 | 2019-04-02 | 临沂大学 | A kind of method of rare earth element in recycling oily waste water |
| CN112620334B (en) * | 2020-11-30 | 2022-09-30 | 衡阳师范学院 | Method for recovering heavy metal from contaminated soil |
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| CN113403489B (en) * | 2021-06-17 | 2023-01-24 | 吉安鑫泰科技有限公司 | Calcium saponification organic phase clarification extraction process and equipment thereof |
| CN113667842B (en) * | 2021-07-14 | 2022-09-20 | 四川省冕宁县方兴稀土有限公司 | Method for removing non-rare earth impurities in rare earth hydrometallurgy |
| CN114990340A (en) * | 2022-06-10 | 2022-09-02 | 贵州大学 | Method for separating and recovering rare earth elements from acid mine wastewater |
| CN114950005A (en) * | 2022-06-29 | 2022-08-30 | 格林爱科(荆门)新能源材料有限公司 | Recovery system and recovery method for ternary positive electrode precursor production regeneration waste liquid |
| CN116282118A (en) * | 2022-12-28 | 2023-06-23 | 广西国盛稀土新材料有限公司 | Method for producing industrial calcium chloride by utilizing rare earth smelting high-salt wastewater |
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| CN103436720B (en) * | 2013-09-18 | 2015-03-25 | 许瑞高 | Process for leaching rare earth from ion-adsorption type rare earth ore without using ammonium salt |
| CN103572064B (en) * | 2013-11-19 | 2015-03-11 | 乐山盛和稀土股份有限公司 | Method for enriching lead and recovering rare earth from rare earth lead slag |
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