CN105219962A - A kind of method of recovering rare earth element from carbonic acid precipitating rare earth mother liquor - Google Patents
A kind of method of recovering rare earth element from carbonic acid precipitating rare earth mother liquor Download PDFInfo
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- CN105219962A CN105219962A CN201510636271.0A CN201510636271A CN105219962A CN 105219962 A CN105219962 A CN 105219962A CN 201510636271 A CN201510636271 A CN 201510636271A CN 105219962 A CN105219962 A CN 105219962A
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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 present invention relates to a kind of method of recovering rare earth element from carbonic acid precipitating rare earth mother liquor, the method comprises the steps such as inspection, siphon, feed supplement, solid-liquid separation and dehydration, and the throw out after dehydration is recovering rare earth element.The present invention can carry out high efficiente callback to the rare earth element in carbonic acid precipitating rare earth mother liquor, avoids the waste of resource, carries out pre-treatment to oxalic acid precipitation rare earth mother solution, alleviate waste water treatment cost, and simple to operate, with low cost, there is good economic benefit and social benefit.
Description
Technical field
The invention belongs to technical field of rare-earth hydrometallurgy, be specifically related to a kind of method of recovering rare earth element from carbonic acid precipitating rare earth mother liquor.
Background technology
The current processing mode to single rare earth feed liquid mainly adds oxalic acid or sodium carbonate, forms oxalic acid precipitation rare earth (the heavy rare earth of grass) or carbonic acid precipitating rare earth (carbon sink rare earth).Grass sink rare earth process in need to add excessive oxalic acid (expecting than 1.1-1.7), in carbon sinks rare earth process, eventually control pH value is slant acidity (5.8-7.0).Therefore precipitate in waste water main containing excessive oxalic acid, certain density hydrochloric acid and the Rare Earth Elements Determination that do not precipitate completely, direct siphon is drained mother liquor waste water, can cause waste to national scarce resource.For the sedimentary dewatering type of single rare earth, general employing centrifuge dripping and these two kinds of modes of vacuum filtration at present.When there is filter cloth breakage or artificial reinforced error, employee does not have Timeliness coverage that rare-earth precipitation thing can be caused directly to drain with jean-washing wastewater, causes the great wasting of resources.In early days for running the process of leaking rare-earth precipitation thing in mother liquor of precipitation of ammonium, jean-washing wastewater, mainly taking to concentrate the mode entering wastewater collection pond, carrying out natural subsidence separation, when sediment is accumulated to a certain degree, manually draw slag, waste time and energy.The heavy rare earth of grass and carbon sink rare earth and mix, the intractability of increasing slag charge.
Summary of the invention
The object of the invention is to overcome the deficiencies in the prior art, a kind of method of recovering rare earth element from carbonic acid precipitating rare earth mother liquor is provided.
The present invention realizes in the following way:
A method for recovering rare earth element from carbonic acid precipitating rare earth mother liquor, comprises the following steps:
(1) detect: the carbonate concentration of carbonic acid precipitating rare earth mother liquor and rare earth ion concentration are detected;
(2) siphon: the siphon of carbonic acid precipitating rare earth mother liquor is entered ground water leg;
(3) feed supplement: according to the detected result of step (1), as carbonic acid >0.5mol/L in carbonic acid precipitating rare earth mother liquor, in carbonic acid precipitating rare earth mother liquor, add rare earth feed liquid, reduce carbonate concentration, make carbonate concentration remain 0.05-0.5mol/L; As carbonic acid precipitating rare earth mother liquor Rare Earth Ion >0.005mol/L, in carbonic acid precipitating rare earth mother liquor, drip sodium carbonate solution, make carbonate concentration remain 0.05-0.5mol/L, precipitating rare earth ion;
(4) solid-liquid separation: step (3) gained feed liquid naturally left standstill, supernatant liquor is discharged to carbonic acid precipitating rare earth wastewater collection pond, reclaims precipitation;
(5) dewater: be deposited in dewatering unit by step (4) gained and dewater, waste water is discharged to carbonic acid precipitating rare earth wastewater collection pond, and the throw out after dehydration is recovering rare earth element.
Preferably, in step (3), when adding sodium carbonate solution, the concentration of described sodium carbonate solution is 120-200g/L;
Preferably, the described time naturally left standstill is 15-20min.
Preferably, described dewatering unit comprises whizzer, suction filtration tank, ground water leg and wash water pipeline, and the wash water water outlet of described whizzer and described suction filtration tank, higher than described ground water leg entrance, utilizes water gravity to realize gravity flow, reduces energy consumption.
Preferably, the washing water outlet of described whizzer and described suction filtration tank arranges the opening of 45 ° downwards, to overflow the recovery of material.
Preferably, the washing water outlet bottom of described whizzer and described suction filtration tank arranges depression filter cloth, is convenient to the dirty of water.
Preferably, described depression filter cloth is for collecting the throw out after described dehydration.
The invention has the beneficial effects as follows:
1. the present invention can carry out high efficiente callback to the rare earth element in carbonic acid precipitating rare earth mother liquor, avoids the waste of resource.
2. the present invention can carry out pre-treatment to carbonic acid precipitating rare earth mother liquor, alleviates waste water treatment cost.
3. the present invention can prevent from causing rare-earth precipitation thing to drain with wash water when there is filter cloth breakage or artificial reinforced error in dehydration.
4. invention increases the availability of rare earth resources, and simple to operate, with low cost, there is good economic benefit and social benefit.
Embodiment
Below in conjunction with specific embodiment, the invention will be further described, but do not limit the scope of the invention and range of application.
embodiment 1
A method for recovering rare earth element from carbonic acid precipitating rare earth mother liquor, comprises the following steps:
(1) detect: the carbonate concentration of carbonic acid precipitating rare earth mother liquor and rare earth ion concentration are detected;
(2) siphon: the siphon of carbonic acid precipitating rare earth mother liquor is entered ground water leg;
(3) feed supplement: according to the detected result of step (1), as carbonic acid >0.5mol/L in carbonic acid precipitating rare earth mother liquor, in carbonic acid precipitating rare earth mother liquor, add rare earth feed liquid, reduce carbonate concentration, carbonate concentration is made to remain 0.05mol/L, precipitating rare earth ion;
(4) solid-liquid separation: step (3) gained feed liquid is left standstill 15min naturally, and supernatant liquor is discharged to carbonic acid precipitating rare earth wastewater collection pond, reclaims precipitation;
(5) dewater: be deposited in dewatering unit by step (4) gained and dewater, waste water is discharged to carbonic acid precipitating rare earth wastewater collection pond, and the throw out after dehydration is recovering rare earth element.
Wherein, described dewatering unit comprises whizzer, suction filtration tank, ground water leg and wash water pipeline, the wash water water outlet of described whizzer and described suction filtration tank is higher than described ground water leg entrance, the washing water outlet of described whizzer and described suction filtration tank arranges the opening of 45 ° downwards, the washing water outlet bottom of described whizzer and described suction filtration tank arranges depression filter cloth, and described depression filter cloth is for collecting the throw out after described dehydration.
embodiment 2
(1) detect: the carbonate concentration of carbonic acid precipitating rare earth mother liquor and rare earth ion concentration are detected;
(2) siphon: the siphon of carbonic acid precipitating rare earth mother liquor is entered ground water leg;
(3) feed supplement: according to the detected result of step (1), as carbonic acid >0.5mol/L in carbonic acid precipitating rare earth mother liquor, in carbonic acid precipitating rare earth mother liquor, add rare earth feed liquid, reduce carbonate concentration, carbonate concentration is made to remain 0.5mol/L, precipitating rare earth ion;
(4) solid-liquid separation: step (3) gained feed liquid is left standstill 20min naturally, and supernatant liquor is discharged to carbonic acid precipitating rare earth wastewater collection pond, reclaims precipitation;
(5) dewater: be deposited in dewatering unit by step (4) gained and dewater, waste water is discharged to carbonic acid precipitating rare earth wastewater collection pond, and the throw out after dehydration is recovering rare earth element.
Wherein, described dewatering unit comprises whizzer, suction filtration tank, ground water leg and wash water pipeline, the wash water water outlet of described whizzer and described suction filtration tank is higher than described ground water leg entrance, the washing water outlet of described whizzer and described suction filtration tank arranges the opening of 45 ° downwards, the washing water outlet bottom of described whizzer and described suction filtration tank arranges depression filter cloth, and described depression filter cloth is for collecting the throw out after described dehydration.
embodiment 3
(1) detect: the carbonate concentration of carbonic acid precipitating rare earth mother liquor and rare earth ion concentration are detected;
(2) siphon: the siphon of carbonic acid precipitating rare earth mother liquor is entered ground water leg;
(3) feed supplement: according to the detected result of step (1), as carbonic acid >0.5mol/L in carbonic acid precipitating rare earth mother liquor, in carbonic acid precipitating rare earth mother liquor, add rare earth feed liquid, reduce carbonate concentration, carbonate concentration is made to remain 0.2mol/L, precipitating rare earth ion;
(4) solid-liquid separation: step (3) gained feed liquid is left standstill 18min naturally, and supernatant liquor is discharged to carbonic acid precipitating rare earth wastewater collection pond, reclaims precipitation;
(5) dewater: be deposited in dewatering unit by step (4) gained and dewater, waste water is discharged to carbonic acid precipitating rare earth wastewater collection pond, and the throw out after dehydration is recovering rare earth element.
Wherein, described dewatering unit comprises whizzer, suction filtration tank, ground water leg and wash water pipeline, the wash water water outlet of described whizzer and described suction filtration tank is higher than described ground water leg entrance, the washing water outlet of described whizzer and described suction filtration tank arranges the opening of 45 ° downwards, the washing water outlet bottom of described whizzer and described suction filtration tank arranges depression filter cloth, and described depression filter cloth is for collecting the throw out after described dehydration.
embodiment 4
(1) detect: the carbonate concentration of carbonic acid precipitating rare earth mother liquor and rare earth ion concentration are detected;
(2) siphon: the siphon of carbonic acid precipitating rare earth mother liquor is entered ground water leg;
(3) feed supplement: according to the detected result of step (1), as carbonic acid precipitating rare earth mother liquor Rare Earth Ion >0.005mol/L, in carbonic acid precipitating rare earth mother liquor, drip the sodium carbonate solution of 200g/L, make carbonate concentration remain 0.05mol/L, precipitating rare earth ion;
(4) solid-liquid separation: step (3) gained feed liquid is left standstill 15min naturally, and supernatant liquor is discharged to carbonic acid precipitating rare earth wastewater collection pond, reclaims precipitation;
(5) dewater: be deposited in dewatering unit by step (4) gained and dewater, waste water is discharged to carbonic acid precipitating rare earth wastewater collection pond, and the throw out after dehydration is recovering rare earth element.
Wherein, described dewatering unit comprises whizzer, suction filtration tank, ground water leg and wash water pipeline, the wash water water outlet of described whizzer and described suction filtration tank is higher than described ground water leg entrance, the washing water outlet of described whizzer and described suction filtration tank arranges the opening of 45 ° downwards, the washing water outlet bottom of described whizzer and described suction filtration tank arranges depression filter cloth, and described depression filter cloth is for collecting the throw out after described dehydration.
embodiment 5
(1) detect: the carbonate concentration of carbonic acid precipitating rare earth mother liquor and rare earth ion concentration are detected;
(2) siphon: the siphon of carbonic acid precipitating rare earth mother liquor is entered ground water leg;
(3) feed supplement: according to the detected result of step (1), as carbonic acid precipitating rare earth mother liquor Rare Earth Ion >0.005mol/L, in carbonic acid precipitating rare earth mother liquor, drip the sodium carbonate solution of 120g/L, make carbonate concentration remain 0.5mol/L, precipitating rare earth ion;
(4) solid-liquid separation: step (3) gained feed liquid is left standstill 20min naturally, and supernatant liquor is discharged to carbonic acid precipitating rare earth wastewater collection pond, reclaims precipitation;
(5) dewater: be deposited in dewatering unit by step (4) gained and dewater, waste water is discharged to carbonic acid precipitating rare earth wastewater collection pond, and the throw out after dehydration is recovering rare earth element.
Wherein, described dewatering unit comprises whizzer, suction filtration tank, ground water leg and wash water pipeline, the wash water water outlet of described whizzer and described suction filtration tank is higher than described ground water leg entrance, the washing water outlet of described whizzer and described suction filtration tank arranges the opening of 45 ° downwards, the washing water outlet bottom of described whizzer and described suction filtration tank arranges depression filter cloth, and described depression filter cloth is for collecting the throw out after described dehydration.
embodiment 6
(1) detect: the carbonate concentration of carbonic acid precipitating rare earth mother liquor and rare earth ion concentration are detected;
(2) siphon: the siphon of carbonic acid precipitating rare earth mother liquor is entered ground water leg;
(3) feed supplement: according to the detected result of step (1), as carbonic acid precipitating rare earth mother liquor Rare Earth Ion >0.005mol/L, in carbonic acid precipitating rare earth mother liquor, drip the sodium carbonate solution of 150g/L, make carbonate concentration remain 0.3mol/L, precipitating rare earth ion;
(4) solid-liquid separation: step (3) gained feed liquid is left standstill 18min naturally, and supernatant liquor is discharged to carbonic acid precipitating rare earth wastewater collection pond, reclaims precipitation;
(5) dewater: be deposited in dewatering unit by step (4) gained and dewater, waste water is discharged to carbonic acid precipitating rare earth wastewater collection pond, and the throw out after dehydration is recovering rare earth element.
Wherein, described dewatering unit comprises whizzer, suction filtration tank, ground water leg and wash water pipeline, the wash water water outlet of described whizzer and described suction filtration tank is higher than described ground water leg entrance, the washing water outlet of described whizzer and described suction filtration tank arranges the opening of 45 ° downwards, the washing water outlet bottom of described whizzer and described suction filtration tank arranges depression filter cloth, and described depression filter cloth is for collecting the throw out after described dehydration.
Claims (7)
1. the method for recovering rare earth element from carbonic acid precipitating rare earth mother liquor, is characterized in that, comprise the following steps:
(1) detect: the carbonate concentration of carbonic acid precipitating rare earth mother liquor and rare earth ion concentration are detected;
(2) siphon: the siphon of carbonic acid precipitating rare earth mother liquor is entered ground water leg;
(3) feed supplement: according to the detected result of step (1), as carbonic acid >0.5mol/L in carbonic acid precipitating rare earth mother liquor, in carbonic acid precipitating rare earth mother liquor, add rare earth feed liquid, reduce carbonate concentration, make carbonate concentration remain 0.05-0.5mol/L; As carbonic acid precipitating rare earth mother liquor Rare Earth Ion >0.005mol/L, in carbonic acid precipitating rare earth mother liquor, drip sodium carbonate solution, make carbonate concentration remain 0.05-0.5mol/L, precipitating rare earth ion;
(4) solid-liquid separation: step (3) gained feed liquid naturally left standstill, supernatant liquor is discharged to carbonic acid precipitating rare earth wastewater collection pond, reclaims precipitation;
(5) dewater: be deposited in dewatering unit by step (4) gained and dewater, waste water is discharged to carbonic acid precipitating rare earth wastewater collection pond, and the throw out after dehydration is recovering rare earth element.
2. the method for recovering rare earth element from oxalic acid precipitation rare earth mother solution according to claim 1, is characterized in that, in step (3), when adding sodium carbonate solution, the concentration of described sodium carbonate solution is 120-200g/L.
3. the method for recovering rare earth element from carbonic acid precipitating rare earth mother liquor according to claim 1, is characterized in that, the described time naturally left standstill is 15-20min.
4. the method for recovering rare earth element from carbonic acid precipitating rare earth mother liquor according to claim 3, it is characterized in that, in step (5), described dewatering unit comprises whizzer, suction filtration tank, ground water leg and wash water pipeline, and the wash water water outlet of described whizzer and described suction filtration tank is higher than described ground water leg entrance.
5. the method for recovering rare earth element from carbonic acid precipitating rare earth mother liquor according to claim 4, is characterized in that, the washing water outlet of described whizzer and described suction filtration tank arranges the opening of 45 ° downwards.
6. the method for recovering rare earth element from carbonic acid precipitating rare earth mother liquor according to claim 5, is characterized in that, the washing water outlet bottom of described whizzer and described suction filtration tank arranges depression filter cloth.
7. the method for recovering rare earth element from carbonic acid precipitating rare earth mother liquor according to claim 6, is characterized in that, described depression filter cloth is for collecting the throw out after described dehydration.
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| CN201510636271.0A CN105219962A (en) | 2015-09-30 | 2015-09-30 | A kind of method of recovering rare earth element from carbonic acid precipitating rare earth mother liquor |
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| CN201510636271.0A CN105219962A (en) | 2015-09-30 | 2015-09-30 | A kind of method of recovering rare earth element from carbonic acid precipitating rare earth mother liquor |
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN109252058A (en) * | 2018-10-19 | 2019-01-22 | 中铝广西国盛稀土开发有限公司 | A kind of method that oxalic acid precipitation RE waste water recycles |
| CN109402395A (en) * | 2018-10-19 | 2019-03-01 | 中铝广西国盛稀土开发有限公司 | A kind of method of ammonium carbonate precipitating rare earth waste water reuse |
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| CN103436697A (en) * | 2013-08-15 | 2013-12-11 | 南昌大学 | Rare-earth carbonate crystallizing and precipitating method for processing aluminum-containing rare-earth feed liquid |
| CN103952554A (en) * | 2014-05-19 | 2014-07-30 | 淄博包钢灵芝稀土高科技股份有限公司 | Method for precipitating excellent-acid-solubility cerium-containing rare-earth carbonate |
| JP2015036430A (en) * | 2013-08-12 | 2015-02-23 | 三菱マテリアル株式会社 | METHOD FOR RECOVERING Ce AT HIGH PURITY |
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2015
- 2015-09-30 CN CN201510636271.0A patent/CN105219962A/en active Pending
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1675131A (en) * | 2002-06-07 | 2005-09-28 | 昭和电工株式会社 | Process for recovering rare earth oxide from waste liquid containing rare earth element, and process for producing rare earth oxide using same |
| CN102978398A (en) * | 2012-12-12 | 2013-03-20 | 南昌大学 | Method for obviously lowering chlorine content in process of carbonic acid rare earth crystallization |
| JP2015036430A (en) * | 2013-08-12 | 2015-02-23 | 三菱マテリアル株式会社 | METHOD FOR RECOVERING Ce AT HIGH PURITY |
| CN103436697A (en) * | 2013-08-15 | 2013-12-11 | 南昌大学 | Rare-earth carbonate crystallizing and precipitating method for processing aluminum-containing rare-earth feed liquid |
| CN103952554A (en) * | 2014-05-19 | 2014-07-30 | 淄博包钢灵芝稀土高科技股份有限公司 | Method for precipitating excellent-acid-solubility cerium-containing rare-earth carbonate |
Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN109252058A (en) * | 2018-10-19 | 2019-01-22 | 中铝广西国盛稀土开发有限公司 | A kind of method that oxalic acid precipitation RE waste water recycles |
| CN109402395A (en) * | 2018-10-19 | 2019-03-01 | 中铝广西国盛稀土开发有限公司 | A kind of method of ammonium carbonate precipitating rare earth waste water reuse |
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