CN105838881B - Southern ion type rareearth ore leaching liquid impurity removal process - Google Patents
Southern ion type rareearth ore leaching liquid impurity removal process Download PDFInfo
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- CN105838881B CN105838881B CN201610406145.0A CN201610406145A CN105838881B CN 105838881 B CN105838881 B CN 105838881B CN 201610406145 A CN201610406145 A CN 201610406145A CN 105838881 B CN105838881 B CN 105838881B
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/44—Treatment or purification of solutions, e.g. obtained by leaching by chemical processes
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/22—Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B59/00—Obtaining rare earth metals
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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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- General Life Sciences & Earth Sciences (AREA)
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- Chemical Kinetics & Catalysis (AREA)
- General Chemical & Material Sciences (AREA)
- Manufacture And Refinement Of Metals (AREA)
- Compounds Of Alkaline-Earth Elements, Aluminum Or Rare-Earth Metals (AREA)
Abstract
A kind of southern ion type rareearth ore leaching liquid impurity removal process, comprises the following steps, and the preparation of mine-for-leach liquid rare earth mother solution, magnesium oxide precipitation enrichment rare earth, rareearth enriching material clarification, alkali leaching are miscellaneous, the molten, Al of acid (OH)3Product output.The southern ion type rareearth ore leaching liquid impurity removal process of the present invention, has used the quick hydroxide of big yield to be enriched with, because rare earth hydrate solubility is minimum, so enriching and recovering rate nearly 100%, precipitated using the characteristic nucleation of magnesia, precipitation is fast, greatly increases the utilization rate of flow sheet equipment；The miscellaneous ultrahigh in efficiency of alkali leaching, rare earth loss is few, can reduce the after-treatment expense of slag, and output Al (OH)3Product, substantially, cost is lower compared with traditional handicraft, and rare earth yield is than traditional handicraft 5% for economic benefit.
Description
Technical field
The present invention relates to Rare Earth Mine recovery process, especially a kind of southern ion type rareearth ore leaching liquid impurity removal process.
Background technology
Southern ion type rareearth ore is also known as weathered superficial leaching rare-earth ore, and late 1960s are sent out in Jiangxi Province Longnan
It is existing, it is found in Nanling mountains such as Fujian, Hunan, Guangdong, Guangxi in succession thereafter.Southern ion type rareearth ore is special due to its
The origin cause of formation so that rare earth ion preservation is in the clay that various Mineral Weatherings are produced, and its leaching follows ion exchange principle, so
Current mining mode substantially enters solution using the rare earth ion that electrolyte solution is exchanged in ore body as leaching ore deposit agent, then by removing
General labourer's sequence, the enriched substance for then obtaining rare earth Zong Liang≤90% with suitable precipitating reagent precipitating rare earth is made into one for Rare Earth Separation factory
Step separation is used.Non-rare earth impurity in rare earth mother solution is mainly Al3+With a small amount of non-ferrous metal, alkaline-earth metal etc., except Al3+
Process is realized by adjusting mother liquor pH=5.4, and part rare earth co-precipitation will be made during this and causes second extraction etc. numerous and diverse
The generation of process, while will also there is part rare earth loss.
The content of the invention
It is an object of the invention to provide one kind except aluminium is simple, rare earth yield is high, while there is economic value Al
(OH)3The southern ion type rareearth ore leaching liquid impurity removal process of product.
The southern ion type rareearth ore leaching liquid impurity removal process of the present invention, comprises the following steps：
1st, magnesium oxide powder is added in mine-for-leach liquid rare earth mother solution, stirred, and detect pH value, with pH≤7.4
For terminal, stand；
2nd, discharge supernatant matches somebody with somebody liquid pool to ore deposit agent is soaked, and bottom slag charge is sent to plate and frame filter press press filtration, and filtrate drains into leaching ore deposit agent
With liquid pool, filter residue is transferred in agitator, test Al (OH)3Content is standby；
3rd, the filter residue in agitator adds clear water to be sized mixing, liquid-solid ratio 1:1, add test Al (OH)3Amount and sodium hydroxide
After the sodium hydrate solid that 1.2 times of reaction theory quantity, leaching 0.5-0.6 hours, plus clear water is to liquid-solid ratio 5:1 stirring
0.5-1 hours, then plate-frame filtering, filtrate collected standby, and slag charge returns to above-mentioned agitator and adds clear water liquid-solid ratio 5:1 stirs and washes, then
Plate-frame filtering, filtrate storage is standby, and it is standby that filter residue is transferred to another agitator；
4th, sour excellent molten, liquid-solid ratio 3 is carried out to the enrichment slag that previous step is produced with any concentration hydrochloric acid or sulfuric acid:1, reaction
Terminal is pH=2.5, and plate-frame filtering, filter residue is stored up, and the rare earth feed liquid of generation can be precipitated by sodium hydroxide or sodium acid carbonate
Output rare earth hydrate or carbonated rare earth；Or filtrate is directly entered storage tank and treats that progress next time is excellent molten, is used as bottom liquid to be superimposed rare earth
The feed liquid of concentration is used；
5、Al(OH)3Product output, the alkali immersion liquid produced to step 3-filtrate acid adding carries out tune pH=9 and produces Al (OH)3It is heavy
Form sediment, plate-frame filtering, filtrate is delivered to the agent of leaching ore deposit and matches somebody with somebody liquid pool, and filter residue adds clear water liquid-solid ratio 5:1 stirs and washes, plate compression, filtrate discharge
Match somebody with somebody liquid pool to the agent of leaching ore deposit, filter residue is Al (OH)3。
The southern ion type rareearth ore leaching liquid impurity removal process of the present invention, has used the quick hydroxide of big yield rich
Collection, because rare earth hydrate solubility is minimum, so enriching and recovering rate nearly 100%, is precipitated using the characteristic nucleation of magnesia, sunk
Form sediment fast, greatly increase the utilization rate of flow sheet equipment；The miscellaneous ultrahigh in efficiency of alkali leaching, rare earth loss is few, can reduce the secondary of slag
Processing cost, and output Al (OH)3Product, substantially, cost is lower compared with traditional handicraft for economic benefit, and rare earth yield is than passing
System technique 5%.
Embodiment
Embodiment
A kind of southern ion type rareearth ore leaching liquid impurity removal process, comprises the following steps：
1st, the preparation of mine-for-leach liquid rare earth mother solution：300m3Storage pool, 250m3Rare earth mother solution, mother liquor middle rare earth concentration
0.2g/L,pH=4.5；
2nd, magnesia warehouse：For an iron 2m3Conical hopper, outlet at bottom is provided with spiral automatic feeder（It is adjustable to turn
Speed control feeding coal）；
3rd, mixing pit：One 10m3Cement with stirring, brick masonry circle pond, magnesia warehouse set up its top, a band
Stir 100m3Cement, brick masonry circle pond；
4th, depositing reservoir： 400m3Cement, brick masonry circle pond or Fang Chi；
5th, magnesium oxide precipitation enrichment rare earth：1 ton of magnesium oxide powder is put into magnesia warehouse, is transported to by batcher
10m3Mixing pit, while rare earth mother solution is delivered to 10 m by PVC pipeline3Mixing pit is mixed into thin pulp shape with magnesia；
6th, step 5 produces slurries and is delivered to 100 m by PVC pipeline3Mixing pit, while by PVC pipeline that rare earth is female
Liquid is delivered to 100m3Mixing pit stirring mixing, survey pH≤7.4 are terminal；
7th, rareearth enriching material is clarified：The mixed serum that step 6 is produced flows into 400 m by PVC bottoms pipe3Depositing reservoir, stands
Half an hour, discharge supernatant matches somebody with somebody liquid pool to ore deposit agent is soaked；
8th, step 7 bottom slag charge is transported to plate and frame filter press press filtration by PVC pipeline, and filtrate drains into the agent of leaching ore deposit and matches somebody with somebody liquid pool,
Filter residue is transferred to 20 m3In PP material stirrings bucket, Al (OH) is tested3Content is standby；
9th, alkali leaching is miscellaneous：It is to be based on Al to carry out the miscellaneous method of alkali leaching to the enrichment slag that step 8 is produced3+Both sexes, it is and dilute
Principle of the native hydroxide insoluble in alkali, sizes mixing to the enrichment slag that step 8 is produced, liquid-solid ratio 1:1, add test Al
(OH)3The sodium hydrate solid of 1.2 times of amount and sodium hydroxide reaction theory quantity（Technical pure）, it is after leaching half an hour plus clear
Water is to liquid-solid ratio 5:1 stirs half an hour, then plate-frame filtering, and filtrate is collected to 10 m3 PP material stirrings bucket, slag charge returns to stirring
Bucket plus clear water liquid-solid ratio 5:1 stirs and washes once, plate-frame filtering, and filtrate storage is standby, and filter residue is transferred to another 10 m3 PP materials are stirred
Mix bucket standby；
10th, acid is molten：Sour excellent molten, liquid-solid ratio 3 is carried out to the enrichment slag that step 9 is produced with any concentration hydrochloric acid or sulfuric acid:1,
Reaction end pH=2.5；Plate-frame filtering, filter residue is stored up, and the rare earth feed liquid of generation can be sunk by sodium hydroxide or sodium acid carbonate
Shallow lake output rare earth hydrate or carbonated rare earth, or filtrate are directly entered storage tank and treat that progress next time is excellent molten as bottom liquid superposition rare earth
Concentration reaches that high concentration feed liquid is used；
11、Al(OH)3Product output：Tune pH=9 are carried out to the alkali immersion liquid acid adding that step 9 is produced and produce Al (OH)3Precipitation, plate
Frame is filtered, and filtrate is piped to the agent of leaching ore deposit and matches somebody with somebody liquid pool, and filter residue adds clear water liquid-solid ratio 5:1 stirs and washes, plate compression, filtrate discharge
Match somebody with somebody liquid pool to the agent of leaching ore deposit, filter residue dress bag can be used as Al (OH)3Product is sold.
Claims (1)
1. a kind of southern ion type rareearth ore leaching liquid impurity removal process, it is characterised in that：It comprises the following steps：
（1）, in mine-for-leach liquid rare earth mother solution add magnesium oxide powder, stir, and detect pH value, be with pH≤7.4
Terminal, stands；
（2）, discharge supernatant match somebody with somebody liquid pool to ore deposit agent is soaked, bottom slag charge is sent to plate and frame filter press press filtration, and filtrate drains into leaching ore deposit agent and matched somebody with somebody
Liquid pool, filter residue is transferred in agitator, test Al (OH)3Content is standby；
（3）, the filter residue in agitator add clear water to be sized mixing, liquid-solid ratio 1:1, add test Al (OH)3Amount is reacted with sodium hydroxide
After the sodium hydrate solid of theoretical 1.2 times of quantity, leaching 0.5-0.6 hours, plus clear water is to liquid-solid ratio 5:1 stirring 0.5-1
Hour, then plate-frame filtering, filtrate collects standby, and slag charge returns to above-mentioned agitator and adds clear water liquid-solid ratio 5:1 stirs and washes, then sheet frame mistake
Filter, filtrate storage is standby, and it is standby that filter residue is transferred to another agitator；
（4）, sour excellent molten, liquid-solid ratio 3 is carried out with any concentration hydrochloric acid or sulfuric acid to the enrichment slag that previous step is produced:1, reaction is eventually
Point is pH=2.5, and plate-frame filtering, filter residue is stored up, and the rare earth feed liquid of generation carries out precipitation output by sodium hydroxide or sodium acid carbonate
Rare earth hydrate or carbonated rare earth；Or filtrate is directly entered storage tank and treats that progress next time is excellent molten, is used as bottom liquid to be superimposed rare earth concentration
Feed liquid use；
（5）、Al(OH)3Product output, to step（3）The alkali immersion liquid of generation-filtrate acid adding carries out tune pH=9 and produces Al (OH)3It is heavy
Form sediment, plate-frame filtering, filtrate is delivered to the agent of leaching ore deposit and matches somebody with somebody liquid pool, and filter residue adds clear water liquid-solid ratio 5:1 stirs and washes, plate compression, filtrate discharge
Match somebody with somebody liquid pool to the agent of leaching ore deposit, filter residue is Al (OH)3。
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| CN201610406145.0A CN105838881B (en) | 2016-06-12 | 2016-06-12 | Southern ion type rareearth ore leaching liquid impurity removal process |
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| CN201610406145.0A CN105838881B (en) | 2016-06-12 | 2016-06-12 | Southern ion type rareearth ore leaching liquid impurity removal process |
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| CN105838881B true CN105838881B (en) | 2017-11-07 |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN108823417A (en) * | 2018-07-16 | 2018-11-16 | 孙东江 | The method of useless power battery recycling non-ferrous metal removal of impurities |
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| CN107217139A (en) * | 2017-05-31 | 2017-09-29 | 赣州稀土开采技术服务有限公司 | Southern ion type rareearth ore is without ammonia production practice |
| CN108893606B (en) * | 2018-08-30 | 2019-11-08 | 江西理工大学 | Precipitating, removal of impurities, middling recurrence extract the method without rare earth in ammonium rare earth mother solution |
| CN114763586B (en) * | 2021-01-11 | 2024-03-08 | 中国科学院江西稀土研究院 | Method for strengthening neutral phase reconstruction and aluminum resource utilization of rare earth mother liquor |
| CN113553787B (en) * | 2021-07-22 | 2023-04-25 | 江西理工大学 | Numerical simulation method for agitation leaching process of ionic rare earth ore |
| CN114107706B (en) * | 2021-11-29 | 2023-09-08 | 江西理工大学 | Method for purifying and removing impurities from ion type rare earth ore leaching solution |
| CN114774719A (en) * | 2022-04-29 | 2022-07-22 | 王静若 | Treatment method for recovering oxalate from heavy metal in rare earth post-solution after oxalic acid precipitation |
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| CN104743586B (en) * | 2013-12-27 | 2017-11-14 | 中国科学院过程工程研究所 | The combine production method of the leaching of aluminium alkali and alumina decomposition mother liquid evaporation salt discharge in a kind of Bayer process red mud |
| CN104611561A (en) * | 2015-03-09 | 2015-05-13 | 龙南县锦易矿业有限公司 | Precipitation process for leaching mother liquid of south rare earth ore |
| CN105506287B (en) * | 2016-01-13 | 2017-09-19 | 赣州稀土开采技术服务有限公司 | The technique that southern RE ore leaches mother liquor precipitation method recovering rare earth |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN108823417A (en) * | 2018-07-16 | 2018-11-16 | 孙东江 | The method of useless power battery recycling non-ferrous metal removal of impurities |
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Effective date of registration: 20170217 Address after: 341700 Jiangxi city of Ganzhou province Zhanggong District Hongqi Road No. 20 building four floor of rare earth Applicant after: Ganzhou rare earth mining technology service Co., Ltd. Address before: Yufeng 341700 Jiangxi city in Ganzhou Province, Longnan County Beverly Industrial Park, Longnan County Mining Co. Ltd. Applicant before: Sun Dongjiang Applicant before: Wang Zhiyong Applicant before: Liao Shengyuan |
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| CB03 | Change of inventor or designer information |
Inventor after: Sun Dongjiang Inventor after: Zhang Cheng Inventor after: Chen Guoliang Inventor after: Li Zhao Inventor after: Huang Bin Inventor after: Zhu Jianling Inventor after: Shi Zhanhua Inventor after: Pan Wei Inventor after: Yuan Xianqiang Inventor after: Huang Kailong Inventor after: Dai Shengxian Inventor after: Wang Zhiyong Inventor after: Yang Yang Inventor after: Liao Shengyuan Inventor after: Wang Youlin Inventor after: Wang Qiang Inventor after: Zou Zhiqiang Inventor after: Zhao Xuefu Inventor after: Lin Hai Inventor after: Cheng Zhe Inventor before: Sun Dongjiang Inventor before: Wang Zhiyong Inventor before: Liao Shengyuan |
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