CN1935658A - Method for producing chlorinated rare earth by decomposing and mixing rare earth headings using calcination of ammonia chloride - Google Patents
Method for producing chlorinated rare earth by decomposing and mixing rare earth headings using calcination of ammonia chloride Download PDFInfo
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- CN1935658A CN1935658A CN 200610159473 CN200610159473A CN1935658A CN 1935658 A CN1935658 A CN 1935658A CN 200610159473 CN200610159473 CN 200610159473 CN 200610159473 A CN200610159473 A CN 200610159473A CN 1935658 A CN1935658 A CN 1935658A
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Abstract
The invention relates to a method of producing rare-earth chloride by resolving mixed rare-earth concentrate with ammonium chloride baking process, especially a method of producing rare-earth chloride by baking Baotou mixed rare-earth concentrate with ammonium chloride, belonging to rare-earth metal smeling technical field. And it mixes ammonium chloride, ammonium sulfate, activated SiO2, charcoal (use petroleum coke in industrial production) and mixed rare-earth concentrate, feeds their mixture into a furnace for baking, preserves heat at initial 300-400 deg.C for 1-3 h, raises temperature to 450-600 deg.C within 30 min and preserves heat for 1-2 h, discharges and water-leaches, neutralizes the water- leaching solution to remove thorium, settles and filters, and obtains rare-earth chloride solution after purification. And it can recover waste water and waste gas for synthetic utilization.
Description
One, technical field
The present invention relates to a kind of method of producing chlorinated rare earth by decomposing and mixing rare earth headings using calcination of ammonia chloride, belong to the rare earth metal technical field of smelting.
Two, background technology
Mixed rare earth concentrate is that packet header, inner mongolia baiyuneboite selects the iron byproduct, mainly is made of hamartite and solitary stone ore, answers the singularity hamartite pre-treating technology of its mineral composition similar.Its treatment process is mainly contained vitriol oil method, soda processes, soda ash method, high-temperature chlorination, oxidizing roasting method, ammonium chloride roasting method etc.Domestic existing main vitriol oil method and two kinds of processing methodes of soda processes of adopting are handled the mixed rear earth concentrate.The vitriol oil genealogy of law adopts vitriol oil roasting at high temperature to decompose mixed rare earth concentrates and generates water-solubility rare-earth vitriol, through water logging removal of impurities abstraction and type-reverting or carbon ammonium precipitation through the dissolving with hydrochloric acid removal of impurities concentrate mixed chlorinated rare earth, the greatest problem that this method exists is the hydrogen fluoride (HF) of roasting process discharge, the tail gas pollution of sulphur oxygen (SO), and control expense is high; The disposal of a large amount of low-activity water logging slags and the discharging of acidic and alkaline waste water etc.The caustic soda genealogy of law adopts concentrated caustic (NaOH) pyrolytic decomposition concentrate to generate the rare earth hydrate slip, through impurity such as washing defluorination phosphorus, the excellent molten re chloride that gets of hydrochloric acid, concentrate preparation rare earth chloride product through removal of impurities again, the greatest problem that this method exists is only to be applicable to the higher-grade concentrate, production cost is higher, and discharged volume of industrial waste water is big, the pollution abatement costs height.For solving the pollution problem of mixed rare earth concentrate production environment, at vitriol oil method propose many low-temperature bakes decompose the mixed rare earth concentrate Chinese invention patents (application number: 98118153.8, application number: 021444405.6, application number: 200410006443.8, application number: 200610005695.8, solve the pollution problem that thorium radiocontamination and fluorine enter waste water in the slag.Propose fluorine carbon cerium raw ore is levigate in the Chinese invention patent " a kind of ammonium chloride hamartite roasting method is decomposed the method that hamartite reclaims carbonated rare earth " (patent No. ZL991061497), evenly mixed in ammonium chloride and calcium chloride grinding then, roasting 0.5～3 hour.Make the rare earth in the mineral change into rare earth chloride.The husky stirring in hot water of roasting leached, and filtration washing obtains the rare earth leaching liquid.Adopt the ammonium bicarbonate precipitation rare earth, drying obtains the carbonated rare earth product after filtration.The medium people of Tsing-Hua University's eight-legged essay further extracts rare earth with the ammonium chloride roasting after proposing " the ammonium chloride roasting method reclaims rare earth from mixed rare earth concentrate " (the 32nd the 4th phase of volume of He'nan University's journal) employing magnesium oxide and the solid fluorine of mixed rare earth concentrate mixing roasting.Calcium salt content height in the rare earth, the rate of recovery of rare earth is only 85%.This method must leach rare earth chloride with hot water.
Three, summary of the invention
The technical problem that the present invention solves is: efficiently solve "dead" waste residue, waste water, exhaust gas discharging in the rare earth leaching process, and " waste water, waste gas " can be reclaimed, make full use of in producing again, realize comprehensive utilization, no waste water is discharged in the production process, has improved the rate of recovery of rare earth, one time yield reaches more than 95%, technology is simple, and is with short production cycle, and manufacturing expense is low.
Technical solution:
The present invention adopts ammonium chloride, ammonium sulfate, active silica, carbon to mix with mixed rare earth concentrates, go into the stove roasting, initial 300～400 ℃ of insulations 1～3 hour, in 30 minutes, rise to 450～600 ℃ of insulations water logging of coming out of the stove after 1～2 hour, with heavy clear, the filtration of infusion, obtain re chloride after the purification.Water logging filter residue after the filtration embathes with 0.5～1N dilute hydrochloric acid, adds the quantity of slag and be 2% NH
4F is heated with stirring to 75～100 ℃, insulated and stirred 60～120 minutes, heavy clear, filtration, drip washing, residue, hydrochloric acid washing filtrate, the hydrochloric acid washing filtrate is returned in the above-mentioned water logging operation.
The ammonium chloride roasting mixed rare earth concentrates that the present invention proposes is produced the method for rare earth chloride, may further comprise the steps:
(1) ammonium chloride, ammonium sulfate, active silica, carbon are mixed with mixed rare earth concentrates, its ratio is: mixed rare earth concentrates: ammonium chloride: ammonium sulfate: active silica: charcoal=1: 0.7～1.5: 1: 0.1～0.5: 1: 0.02～0.1: 1: 0.1～0.5;
(2) material that mixes is put into iron pan, goes into the stove starting temperature: 300～400 ℃, be incubated 1～3 hour, and temperature rises to 450～600 ℃ in 30-90 minute, is incubated and comes out of the stove the gas cooling of generation, recycling after 1～2 hour;
(3) expect that the water that adds 3 times is heated to 65～95 ℃ after the burning after will coming out of the stove, add hydrochloric acid and transfer to PH=0.5～1 that water logging was stirred 60-90 minute, filtrate adds 10% barium chloride solution and removes SO
4 -2Stir, heavy clear, filtration, drip washing, leach liquor;
(4) above-mentioned leach liquor is heated to 80～85 ℃, stirring adds ammonium bicarbonate solution and transfers PH=4.5～5, and it is heavy after clear 2-3 hour to stir after 15 minutes, filters drip washing, gets rare earth chloride clear liquid and rich thorium slag;
(5) the water logging filter residue in the step (3) is embathed with 0.5～1N dilute hydrochloric acid, add the quantity of slag and be 2% NH
4F is heated with stirring to 75～100 ℃, insulated and stirred 60～120 minutes, heavy clear, filtration, drip washing, residue, pickling filtrate, pickling filtrate is returned in the water logging operation of step (3);
(6) the rare earth chloride clear liquid is produced single rare earth oxide or concentrated crystallisation by cooling for extracting and separating, gets solid rare earth chloride product;
(7) with the rare earth chloride clear liquid in the step (4) in extraction separation process, the waste water in the carbon ammonium precipitation of generation, with through evaporation, concentrate the ammonium chloride obtain and be used for roasting.
Mixed rare earth concentrates also can mix with carbon, active silica, industrial boric acid, its proportioning is: mixed rare earth concentrates RE0: carbon: active silica: industrial boric acid=1: 0.3～0.5: 1: 0.1～0.5: 1: 0.2～0.3, go into the stove starting temperature: 600～850 ℃, roasting 3～4 hours.
Carbon can be charcoal, coal dust or refinery coke.
The product analysis result is as follows:
Composition REO Fe
2O
3CaO+MgO SO
4 -2SiO
2ThO
2
Content % 〉=45.2＜0.01＜2.3＜0.03＜0.05 trace
The rare earth total recovery is greater than 95%, and quality is up to state standards.
The present invention reaches on-radiation waste sludge discharge standard for making waste residue, purify through the dilute hydrochloric acid method of soaking through water logging slag: REO＜2%, ThO
2＜0.003% residue.
The present invention adopts the main chemical reaction of ammonium chloride roasting mixed rare earth concentrates as follows:
REFCO
3+3NH
4Cl+C+O
2→RECl
3+(NH
4)
2CO
3↑+NHF↑+CO
2↑
3CaF
2+2(NH
4)
2SO
4+SiO
2nH
2O+2C+2O
2→
2CaSO
4+CaSiF
6+2(NH
4)
2CO
3↑+nH
2O↑
ThO
2+2(NH
4)
2SO
4→Th(SO
4)
2+4NH
3↑+2H
2O
REPO
4+3NH
4Cl+1/2C+1/2O
2→RECl
3+(NH
4)
3PO
4+1/2CO
2↑
Fe
2O
3+6NH
4Cl+3C+3/2O
2→2FeCl
3+3(NH
4)
2CO
3↑
FeCl
3+(NH
4)
3PO
4→FePO
4+3NH
4Cl
Material therefor of the present invention and effect:
Ammonium chloride: be the main chemical materials of this technology, can derive from when producing single rare earth oxide Wastewater Recovery in the carbon ammonium precipitation process.This material by working in coordination with under given temperature of other material, is converted into water-soluble salt with insoluble rare earth fluoro carbonate with after mixed rare earth concentrate mixes.
Ammonium sulfate: the calcium salt in the concentrate transfers the excessive decomposition of separating and control ammonium chloride that calcium sulfate reaches calcium and rare earth to.
Solvable active SiO
2: the water glass (liquid) with high-module forms by chemical process.Its purposes is: (1) is tackiness agent during agglomerate behind batch mixing; (2) decomposition of conduct " accepting agent of fluorine " promotion fluoro carbonate in the reaction process of roasting of heating improves rate of decomposition.
Carbon: can make rare earth oxide in the free energy variable of chlorine reaction less than zero, and the carrying out of in 350 ℃～500 ℃ temperature, accelerating the rare-earth chlorination reaction.
The method of producing chlorinated rare earth by decomposing and mixing rare earth headings using calcination of ammonia chloride of the present invention possesses following characteristics:
(1) technology is simple, and is with short production cycle, is 1/3rd of the caustic soda method prepared rare earth chloride production cycle.
(2) " waste water " that can contain ammonium chloride when producing single rare earth oxide in the carbon ammonium precipitation process reclaims, and makes full use of in producing again, realizes comprehensive utilization.
(3) manufacturing expense is low, and a materials consumption expense just reduces more than 1000 yuan than " caustic soda method " product per ton.
(4) waste gas that produces in the calcining process in this technology is Neutral ammonium fluoride, ammonium chloride, volatile salt.Receive method with condensation and recycle easily, the simple investment cost of receiving equipment is low; Thorium in the mixed rear earth concentrate has been carried out enrichment, made a large amount of waste residues reach on-radiation waste sludge discharge standard; There is not waste water in the production process.
(5) take plant capacity little (wet processing), reduce facility investment, design identical industrial scale, comparable " caustic soda method " reaches " sulfuric acid process " and reduces by 1/2nd facility investment.
(6) because of not using strong acid and strong base in process of production, thus help labour protection and equipment guarantee prolongation equipment usage period, and safety in production.
Four, description of drawings
Accompanying drawing is a process flow sheet of the present invention;
Five, embodiment
Embodiment 1: take by weighing Baotou rare earth ore concentrate RE050% 100 gram (drying), (NH
4)
2S0
430 grams, NH
4Cl100 gram, n SiO
2NH
2O15 gram (n=2-10, contains SiO
23 grams), charcoal 20 gram (pulverizing the 100-200 order), water is mixed thoroughly and is the mud shape.(150 * 120 * 60m/m) compactings when muffle furnace rises to 340 ℃, are put into stove, have white cigarette to emerge after 40 minutes, are ammonia flavor, are placed on fire door with the test paper of PH1～14 and test PH=10 in stitching, and are incubated and come out of the stove after 90 minutes to put into iron pan.It is cellular to expect to be taupe after burning, net weight 133 grams.It is burnt the back material put into the 500ml container, add water 300ml, 85 ℃ of stirring heating, PH=3.5 drips with technical hydrochloric acid and to transfer to PH=0.5～1, and insulated and stirred was used 10%BaCl after 90 minutes
2Solution removes SO
4 -2, stir after 10 minutes and sank clear 30 minutes, vacuum filtration drip washing.Get filtrate 400ml, rare earth concentration 121.75g/l; Leaching yield 97.20%.Wet filter residue: net weight 54.5 grams.The water logging cleaner liquid is heated to adds 15% industrial carbonic acid hydrogen ammonium solution under 85 ℃ the agitation condition at leisure and transfer to PH=4～4.5, stir quiet putting 2 hours after 15 minutes, promptly carry out vacuum filtration drip washing.Get rare earth chloride clear liquid 480ml.Rare earth concentration 99.48g/l, a yield 95.31%.Get rich thorium slag weight in wet base 5.5 grams, REO17.27%, ThO
230.14%.For making waste residue reach on-radiation waste sludge discharge standard, this process using has been carried out dilute hydrochloric acid with a water logging slag and has been embathed, and then the hydrochloric acid washing filtrate is returned to be used for new water logging operation of burning back material next time.Water logging filter residue 54.5 grams (weight in wet base) are put into the 1N dilute hydrochloric acid that beaker adds 150ml, add 1 gram NH
4F is heated with stirring to 85～90 ℃, insulated and stirred 90 minutes, the heavy clear drip washing of filtering.Get filtrate 210ml, rare earth concentration REO3.10g/l; Get residue 50,6 grams (weight in wet base), REO1.98%, ThO
2Content less than 0.003%.
Embodiment 2: get and produce single rare earth oxide " waste water " 20 liters behind carbon ammonium precipitation, NH
4Cl concentration 61.2g/l (calculating) by 60%.Get " waste water " 4000ml, evaporation concentration stops evaporation, promptly in order to spice (NH when being evaporated near 350ml
4Cl is 240 grams).With 200 gram rare earth ore concentrates, 50 gram (NH
4)
2SO
4, wood charcoal powder 50 gram, active SiO
2NH
2O (presses SiO
2Metering) 12 grams have the NH of moisture with above-mentioned pasty state
4Cl mixes (being the lump thing after the cooling) thoroughly. will mix the iron pan compacting that uniform product is put into two same sizes respectively then, one is dropped in the burner hearth, be warming up to 340～350 ℃ of insulations 2 hours, rise to 500～550 ℃ of insulations again after 2 hours, the blowing out cooling was come out of the stove after 2 hours.Burn back material net weight 271 grams, divide equally two parts of each 135.5 grams.Get a back material (135.5 gram) that burns and put into container, dilute hydrochloric acid is embathed the filtrate 210ml of a water logging slag, add 100ml water and pour vessel in heating into and stir, be incubated 85～90 ℃ of BaCl that stir addings 10% in 2 hours
2Solution removes SO
4 -2, restir heavy after-filtration drip washing in clear 30 minutes in 10 minutes gets filtrate 420ml, filter residue 55 grams (weight in wet base).Again filter residue is added 1N dilute hydrochloric acid 150ml and 1 gram NH
4F is incubated 85～90 ℃ of stirrings and embathes, the heavy clear drip washing of filtering after 90 minutes, get pickling filtrate 230ml, residue 50 gram (weight in wet base) can leach the filtrate 100ml water of pickling slag after rare material 135.5 grams after another part burning again, and the same insulation is stirred for 85～90 ℃ and added BaCl in 2 hours
2Solution removes SO
4 -2., the heavy clear drip washing of filtering.Get immersion liquid and last a immersion liquid merging 800ml altogether, REO122.74%, leaching yield 98%; The filter residue of leaching carries out the dilute hydrochloric acid pickling with identical technical qualification, filters to such an extent that residue restrains (weight in wet base), REO1.87% with last a residue merging 107.5; ThO＜0.003%.Pour this twice leach liquor 800ml vessel in heating to 80～85 ℃ of 1000ml into, stir and add ammonium bicarbonate solution and transfer PH=4.5, it is heavy after clear 3 hours to stir after 15 minutes, filters drip washing, gets rare earth chloride clear liquid 1000ml; Rare earth concentration REO96.39%, a yield 96.2% gets rich thorium slag (weight in wet base) 10.5 grams, REO17.16%, ThO30.15%.
Embodiment 3
Take by weighing Baotou rare earth ore concentrate REO50%100 gram, add carbon dust 50 grams, active SiO
23 grams, industrial boric acid 15 grams after mixing, are put into iron pan, go into stove, under 600-850 ℃ temperature condition, come out of the stove after roasting 3-4 hour.Burn the back material and be reddish brown powder thing, net weight 109.5 grams with burning stirrings of sizing mixing of water that the back material adds 3 times, are heated to 80-90 ℃, add dilute hydrochloric acid, remain on PH=0.5-1, and insulated and stirred is after 3 hours, heavy clearly, filtration, drip washing.Back prologue after the roasting is with embodiment 1.
Claims (4)
1, the method for producing chlorinated rare earth by decomposing and mixing rare earth headings using calcination of ammonia chloride is characterized in that, this method comprises the following steps:
(1) ammonium chloride, ammonium sulfate, active silica, carbon are mixed with mixed rare earth concentrates, its ratio is: mixed rare earth concentrates: ammonium chloride: ammonium sulfate: active silica: carbon=1: 0.7～1.5: 1: 0.1～0.5: 1: 0.02～0.1: 1: 0.1～0.5;
(2) material that mixes is put into iron pan, goes into the stove starting temperature: 300～400 ℃, be incubated 1～3 hour, and temperature rises to 450～600 ℃ in 30-90 minute, is incubated and comes out of the stove the gas cooling of generation, recycling after 1～2 hour;
(3) expect that the water that adds 3 times is heated to 65～95 ℃ after the burning after will coming out of the stove, add hydrochloric acid and transfer to PH=0.5～1 that water logging was stirred after 60-90 minute, add 10% barium chloride solution and remove SO
4 -2Stir, heavy clear, filtration, drip washing, leach liquor;
(4) above-mentioned leach liquor is heated to 80～85 ℃, stirring adds ammonium bicarbonate solution and transfers PH=4.5～5, and it is heavy after clear 2-3 hour to stir after 15 minutes, filters drip washing, gets rare earth chloride clear liquid and rich thorium slag;
(5) the water logging filter residue in the step (3) is embathed with 0.5～1N dilute hydrochloric acid, add the quantity of slag and be 2% NH
4F is heated with stirring to 75～100 ℃, insulated and stirred 60～120 minutes, heavy clear, filtration, drip washing, residue, pickling filtrate, pickling filtrate is returned in the water logging operation of step (3);
(6) the rare earth chloride clear liquid is produced single rare earth oxide or through concentrating crystallisation by cooling, is got solid rare earth chloride product for extracting and separating;
(7) with the rare earth chloride clear liquid in the step (4) in extraction separation process, the waste water in the carbon ammonium precipitation of generation is through evaporation, concentrate the ammonium chloride obtain and be used for roasting.
2, the method for producing chlorinated rare earth by decomposing and mixing rare earth headings using calcination of ammonia chloride according to claim 1, it is characterized in that: mixed rare earth concentrates also can mix with carbon, active silica, industrial boric acid, and its proportioning is: mixed rare earth concentrates: carbon: active silica: industrial boric acid=1: 0.3～0.5: 1: 0.1～0.5: 1: 0.2～0.3.
3, the method for producing chlorinated rare earth by decomposing and mixing rare earth headings using calcination of ammonia chloride according to claim 2 is characterized in that: go into the stove starting temperature: 600～850 ℃, and roasting 3～4 hours.
4, the method for producing chlorinated rare earth by decomposing and mixing rare earth headings using calcination of ammonia chloride according to claim 1 and 2 is characterized in that: carbon can be charcoal, coal dust or refinery coke.
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| CN108559851A (en) * | 2018-06-22 | 2018-09-21 | 长沙中硅水泥技术开发有限公司 | A kind of System and method for of cement kiln synergic processing polishing powder from rare earth waste material |
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| CN113025835A (en) * | 2020-07-28 | 2021-06-25 | 江西理工大学 | Method for efficiently extracting rare earth from bastnaesite |
| CN112744854A (en) * | 2020-12-25 | 2021-05-04 | 中国科学院江西稀土研究院 | Rare earth fluoride and preparation method and application thereof |
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| CN115057445A (en) * | 2022-07-22 | 2022-09-16 | 包头稀土研究院 | Production method of silicofluoric acid and treatment process of mixed rare earth concentrate |
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| CN116377521A (en) * | 2022-12-30 | 2023-07-04 | 中国科学院江西稀土研究院 | Method for recycling mixed rare earth from NdFeB waste |
| CN116377521B (en) * | 2022-12-30 | 2024-04-16 | 中国科学院江西稀土研究院 | Method for recycling mixed rare earth from NdFeB waste |
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