CN109628736A - A kind of south ion type rareearth ore rare-earth products intermediate processing - Google Patents
A kind of south ion type rareearth ore rare-earth products intermediate processing Download PDFInfo
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- CN109628736A CN109628736A CN201910091387.9A CN201910091387A CN109628736A CN 109628736 A CN109628736 A CN 109628736A CN 201910091387 A CN201910091387 A CN 201910091387A CN 109628736 A CN109628736 A CN 109628736A
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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
- C22B3/04—Extraction of metal compounds from ores or concentrates by wet processes by leaching
- C22B3/06—Extraction of metal compounds from ores or concentrates by wet processes by leaching in inorganic acid solutions, e.g. with acids generated in situ; in inorganic salt solutions other than ammonium salt solutions
- C22B3/08—Sulfuric acid, other sulfurated acids or salts thereof
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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
- 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
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
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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
- 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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Abstract
A kind of south ion type rareearth ore rare-earth products intermediate processing, the rareearth enriching material generated using southern ion type rareearth ore mine recovering rare earth process is raw material, its main component is magnesia, rare earth hydrate, aluminium hydroxide, wherein rare earth total content is between 20 more than ten percent to percent, it is molten that acid is carried out to rareearth enriching material first, so that rare earth dissolves, then acid decomposition liquid pH >=5.4 are adjusted with rareearth enriching material again, plate compression, filter residue returns to acid dissolution, filtrate carries out rare-earth precipitation output purpose rare-earth products, it can directly be dissolved with extractant after this rare-earth products is washed and obtain supported rare earth organic phase progress rare earths separation.Southern ion type rareearth ore rare-earth products intermediate processing production cost of the invention is low, simple process, and the rare-earth products purity is high of obtained south ion type rareearth ore output is free of Al2O3Or content is extremely low, and solves the problems, such as the emulsification of Rare Earth Separation factory organic phase and a large amount of high salinity waste waters.
Description
Technical field
The present invention relates to a kind of southern ion type rareearth ore rare-earth products intermediate processings.
Background technique
While leaching rare earth, the non-rare earth impurities such as aluminium can be leached southern ion type rareearth ore simultaneously.And it is traditional
Impurity-removing precipitating process is difficult to make Al2O3It completely removes, so that the Al in the rare-earth products of output2O3Content is in percent zero point
It is several between a few percent, cause rare-earth smelting separation enterprise to carry out secondary removal of impurities, process is many and diverse, and rare earth is made to have few portion
The loss divided, especially Al2O3The not clean organic phase that can cause extraction process is removed to emulsify.
Summary of the invention
A kind of it is an object of the invention to provide production costs low, simple process southern ion type rareearth ore rare-earth products
Intermediate processing, this method makes the rare-earth products purity is high of southern ion type rareearth ore output, and it is organic to solve Rare Earth Separation factory
Mutually emulsification and a large amount of high salinity waste water problems.
A kind of southern ion type rareearth ore rare-earth products intermediate processing of the invention, is returned with southern ion type rareearth ore mine
Receiving the rareearth enriching material that rare earth process generates is raw material, and main component is magnesia, rare earth hydrate, aluminium hydroxide, wherein
It is molten that rare earth total content carries out acid to rareearth enriching material between 20 more than ten percent to percent, first, so that rare earth dissolves,
Then acid decomposition liquid pH >=5.4, plate compression are adjusted with rareearth enriching material again, filter residue returns to acid dissolution, and it is heavy that filtrate carries out rare earth
Shallow lake output purpose rare-earth products, can directly be dissolved that obtain supported rare earth organic with extractant after this rare-earth products is washed
Mutually carry out rare earths separation, the specific steps are as follows:
1, acid dissolution: taking the rareearth enriching material of total amount a quarter in sour decomposition bucket, adds clear water stirring to size mixing, is then added dropwise dense
Sulfuric acid carries out sour decomposition, and reaction end stablizes half an hour with pH=1, and then plus clear water is to standing, and filters, filters through plate and frame filter press
Wash heat discards after washing, and filtrate is transferred to spare in another sour decomposition bucket.
2, the filtrate of the rareearth enriching material of surplus 3/4ths and above-mentioned steps is mixed, and rareearth enriching material is gradually added
Enter, when material liquid pH to be mixed reaches 4.8-5.4, stir half an hour, material liquid pH adds rareearth enriching material when being not up to 5.4, adjust
PH stablizes in >=5.4 plate-frame filterings, and filtrate is transferred to settling box, and filter residue return step 1 carries out acid dissolution.
3, rare-earth precipitation: under agitation to step 2 generate rare-earth liquid in be passed through concentration 5% ~ 10% ammonium hydroxide or
Ammonium bicarbonate soln carries out rare-earth precipitation, and precipitating terminal is pH >=7；Then it is filtered through plate and frame filter press, filtrate to fluid reservoir is stored up
It deposits, filter residue is spare after 3 ~ 5 times clear water agitator treatings.
4, ammonium recovery ammonium hydroxide: magnesium oxide powder will be added in the filtrate after precipitating that step 3 generates, after mixing evenly
It is pumped into jet-flow aeration tower with pump, cyclic aeration is carried out in >=80 DEG C of system, ammonia imports ammonia through top of tower venthole
Absorption tower carries out counter-current absorption with clear water, the NH in liquid after precipitating4 +Content filters after being lower than 50mg/l through board and frame machine, and filtrate is led
Enter fluid reservoir and can be used as leaching mine agent to be recycled, filter residue is used for production magnesium sulfate, and the ammonium hydroxide of recycling reaches after concentration as heavy
Shallow lake agent is recycled.
5, extractant dissolution rare-earth products (or rare-earth sodium saponification organic phase): the rare-earth products clear water that step 3 is generated
Be slurred, the mixing chamber for being placed with P507 imported by pipeline, organic phase: slurry carries out mixing half an hour compared to 1:1, then mixes
It mutually imports clarifying chamber to be clarified, upper organic phase is supported rare earth organic phase, is used for Rare Earth Separation, and lower layer's water phase, which returns, to be adjusted
Rare-earth products slurry uses.
6, remove aluminium: the slag that step 2 generates is transferred to alkali turning barrel after 3-4 times is recycled, and is sized mixing with clear water, liquid-solid ratio 2:1,
Then it is added solid sodium hydroxide, it is naoh concentration >=250g/l that addition amount of sodium hydroxide, which is subject to alkali swivel,；It is stirring
Under the conditions of, system temperature maintains 120 DEG C or more, reacts half an hour, then filters through plate and frame filter press, and filtrate is for recycling hydroxide
Aluminium uses, and return step 1 uses after filter residue is washed.
Southern ion type rareearth ore rare-earth products intermediate processing production cost of the invention is low, simple process, obtained
The rare-earth products purity is high of southern ion type rareearth ore output, is free of Al2O3Or content is extremely low (≤0.1%), and solves rare earth
Separate the emulsification of factory's organic phase and a large amount of high salinity waste water problems.
Specific embodiment
A kind of south ion type rareearth ore rare-earth products intermediate processing, comprising the following steps:
The preparation of rareearth enriching material: rareearth enriching material (butt) 1000kg for taking mine recovering rare earth to generate is spare；
The preparation of equipment:
Sour decomposition bucket: 1m3PP material drum 2 with stirring；
Settling box: 1m3PP material drum 2 with stirring；
Fluid reservoir: 5 m32, PE tank；
Plate and frame filter press: 10 m3Plate and frame filter press 4；
Ammonium decomposes and absorption system is a set of: including 1m31, ammonium solution bucket, jet-flow aeration tower 1,1 set of ammonia absorption tower；
Extractant dissolves rare-earth products groove body: 1 set of the mixer-settler of PVC material, wherein 0.5 m of mixing chamber3, 5 m of clarifying chamber3
Alkali turning barrel: 1 m3Drum 1 of irony band stirring, bottom is equipped with electric heater unit；
Specific implementation step:
1, acid dissolution: taking rareearth enriching material 250kg in sour decomposition bucket, adds 0.5 m3Clear water stirring is sized mixing, and dense sulphur is then added dropwise
Acid carries out sour decomposition, and reaction end stablizes half an hour with pH=1, and then plus clear water is to 1 m3It stands, is filtered through plate and frame filter press,
It is discarded after residue washing, filtrate is transferred to spare in another sour decomposition bucket.
2, it by surplus rareearth enriching material, is added step-wise in the bucket stirring of above-mentioned generation rare-earth liquid, expects in bucket to be mixed
When liquid pH reaches 5 or so, stir half an hour, material liquid pH adds a small amount of rareearth enriching material when being not up to 5.4, adjustment pH stablize >=
5.4 plate-frame filterings, filtrate are transferred to settling box, and filter residue return step 1 carries out acid dissolution.
3, rare-earth precipitation: under agitation to step 2 generate rare-earth liquid in be passed through concentration 5% ~ 10% ammonium hydroxide or
Ammonium bicarbonate soln carries out rare-earth precipitation, and precipitating terminal is subject to PH >=7；Then it is filtered through plate and frame filter press, filtrate to liquid storage
Tank storage, filter residue are spare after 3 ~ 5 times clear water agitator treatings.
4, ammonium recovery ammonium hydroxide: liquid after precipitating that step 3 generates is delivered in ammonium decomposition bucket, a certain amount of oxygen is added
Change magnesium dust and carries out cyclic aeration in >=80 DEG C of system, ammonia is through tower after mixing evenly with being pumped into jet-flow aeration tower
Top venthole imports ammonia absorption tower and carries out counter-current absorption with clear water, the NH in liquid after precipitating4 +After content is lower than 50mg/l
It is filtered through board and frame machine, filtrate, which imports fluid reservoir, can be used as leaching mine agent recycling, and filter residue is used for production magnesium sulfate, the ammonia of recycling
Water is recycled after reaching concentration as precipitating reagent.
5, extractant dissolution rare-earth products (or rare-earth sodium saponification organic phase): the rare-earth products clear water that step 3 is generated
It is slurred the mixing chamber for importing by pipeline and being placed with P507 in advance, compares 1:1(organic phase: slurry) mixing half an hour is carried out, so
Mixed phase imports clarifying chamber and is clarified afterwards, and upper organic phase is supported rare earth organic phase, uses for Rare Earth Separation, lower layer's water phase
Return is let down the use of native produce slurry.
6, remove aluminium: the slag that step 2 generates is transferred to alkali turning barrel after 3-4 times is recycled, and is sized mixing with clear water, liquid-solid ratio 2:1,
Then it is added solid sodium hydroxide, it is naoh concentration >=250g/l that addition amount of sodium hydroxide, which is subject to alkali swivel,.It is stirring
Under the conditions of, system temperature maintains 120 DEG C or more, reacts half an hour, then filters through plate and frame filter press, and filtrate is for recycling hydroxide
Aluminium uses, and return step 1 uses after filter residue is washed.
Claims (1)
1. a kind of south ion type rareearth ore rare-earth products intermediate processing, it is characterised in that: it the following steps are included:
(1), acid dissolution: taking the rareearth enriching material of total amount a quarter in sour decomposition bucket, adds clear water stirring to size mixing, is then added dropwise
The concentrated sulfuric acid carries out sour decomposition, and reaction end stablizes half an hour with pH=1, and then plus clear water is to standing, and filters through plate and frame filter press,
It is discarded after residue washing, filtrate is transferred to spare in another sour decomposition bucket；
(2), the filtrate of the rareearth enriching material of surplus 3/4ths and above-mentioned steps is mixed, and rareearth enriching material is gradually added
Enter, when material liquid pH to be mixed reaches 4.8-5.4, stir half an hour, material liquid pH adds rareearth enriching material when being not up to 5.4, adjust
PH stablizes in >=5.4 plate-frame filterings, and filtrate is transferred to settling box, and filter residue return step 1 carries out acid dissolution；
(3), rare-earth precipitation: under agitation to step (2) generate rare-earth liquid in be passed through concentration 5% ~ 10% ammonium hydroxide or
Ammonium bicarbonate soln carries out rare-earth precipitation, and precipitating terminal is pH >=7；Then it is filtered through plate and frame filter press, filtrate to fluid reservoir is stored up
It deposits, filter residue is spare after 3 ~ 5 times clear water agitator treatings；
(4), ammonium recovery ammonium hydroxide: magnesium oxide powder will be added in the filtrate after the precipitating of step (3) generation, after mixing evenly
It is pumped into jet-flow aeration tower with pump, cyclic aeration is carried out in >=80 DEG C of system, ammonia imports ammonia through top of tower venthole
Absorption tower carries out counter-current absorption with clear water, the NH in liquid after precipitating4 +Content filters after being lower than 50mg/l through board and frame machine, and filtrate is led
Enter fluid reservoir and can be used as leaching mine agent to be recycled, filter residue is used for production magnesium sulfate, and the ammonium hydroxide of recycling reaches after concentration as heavy
Shallow lake agent is recycled；
(5), extractant dissolves rare-earth products: the rare-earth products that step (3) generate being slurred with clear water, are put by pipeline importing
Have the mixing chamber of P507, organic phase: slurry carries out mixing half an hour compared to 1:1, and then mixed phase imports clarifying chamber and clarified,
Upper organic phase is supported rare earth organic phase, is used for Rare Earth Separation, and the return of lower layer's water phase is let down the use of native produce slurry；
(6), remove aluminium: the slag that step (2) generates is transferred to alkali turning barrel after 3-4 times is recycled, and is sized mixing with clear water, liquid-solid ratio 2:1,
Then it is added solid sodium hydroxide, it is naoh concentration >=250g/l that addition amount of sodium hydroxide, which is subject to alkali swivel,；It is stirring
Under the conditions of, system temperature maintains 120 DEG C or more, reacts half an hour, then filters through plate and frame filter press, and filtrate is for recycling hydroxide
Aluminium uses, and return step (1) uses after filter residue is washed.
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Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101260466A (en) * | 2007-02-08 | 2008-09-10 | 有研稀土新材料股份有限公司 | Pretreatment method for organic extracting agent and application thereof |
| CN102994750A (en) * | 2012-12-19 | 2013-03-27 | 南昌大学 | Rare earth saponification method of acidic complex extraction organic phase |
| CN107055569A (en) * | 2017-06-26 | 2017-08-18 | 孙东江 | A kind of comprehensive utilization process of liquid containing ammonium sulfate industrial wastewater |
| 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 |
| CN107434291A (en) * | 2017-09-05 | 2017-12-05 | 浙江南化防腐设备有限公司 | One kind reclaims high strength ammonia water system from ammonia nitrogen waste water |
| CN108396158A (en) * | 2018-02-24 | 2018-08-14 | 宁夏天元锰业有限公司 | A kind of processing method of the complex salt crystal object of electrolytic manganese process |
-
2019
- 2019-01-30 CN CN201910091387.9A patent/CN109628736A/en active Pending
Patent Citations (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101260466A (en) * | 2007-02-08 | 2008-09-10 | 有研稀土新材料股份有限公司 | Pretreatment method for organic extracting agent and application thereof |
| CN102994750A (en) * | 2012-12-19 | 2013-03-27 | 南昌大学 | Rare earth saponification method of acidic complex extraction organic phase |
| 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 |
| CN107055569A (en) * | 2017-06-26 | 2017-08-18 | 孙东江 | A kind of comprehensive utilization process of liquid containing ammonium sulfate industrial wastewater |
| CN107434291A (en) * | 2017-09-05 | 2017-12-05 | 浙江南化防腐设备有限公司 | One kind reclaims high strength ammonia water system from ammonia nitrogen waste water |
| CN108396158A (en) * | 2018-02-24 | 2018-08-14 | 宁夏天元锰业有限公司 | A kind of processing method of the complex salt crystal object of electrolytic manganese process |
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