CN107217139A - Southern ion type rareearth ore is without ammonia production practice - Google Patents

Southern ion type rareearth ore is without ammonia production practice Download PDF

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Publication number
CN107217139A
CN107217139A CN201710396017.7A CN201710396017A CN107217139A CN 107217139 A CN107217139 A CN 107217139A CN 201710396017 A CN201710396017 A CN 201710396017A CN 107217139 A CN107217139 A CN 107217139A
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rare earth
liquid
extraction
standby
tank
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孙东江
王志勇
王有霖
程哲
张�诚
林海
赵学付
王强
黄彬
朱健玲
邹志强
李钊
施展华
潘伟
袁宪强
陈国梁
黄凯龙
戴圣贤
杨阳
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Ganzhou Rare Earth Mining Technology Service Co Ltd
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Ganzhou Rare Earth Mining Technology Service Co Ltd
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    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/04Extraction of metal compounds from ores or concentrates by wet processes by leaching
    • C22B3/06Extraction 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
    • C22B3/08Sulfuric acid, other sulfurated acids or salts thereof
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/02Apparatus therefor
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/22Treatment or purification of solutions, e.g. obtained by leaching by physical processes, e.g. by filtration, by magnetic means, or by thermal decomposition
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B3/00Extraction of metal compounds from ores or concentrates by wet processes
    • C22B3/20Treatment or purification of solutions, e.g. obtained by leaching
    • C22B3/26Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
    • C22B3/38Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
    • C22B3/384Pentavalent phosphorus oxyacids, esters thereof
    • C22B3/3846Phosphoric acid, e.g. (O)P(OH)3
    • CCHEMISTRY; METALLURGY
    • C22METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
    • C22BPRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
    • C22B59/00Obtaining rare earth metals
    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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  • Chemical & Material Sciences (AREA)
  • Engineering & Computer Science (AREA)
  • Mechanical Engineering (AREA)
  • Geology (AREA)
  • General Life Sciences & Earth Sciences (AREA)
  • Manufacturing & Machinery (AREA)
  • Environmental & Geological Engineering (AREA)
  • Materials Engineering (AREA)
  • Life Sciences & Earth Sciences (AREA)
  • Metallurgy (AREA)
  • Organic Chemistry (AREA)
  • Geochemistry & Mineralogy (AREA)
  • Inorganic Chemistry (AREA)
  • Processing Of Solid Wastes (AREA)

Abstract

The southern ion type rareearth ore of the present invention is without ammonia production practice, in situ on the basis of leaching ore deposit technology, leaching ore deposit agent is used as using magnesium sulfate+sodium sulphate, sodium acid carbonate is as precipitating reagent output carbonated rare earth or uses the qualified high concentration rare earth feed liquid of the mode output of extraction for product, its process leaches rare earth for the agent diafiltration of leaching ore deposit, collect rare earth mother solution, magnesia is enriched with rare earth, sulfuric acid dissolution rareearth enriching material, rareearth enriching material this groove removal of impurities, sodium acid carbonate precipitating rare earth or extracting rare-earth, fundamentally avoid influence of the ammonia nitrogen to environment, make rareearth enriching material rapid precipitation using the characteristic of magnesia, sediment volume is small, the whole flow process time greatly shortens.

Description

Southern ion type rareearth ore is without ammonia production practice
Technical field
The present invention relates to Rare Earth Mine production practice, especially a kind of southern ion type rareearth ore is without ammonia production practice.
Background technology
The production practice that southern ion type rareearth ore is taken at present is that, as leaching ore deposit agent, ammonium hydrogen carbonate is made using ammonium sulfate [A1] precipitating reagent, its process leaches rare earth for the agent diafiltration of leaching ore deposit, collects rare earth mother solution, and ammonium hydrogen carbonate removal of impurities, clarification stands, put Go out supernatant and use ammonium bicarbonate precipitation again, then stand clarification ageing output carbonate rare earth, supernatant is returned can after acid adjustment Make the agent of leaching ore deposit to recycle.[A2] is protected massif vegetation by the way of in_situ leaching, well and avoids soil erosion; But it is numerous and diverse to there is process operation, and flow time is long, the shortcoming of big and unstable product quality is lost in rare earth recovery, while part sulphur The underground water and surface water on inorganization infiltration [A3] mining area periphery of sour ammonium leaching ore deposit agent have a certain impact.
The content of the invention
It is an object of the invention to provide a kind of operating efficiency is high, rare earth loss is small, process is simple, is avoided that ammonia and nitrogen pollution The southern ion type rareearth ore of environment is without ammonia production practice.
The southern ion type rareearth ore of the present invention comprises the following steps without ammonia production practice:
1st, rare earth is leached
Step a:The preparation of ore deposit agent is soaked, in 200m3Match somebody with somebody liquid pool in add 100m3Clear water, then adds 8-12 tons of epsom salts, Epsom salt all dissolvings, supplement clear water to 200m are made by stirring3, pH=4-5 is adjusted by the way that sulfuric acid is added dropwise;
Step b:The high-order liquid storage tank of massif, then passes through the difference of more than two where the leaching ore deposit agent of preparation is delivered into ore body The main pipeline in direction is delivered to the fluid injection well conduit being evenly arranged on ore body under natural pressure and carries out maceration, until ore body bottom Untill the pod apertures of arrangement go out liquid;
Step c:Top water supplement leaching ore deposit is made of pH=4-5 clear water on the basis of previous step, rare earth is collected by intercepting gutter female Liquid is to mother liquor collecting pit.
2nd, the enrichment of rare earth mother solution
Rare earth mother solution is put into enrichment pond, while being 1 liquid-solid ratio is mixed up in advance:1-3(Mass ratio)Magnesia slurry be put into Pond is enriched with, and is stirred, enrichment pond reclaimed water pH value of solution is maintained between 7-7.5, tests solution ph, it is terminal to reach 7.5, And stop plus magnesia slurry, 1-2 hours are stood, after after solution clarification, supernatant is discharged into standby with liquid pool.
3rd, sulfuric acid dissolution rareearth enriching material and alkali turn to remove aluminium
Step 1:The rareearth enriching material slurry that rare earth mother solution enriched substance is produced is transferred to plate and frame filter press press filtration, and filtrate is transferred to liquid Pond, filter residue is standby;
Step 2:The slag that previous step is produced is sized mixing, liquid-solid ratio 3-5:1, add what is mixed up in advance under conditions of stirring The dilute sulfuric acid progress acid of 5% concentration is molten, and sour molten terminal is stablized by pH=2.5 to be defined, and is then uniformly added into the dilute of previous step generation Soil enrichment slag is adjusted pH=5.2, is filtered by plate and frame filter press;
Step 3:Alkali turns to remove aluminium, and the filter residue that step 2 is produced is sized mixing, liquid-solid ratio 2:1, then add solid sodium hydroxide and carry out alkali Turn, the addition of alkali is defined by course of reaction pH stabilizations more than 13, plate-frame filtering,.
4th, precipitating rare earth product or extracting rare-earth product
Precipitating rare earth product:
Step 1:Determine the rare earth concentration of rare earth feed liquid;It is standard with≤5% to prepare sodium bicarbonate solution concentration;
Step 2:Sodium bicarbonate solution is added in rare earth feed liquid stirring while adding, during the continuous pH value for surveying solution reaction, Using pH=6.7-7 as the terminal of precipitation reaction, then filtered by plate and frame filter press, filter residue is transferred to kitchen sink agitator treating, solid-liquid Than 1:10, filtered after carbonate rare earth is stirred into slurry by plate and frame filter press, filtrate is discharged into liquid pool, and filter residue packaging is For carbonate rare-earth products.
The extracted products of rare earth feed liquid:
Step 1:2 extraction tank dislocation arrangements, higher than two grades of one-level bottom top inlet;One-level extraction tank top inlet is less than Two grades of extraction outlet at bottoms, less than 1 grade back extraction groove of two grades of back extraction grooves;
Step 2:The preparation of extractant, by 2.5m3P204With 2.5m3Sulfonated kerosene is well mixed standby respectively in 2 extraction tanks With;
Step 3:Rare earth feed liquid obtained by sulfuric acid dissolution rareearth enriching material is tested into rare earth concentration, by causing its rare earth with liquid Concentration balance is in 9.5-10.5g/L;
Step 4:The extraction of rare earth, by the rare earth feed liquid 4m of upper step3One-level extraction tank is imported into, is stirred while opening extraction tank Mix, mix 5 minutes, stopping stirring standing 5 minutes, treat that raffinate two grades of extraction tanks of importing extract instead after the completion of split-phase Should, incorporation time 5 minutes stands 5 minutes, and importing the agent of leaching ore deposit after raffinate after complete split-phase matches somebody with somebody liquid pool, and load organic phases are stayed in Extraction tank is standby;
Step 5:The back extraction of rare earth, by step 4 one-level extract load organic phases imported into back extraction groove in it is standby, lead simultaneously Enter the 8M hydrochloric acid 2m3 in the acid storage tank prepared in advance and be stirred well mixed, reaction 5 minutes, stand 5 minutes, treat that split-phase is complete It is after complete that 2 grades of back extraction grooves of top organic phase importing are standby, equally import 2m38M hydrochloric acid repetition one-level in two grades of back extraction grooves anti- Extraction tank program is stripped, and raffinate blank organic phase imports low level transfer pond, and it is standby to be delivered to 1 grade of extraction tank by pump, instead Extract stays in standby in back extraction groove.So 4 times repeatedly, imported into after 1 grade of anti-stripping agent rare earth concentration >=0.5M is measured Product material liquid tank is stored;2 grades of anti-stripping agents are standby by 1 grade of back extraction groove of low level transfer pond importing, it is heavy in two grades of back extraction grooves New importing 2m38M hydrochloric acid is standby.
The southern ion type rareearth ore of the present invention in situ on the basis of leaching ore deposit technology, uses sulfuric acid without ammonia production practice Magnesium+sodium sulphate is as leaching ore deposit agent, and output is qualified as precipitating reagent output carbonated rare earth or by the way of extraction for sodium acid carbonate High concentration rare earth feed liquid is product, and its process is that rare earth is leached in the agent diafiltration of leaching ore deposit, collects rare earth mother solution, magnesia is enriched with rare earth, Sulfuric acid dissolution rareearth enriching material, rareearth enriching material this groove removal of impurities, sodium acid carbonate precipitating rare earth or extracting rare-earth, are fundamentally avoided Influence of the ammonia nitrogen to environment, makes rareearth enriching material rapid precipitation, sediment volume is small, whole flow process using the characteristic of magnesia Time greatly shortens.
Embodiment
A kind of southern ion type rareearth ore comprises the following steps without ammonia production practice:
1st, rare earth is leached
Step a:The preparation of ore deposit agent is soaked, in 200m3Match somebody with somebody liquid pool in add 100m3Clear water, then adds 8-12 tons of epsom salts, Epsom salt all dissolvings, supplement clear water to 200m are made by stirring3, pH=4-5 is adjusted by the way that sulfuric acid is added dropwise;
Step b:The high-order liquid storage tank of massif, then passes through the difference of more than two where the leaching ore deposit agent of preparation is delivered into ore body The main pipeline in direction is delivered to the fluid injection well conduit being evenly arranged on ore body under natural pressure and carries out maceration, the soil according to ore body Side's amount is different and fluid injection quantity is different, and leaching ore deposit agent concentration is without adjustment, untill the pod apertures that ore body bottom is arranged go out liquid;
Step c:Top water supplement leaching ore deposit is made of pH=4-5 clear water on the basis of previous step, rare earth is collected by intercepting gutter female Liquid is to mother liquor collecting pit, and subsequently into the recycling step of rare earth, the top water of follow-up leaching ore deposit is with the supernatant of recovering rare earth process PH=4-5 is adjusted to circulate leaching ore deposit.
2nd, the enrichment of rare earth mother solution
(d)Facility is equipped with
Rare earth mother solution collecting pit:400m3, 1, bottom laying antiseepage film;Rare earth mother solution is enriched with pond:200m3, 2, lay bricks plus anti- Ooze cloth;With liquid pool:200m3, 2, lay bricks plus antiseepage cloth;Size-mixing tank:5m3, 1, cement pit band of laying bricks stirring;
Above pond is connected step by step with pipeline, and size-mixing tank is arranged in the middle of two enrichment ponds, and both sides enrichment pond is passed through with pipeline;
(e)Operating procedure
Rare earth mother solution collecting pit pipeline gate valve is opened, rare earth mother solution is put into by enrichment pond by pipeline, while handle is mixed up in advance It is 1 to starch liquid-solid ratio:1-3(Mass ratio)Magnesia slurry by pipeline be put into enrichment pond, by rare earth mother solution be enriched with pond in following Ring water pump is opened and is stirred, to ensure that enrichment pond reclaimed water pH value of solution is maintained between 7-7.5, until enrichment pond soon completely when stop Rare earth mother solution is put into, solution ph is tested, it is terminal to reach 7.5, and is stopped plus magnesia slurry, stands 1-2 hours, treats solution Supernatant is discharged into by pipeline by 200m after clarification3Standby with liquid pool, without playing slag, repeat the above steps operation, until enrichment Place standby when the quantity of slag reaches certain amount in pond.
3rd, sulfuric acid dissolution rareearth enriching material and alkali turn to remove aluminium
(f)Facility is equipped with
The molten bucket of acid:200m3Band stirring PP materials drum 3, alkali turning barrel:200m3Band stirring PP materials drum 2, rare earth feed liquid Storage pool:100m31, the pond of laying bricks of lined with PVC soft board, alkali turns feed liquid storage and reaction tank:50m3The stirring of glass inner-lining steel band Lay bricks 1, pond, plate and frame filter press:4, complex acid barrel:10m3Band stirring PP material buckets;
(g)Operating procedure
Step 1:The rareearth enriching material slurry that rare earth mother solution enriched substance is produced is transferred to plate and frame filter press press filtration by pump, and filtrate turns Enter to match somebody with somebody liquid pool, filter residue is transferred to standby in sour molten bucket;
Step 2:The slag that previous step is produced is sized mixing, liquid-solid ratio 3-5:1, added in advance by pipeline under conditions of stirring The dilute sulfuric acid progress acid of 5% concentration first mixed up is molten, and sour molten terminal is stablized by pH=2.5 to be defined, and is then uniformly added into previous step The rare-earth enrichment slag of generation is adjusted pH=5.2, is filtered by plate and frame filter press, and solution imports rare earth feed liquid by pipeline and stored up Deposit pond standby, filter residue is transferred to standby in alkali turning barrel;
Step 3:Alkali turns to remove aluminium, and the filter residue that step 2 is produced is sized mixing in alkali turning barrel, liquid-solid ratio 2:1, then add solid hydrogen-oxygen Change sodium and carry out alkali turn, the addition of alkali is defined by course of reaction pH stabilizations more than 13, and plate-frame filtering, filtrate is transferred to by pipeline It is standby that alkali turns feed liquid storage pool, and filter residue, which returns to sour molten bucket and makes adjustments pH, to be used.
4th, precipitating rare earth product or extracting rare-earth product
Scheme one:Precipitating rare earth product
(1)Facilities and equipment
Sedimentation basin:50m3The lay bricks cement pit 1, kitchen sink of Corrosion Protection of Fiber Reinforced Plastics with stirring:50m3Fiberglass with stirring is prevented Rotten lay bricks cement pit 1, plate and frame filter press:2, sodium acid carbonate matches somebody with somebody liquid pool:20m3Cement pit of laying bricks with stirring;
(2)Operating procedure
Step 1:Rare earth feed liquid in rare earth feed liquid storage pool is piped to standby in sedimentation basin, measure rare earth concentration, Sedimentation basin material liquid volume is determined with rare earth concentration;
Step 2:Sodium acid carbonate is prepared, and input solid sodium bicarbonate is some in sodium acid carbonate matches somebody with somebody liquid pool, is then added clear water and is stirred Mix, the sodium bicarbonate solution concentration of preparation is standard with≤5%;
Step 3:The sedimentation basin of step 1 is opened into stirring, it is molten to be put into the sodium acid carbonate that step 2 prepares by pipeline while stirring Liquid, during the continuous pH value for surveying solution reaction, using pH=6.7-7 as the terminal of precipitation reaction, then pass through plate and frame filter press mistake Filter, filtrate is discharged into the agent of leaching ore deposit and matches somebody with somebody liquid pool, and filter residue is transferred to kitchen sink agitator treating(Solid-to-liquid ratio 1:10), treat that carbonate rare earth is stirred entirely It is uniform into being filtered by plate and frame filter press after slurry, filtrate is discharged into liquid pool, and filter residue packaging is carbonate rare-earth products.
Scheme two:The extracted products of rare earth feed liquid
1. facilities and equipment
Extraction tank:10m3Mixing cell-type single-stage extraction tank with stirring(PVC materials)2;Reactive tank:5m3Drum with stirring (PVC materials)2;Extractant high position storage tank:10m3Glass steel material round can, outlet at bottom, upper inlet, 1;Feed liquid is high-order Measuring tank:5m3Glass steel material round can, outlet at bottom, upper inlet, 1;Acid storage tank:20m31, glass steel material tank;Finished product Material liquid tank:50m31, glass steel material tank;Low level transfer pond:10m3Cement is laid bricks, and serves as a contrast PVC board 2;
2. operating procedure
Step 1:2 extraction tank dislocation arrangements, higher than two grades of one-level bottom top inlet.One-level extraction tank top inlet is less than Two grades of extraction outlet at bottoms.Less than 1 grade back extraction groove of two grades of back extraction grooves;
Step 2:The preparation of extractant.By 2.5m3P204With 2.5m3Sulfonated kerosene is well mixed standby respectively in 2 extraction tanks With;
Step 3:Rare earth feed liquid obtained by sulfuric acid dissolution rareearth enriching material is tested into rare earth concentration, by causing its rare earth with liquid Then concentration balance imports the high-order measuring tank of feed liquid standby in 10g/L or so by conveyance conduit;
Step 4:The extraction of rare earth.By the rare earth feed liquid 4m in step 3 measuring tank3One-level extraction tank is imported into by pipeline, together Shi Kaiqi extraction tanks are stirred, and are mixed 5 minutes, stop stirring, are stood 5 minutes, are treated to lead raffinate by pipeline after the completion of split-phase Enter two grades of extraction tanks and carry out extractive reaction, incorporation time 5 minutes stands 5 minutes, and leaching ore deposit agent is imported after raffinate after complete split-phase With liquid pool, it is standby that load organic phases stay in extraction tank;
Step 5:The back extraction of rare earth.By step 4 one-level extract load organic phases imported into back extraction groove in it is standby, lead simultaneously Enter the 8M hydrochloric acid 2m3 in the acid storage tank prepared in advance and be stirred well mixed, reaction 5 minutes, stand 5 minutes, treat that split-phase is complete It is after complete that 2 grades of back extraction grooves of top organic phase importing are standby, grooves are stripped at two grades and equally import 2m3,8M hydrochloric acid repetition one-level Back extraction groove program is stripped, and raffinate blank organic phase imports low level transfer pond, is delivered to 1 grade of extraction tank by pump standby. Anti-stripping agent stays in standby in back extraction groove, so repeatedly 4 times, the importing after 1 grade of anti-stripping agent rare earth concentration >=0.5M is measured Finished product material liquid tank is stored;2 grades of anti-stripping agents are standby by 1 grade of back extraction groove of low level transfer pond importing, in two grades of back extraction grooves Again 2m3,8M hydrochloric acid are imported standby.

Claims (3)

1. a kind of southern ion type rareearth ore is without ammonia production practice, it is characterised in that:It comprises the following steps:
(1), rare earth leach
Step a:The preparation of ore deposit agent is soaked, in 200m3Match somebody with somebody liquid pool in add 100m3Clear water, then adds 8-12 tons of epsom salts, Epsom salt all dissolvings, supplement clear water to 200m are made by stirring3, pH=4-5 is adjusted by the way that sulfuric acid is added dropwise;
Step b:The high-order liquid storage tank of massif, then passes through the difference of more than two where the leaching ore deposit agent of preparation is delivered into ore body The main pipeline in direction is delivered to the fluid injection well conduit being evenly arranged on ore body under natural pressure and carries out maceration, until ore body bottom Untill the pod apertures of arrangement go out liquid;
Step c:Top water supplement leaching ore deposit is made of pH=4-5 clear water on the basis of previous step, rare earth is collected by intercepting gutter female Liquid is to mother liquor collecting pit;
(2), rare earth mother solution enrichment
Rare earth mother solution is put into enrichment pond, while being 1 liquid-solid ratio is mixed up in advance:1-3 magnesia slurry is put into enrichment pond, and It is stirred, tests solution ph, it is terminal to reach 7.5, and is stopped plus magnesia slurry, stands 1-2 hours, treats that solution is clarified Afterwards, supernatant is discharged into standby with liquid pool;
(3), sulfuric acid dissolution rareearth enriching material and alkali turns to remove aluminium
Step d:The rareearth enriching material slurry that rare earth mother solution enriched substance is produced is transferred to plate and frame filter press press filtration, and filtrate is transferred to liquid Pond, filter residue is standby;
Step e:The slag that previous step is produced is sized mixing, liquid-solid ratio 3-5:1, add what is mixed up in advance under conditions of stirring The dilute sulfuric acid progress acid of 5% concentration is molten, and sour molten terminal is stablized by pH=2.5 to be defined, and is then uniformly added into the dilute of previous step generation Soil enrichment slag is adjusted pH=5.2, is filtered by plate and frame filter press;
Step f:Alkali turns to remove aluminium, and the filter residue that previous step is produced is sized mixing, liquid-solid ratio 2:1, then add solid sodium hydroxide and enter Row alkali turns, and the addition of alkali is defined by course of reaction pH stabilizations more than 13, plate-frame filtering;
(4), precipitating rare earth product or extracting rare-earth product.
2. southern ion type rareearth ore according to claim 1 is without ammonia production practice, it is characterised in that:Described precipitation is dilute Native produce step is as follows:
Step(1):Determine the rare earth concentration of rare earth feed liquid;It is standard with≤5% to prepare sodium bicarbonate solution concentration;
Step(2):Sodium bicarbonate solution is added in rare earth feed liquid stirring while adding, during the continuous pH for surveying solution reaction Value, using pH=6.7-7 as the terminal of precipitation reaction, is then filtered, filter residue is transferred to kitchen sink agitator treating by plate and frame filter press, Solid-to-liquid ratio 1:10, filtered after carbonate rare earth is stirred into slurry by plate and frame filter press, filtrate is discharged into liquid pool, filter residue bag Dress is carbonate rare-earth products.
3. southern ion type rareearth ore according to claim 1 is without ammonia production practice, it is characterised in that:Described extraction is dilute Native produce step is as follows:
Step(1):2 extraction tank dislocation arrangements, higher than two grades of one-level bottom top inlet;One-level extraction tank top inlet is low Outlet at bottom, less than 1 grade back extraction groove of two grades of back extraction grooves are extracted in two grades;
Step(2):The preparation of extractant, by 2.5m3P204With 2.5m3Sulfonated kerosene is well mixed standby respectively in 2 extraction tanks With;
Step(3):Rare earth feed liquid obtained by sulfuric acid dissolution rareearth enriching material is tested into rare earth concentration, by causing its dilute with liquid Native concentration balance is in 9.5-10.5g/L;
Step(4):The extraction of rare earth, by the rare earth feed liquid 4m of upper step3One-level extraction tank is imported into, is stirred while opening extraction tank Mix, mix 5 minutes, stopping stirring standing 5 minutes, treat that raffinate two grades of extraction tanks of importing extract instead after the completion of split-phase Should, incorporation time 5 minutes stands 5 minutes, and importing the agent of leaching ore deposit after raffinate after complete split-phase matches somebody with somebody liquid pool, and load organic phases are stayed in Extraction tank is standby;
Step(5):The back extraction of rare earth, by step(4)One-level extraction load organic phases imported into back extraction groove in it is standby, together When the 8M hydrochloric acid 2m3 that imports in the acid storage tank for preparing in advance be stirred well mixed, react 5 minutes, stand 5 minutes, treat point It is after phase is complete that 2 grades of back extraction grooves of top organic phase importing are standby, grooves are stripped at two grades and equally import the repetition of 2m3,8M hydrochloric acid One-level back extraction groove program is stripped, and raffinate blank organic phase imports low level transfer pond, is delivered to 1 grade of extraction tank by pump standby Stayed in standby in back extraction groove, so repeatedly 4 times, led after 1 grade of anti-stripping agent rare earth concentration >=0.5M is measured with, anti-stripping agent Enter the storage of finished product material liquid tank.
CN201710396017.7A 2017-05-31 2017-05-31 Southern ion type rareearth ore is without ammonia production practice Pending CN107217139A (en)

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Cited By (12)

* Cited by examiner, † Cited by third party
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CN108034842A (en) * 2017-12-06 2018-05-15 五矿勘查开发有限公司 Ion type rareearth ore is without the environmentally protective production practice of ammoniumization
CN108486373A (en) * 2018-07-01 2018-09-04 广西那神晞途环保科技有限公司 ionic mineral precipitation agent and preparation method thereof
CN108486374A (en) * 2018-07-01 2018-09-04 广西那神晞途环保科技有限公司 Minerals environmental protection rare-earth precipitation agent and preparation method thereof
CN108707749A (en) * 2018-07-01 2018-10-26 广西那神晞途环保科技有限公司 Special precipitating reagent of ionic minerals separation factory and preparation method thereof
CN108821307A (en) * 2018-07-16 2018-11-16 孙东江 Ammonium ion recovery method is remained in ore body after ion adsorption type rare earth ore exploitation
CN108893606A (en) * 2018-08-30 2018-11-27 江西理工大学 Precipitating, removal of impurities, middling recurrence extract the method without rare earth in ammonium rare earth mother solution
CN108893607A (en) * 2018-08-30 2018-11-27 江西理工大学 Substep impurity-removing precipitating recycles the method without rare earth in ammonium rare earth mother solution
CN109628736A (en) * 2019-01-30 2019-04-16 赣州稀土开采技术服务有限公司 A kind of south ion type rareearth ore rare-earth products intermediate processing
CN110607442A (en) * 2019-10-14 2019-12-24 中铝广西有色稀土开发有限公司 Method for applying heavy saponification removal wastewater to rare earth in-situ leaching
CN115417535A (en) * 2022-11-07 2022-12-02 矿冶科技集团有限公司 Method for enriching and recycling leaching tail water of ionic rare earth mine ammonium salt leaching field
CN115522080A (en) * 2022-10-11 2022-12-27 江西立源环境技术有限公司 High-power membrane concentration extraction process for mine mother liquor
CN115896489A (en) * 2021-08-25 2023-04-04 中国科学院江西稀土研究院 Method for enriching rare earth from rare earth leaching mother liquor

Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104561614A (en) * 2015-01-29 2015-04-29 赣州稀土矿业有限公司 Process for recycling rare earth from south ion adsorption type rare earth ore leaching mother liquor
CN105506287A (en) * 2016-01-13 2016-04-20 龙南县锦易矿业有限公司 Process for recycling rare earth from Southern rare earth ore through leached mother liquor precipitation method
CN105838881A (en) * 2016-06-12 2016-08-10 孙东江 South ionic rare earth ore leaching liquid impurity removing process
CN105907959A (en) * 2016-05-16 2016-08-31 龙南县锦易矿业有限公司 Ammonia-free mining method for rare earth ore in south China

Patent Citations (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN104561614A (en) * 2015-01-29 2015-04-29 赣州稀土矿业有限公司 Process for recycling rare earth from south ion adsorption type rare earth ore leaching mother liquor
CN105506287A (en) * 2016-01-13 2016-04-20 龙南县锦易矿业有限公司 Process for recycling rare earth from Southern rare earth ore through leached mother liquor precipitation method
CN105907959A (en) * 2016-05-16 2016-08-31 龙南县锦易矿业有限公司 Ammonia-free mining method for rare earth ore in south China
CN105838881A (en) * 2016-06-12 2016-08-10 孙东江 South ionic rare earth ore leaching liquid impurity removing process

Cited By (14)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN108034842A (en) * 2017-12-06 2018-05-15 五矿勘查开发有限公司 Ion type rareearth ore is without the environmentally protective production practice of ammoniumization
CN108486373A (en) * 2018-07-01 2018-09-04 广西那神晞途环保科技有限公司 ionic mineral precipitation agent and preparation method thereof
CN108486374A (en) * 2018-07-01 2018-09-04 广西那神晞途环保科技有限公司 Minerals environmental protection rare-earth precipitation agent and preparation method thereof
CN108707749A (en) * 2018-07-01 2018-10-26 广西那神晞途环保科技有限公司 Special precipitating reagent of ionic minerals separation factory and preparation method thereof
CN108821307B (en) * 2018-07-16 2021-06-11 孙东江 Method for recovering residual ammonium ions in ore body after mining of ion adsorption type rare earth ore
CN108821307A (en) * 2018-07-16 2018-11-16 孙东江 Ammonium ion recovery method is remained in ore body after ion adsorption type rare earth ore exploitation
CN108893606A (en) * 2018-08-30 2018-11-27 江西理工大学 Precipitating, removal of impurities, middling recurrence extract the method without rare earth in ammonium rare earth mother solution
CN108893607A (en) * 2018-08-30 2018-11-27 江西理工大学 Substep impurity-removing precipitating recycles the method without rare earth in ammonium rare earth mother solution
CN109628736A (en) * 2019-01-30 2019-04-16 赣州稀土开采技术服务有限公司 A kind of south ion type rareearth ore rare-earth products intermediate processing
CN110607442A (en) * 2019-10-14 2019-12-24 中铝广西有色稀土开发有限公司 Method for applying heavy saponification removal wastewater to rare earth in-situ leaching
CN115896489A (en) * 2021-08-25 2023-04-04 中国科学院江西稀土研究院 Method for enriching rare earth from rare earth leaching mother liquor
CN115522080A (en) * 2022-10-11 2022-12-27 江西立源环境技术有限公司 High-power membrane concentration extraction process for mine mother liquor
CN115417535A (en) * 2022-11-07 2022-12-02 矿冶科技集团有限公司 Method for enriching and recycling leaching tail water of ionic rare earth mine ammonium salt leaching field
CN115417535B (en) * 2022-11-07 2023-01-31 矿冶科技集团有限公司 Method for enriching and recycling leaching tail water of ionic rare earth mine ammonium salt leaching field

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Application publication date: 20170929