CN105200250A - Method of recovering rare-earth elements from oxalic acid precipitate rare-earth mother liquor - Google Patents
Method of recovering rare-earth elements from oxalic acid precipitate rare-earth mother liquor Download PDFInfo
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- CN105200250A CN105200250A CN201510636320.0A CN201510636320A CN105200250A CN 105200250 A CN105200250 A CN 105200250A CN 201510636320 A CN201510636320 A CN 201510636320A CN 105200250 A CN105200250 A CN 105200250A
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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 relates to a method of recovering rare-earth elements from oxalic acid precipitate rare-earth mother liquor. The method includes the steps such as examining, siphoning, supplementing, solid-liquid separating and dewatering; dewatered precipitate is recovered rare-earth elements. Resource waste may be avoided by efficiently recovering the rare-earth elements from the oxalic acid precipitate rare-earth mother liquor; by pretreating the oxalic acid precipitate rare-earth mother liquor, oxalic acid concentration is decreased and waste water treatment cost is lowered; the method is simple to operate and low in cost and has good economic and social benefits.
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 oxalic acid precipitation rare earth mother solution.
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 oxalic acid precipitation rare earth mother solution is provided.
The present invention realizes in the following way:
A method for recovering rare earth element from oxalic acid precipitation rare earth mother solution, comprises the following steps:
(1) detect: the concentration of oxalic acid of oxalic acid precipitation rare earth mother solution and rare earth ion concentration are detected;
(2) siphon: the siphon of oxalic acid precipitation rare earth mother solution is entered ground water leg;
(3) feed supplement: according to the detected result of step (1), as oxalic acid precipitation rare earth mother solution mesoxalic acid content >0.008mol/L, in oxalic acid precipitation rare earth mother solution, add rare earth feed liquid, reduce concentration of oxalic acid, make concentration of oxalic acid remain 0.004-0.008mol/L; As oxalic acid precipitation rare earth mother solution Rare Earth Ion content >0.005mol/L, in oxalic acid precipitation rare earth mother solution, drip oxalic acid solution, make concentration of oxalic acid remain 0.004-0.008mol/L, precipitating rare earth ion;
(4) solid-liquid separation: step (3) gained feed liquid naturally left standstill, supernatant liquor is discharged to oxalic acid precipitation RE waste water collecting tank, reclaims precipitation;
(5) dewater: be deposited in dewatering unit by step (4) gained and dewater, waste water is discharged to oxalic acid precipitation RE waste water collecting tank, and the throw out after dehydration is recovering rare earth element.
Preferably, in step (3), when dripping oxalic acid solution, the concentration of described oxalic acid solution is 2-4mol/L.
Preferably, the described time naturally left standstill is 10-15min.
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 oxalic acid precipitation rare earth mother solution, avoids the waste of resource.
2. the present invention can carry out pre-treatment to oxalic acid precipitation rare earth mother solution, reduces concentration of oxalic acid, 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 oxalic acid precipitation rare earth mother solution, comprises the following steps:
(1) detect: the concentration of oxalic acid of oxalic acid precipitation rare earth mother solution and rare earth ion concentration are detected;
(2) siphon: the siphon of oxalic acid precipitation rare earth mother solution is entered ground water leg;
(3) feed supplement: according to the detected result of step (1), as oxalic acid precipitation rare earth mother solution mesoxalic acid content >0.008mol/L, in oxalic acid precipitation rare earth mother solution, add rare earth feed liquid, reduce concentration of oxalic acid, concentration of oxalic acid is made to remain 0.004mol/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 oxalic acid precipitation RE waste water collecting tank, reclaims precipitation;
(5) dewater: be deposited in dewatering unit by step (4) gained and dewater, waste water is discharged to oxalic acid precipitation RE waste water collecting tank, 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
A method for recovering rare earth element from oxalic acid precipitation rare earth mother solution, comprises the following steps:
(1) detect: the concentration of oxalic acid of oxalic acid precipitation rare earth mother solution and rare earth ion concentration are detected;
(2) siphon: the siphon of oxalic acid precipitation rare earth mother solution is entered ground water leg;
(3) feed supplement: according to the detected result of step (1), as oxalic acid precipitation rare earth mother solution Rare Earth Ion content >0.005mol/L, in oxalic acid precipitation rare earth mother solution, drip the oxalic acid solution of 4mol/L, make concentration of oxalic acid remain 0.008mol/L, precipitating rare earth ion;
(4) solid-liquid separation: step (3) gained feed liquid is left standstill 10min naturally, and supernatant liquor is discharged to oxalic acid precipitation RE waste water collecting tank, reclaims precipitation;
(5) dewater: be deposited in dewatering unit by step (4) gained and dewater, waste water is discharged to oxalic acid precipitation RE waste water collecting tank, 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
A method for recovering rare earth element from oxalic acid precipitation rare earth mother solution, comprises the following steps:
(1) detect: the concentration of oxalic acid of oxalic acid precipitation rare earth mother solution and rare earth ion concentration are detected;
(2) siphon: the siphon of oxalic acid precipitation rare earth mother solution is entered ground water leg;
(3) feed supplement: according to the detected result of step (1), as oxalic acid precipitation rare earth mother solution Rare Earth Ion content >0.005mol/L, in oxalic acid precipitation rare earth mother solution, drip the oxalic acid solution of 3mol/L, make concentration of oxalic acid remain 0.006mol/L, precipitating rare earth ion;
(4) solid-liquid separation: step (3) gained feed liquid is left standstill 12min naturally, and supernatant liquor is discharged to oxalic acid precipitation RE waste water collecting tank, reclaims precipitation;
(5) dewater: be deposited in dewatering unit by step (4) gained and dewater, waste water is discharged to oxalic acid precipitation RE waste water collecting tank, 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 oxalic acid precipitation rare earth mother solution, is characterized in that, comprise the following steps:
(1) detect: the concentration of oxalic acid of oxalic acid precipitation rare earth mother solution and rare earth ion concentration are detected;
(2) siphon: the siphon of oxalic acid precipitation rare earth mother solution is entered ground water leg;
(3) feed supplement: according to the detected result of step (1), as oxalic acid precipitation rare earth mother solution mesoxalic acid content >0.008mol/L, in oxalic acid precipitation rare earth mother solution, add rare earth feed liquid, reduce concentration of oxalic acid, make concentration of oxalic acid remain 0.004-0.008mol/L; As oxalic acid precipitation rare earth mother solution Rare Earth Ion content >0.005mol/L, in oxalic acid precipitation rare earth mother solution, drip oxalic acid solution, make concentration of oxalic acid remain 0.004-0.008mol/L, precipitating rare earth ion;
(4) solid-liquid separation: step (3) gained feed liquid naturally left standstill, supernatant liquor is discharged to oxalic acid precipitation RE waste water collecting tank, reclaims precipitation;
(5) dewater: be deposited in dewatering unit by step (4) gained and dewater, waste water is discharged to oxalic acid precipitation RE waste water collecting tank, 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 dripping oxalic acid solution, the concentration of described oxalic acid solution is 2-4mol/L.
3. the method for recovering rare earth element from oxalic acid precipitation rare earth mother solution according to claim 1, is characterized in that, the described time naturally left standstill is 10-15min.
4. the method for recovering rare earth element from oxalic acid precipitation rare earth mother solution 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 oxalic acid precipitation rare earth mother solution 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 oxalic acid precipitation rare earth mother solution 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 oxalic acid precipitation rare earth mother solution 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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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106119541A (en) * | 2016-06-23 | 2016-11-16 | 五矿（北京）稀土研究院有限公司 | A kind of method of oxalic acid precipitation rare earth |
| 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 |
| CN109293048A (en) * | 2018-10-19 | 2019-02-01 | 中铝广西国盛稀土开发有限公司 | A kind of method of RE waste water resource reutilization |
Citations (5)
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| JPH01230732A (en) * | 1988-03-09 | 1989-09-14 | Sumitomo Light Metal Ind Ltd | Recovering method for rare earth metal |
| WO2003104149A1 (en) * | 2002-06-07 | 2003-12-18 | Showa Denko K.K. | Process for recovering rare earth oxide from waste liquid containing rare earth element, and process for producing rare earth oxide using same |
| CN201650891U (en) * | 2010-03-25 | 2010-11-24 | 江阴加华新材料资源有限公司 | Supernatant fluid siphoning device of rare earth reaction vessel |
| CN103131862A (en) * | 2013-03-13 | 2013-06-05 | 龙南县中利再生资源开发有限公司 | Pretreatment decomposition method for extracting high-purity rare earth oxide from phosphor powder waste material |
| CN104419839A (en) * | 2013-08-19 | 2015-03-18 | 中铝稀土（常州）有限公司 | Method for preparing rare earth oxalate precipitation |
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2015
- 2015-09-30 CN CN201510636320.0A patent/CN105200250A/en active Pending
Patent Citations (5)
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| JPH01230732A (en) * | 1988-03-09 | 1989-09-14 | Sumitomo Light Metal Ind Ltd | Recovering method for rare earth metal |
| WO2003104149A1 (en) * | 2002-06-07 | 2003-12-18 | Showa Denko K.K. | Process for recovering rare earth oxide from waste liquid containing rare earth element, and process for producing rare earth oxide using same |
| CN201650891U (en) * | 2010-03-25 | 2010-11-24 | 江阴加华新材料资源有限公司 | Supernatant fluid siphoning device of rare earth reaction vessel |
| CN103131862A (en) * | 2013-03-13 | 2013-06-05 | 龙南县中利再生资源开发有限公司 | Pretreatment decomposition method for extracting high-purity rare earth oxide from phosphor powder waste material |
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| 张凌云等: "草酸沉淀法制备氧化钕工艺研究", 《无机盐工业》 * |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN106119541A (en) * | 2016-06-23 | 2016-11-16 | 五矿（北京）稀土研究院有限公司 | A kind of method of oxalic acid precipitation rare earth |
| 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 |
| CN109293048A (en) * | 2018-10-19 | 2019-02-01 | 中铝广西国盛稀土开发有限公司 | A kind of method of RE waste water resource reutilization |
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