CN106498166A - A kind of method that neodymium iron boron greasy filth waste material oxidoreduction full constituent is reclaimed - Google Patents
A kind of method that neodymium iron boron greasy filth waste material oxidoreduction full constituent is reclaimed Download PDFInfo
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry 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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- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
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Abstract
The invention discloses a kind of method that neodymium iron boron greasy filth waste material oxidoreduction full constituent is reclaimed, specifically includes following steps：First to neodymium iron boron greasy filth waste material under anaerobic, react 100min 180min at a temperature of 350 550 DEG C, carry out pyrolysis deoiling treatment, obtain residual solid product and gaseous product, then oxidant direct oxidation reduction is added as raw material with residual solid product, then through gravity treatment, sour molten, extract and separate production rare-earth products.The method can not only be such that the chip oil in waste material effectively removes and fully recovering, and chip waste material therein can be transformed into simple rare-earth products, its rare earth yield and purity are high, and pollution on the environment is avoided during closed processes, ensure that greasy filth harmless resource utilization is reclaimed, therefore, the technical matters have good economic benefit, environmental benefit and social benefit.
Description
Technical field
The present invention relates to the process of neodymium iron boron greasy filth waste material, the oil produced after specially a kind of chip to Nd-Fe-B permanent magnet
The processing method of mud waste material.
Background technology
Neodymium-iron-boron magnetic material, is referred to as " magnetic king " as which has excellent magnetic, is widely applied to multiple necks
Domain.The neodymium iron boron waste material of about 30% raw material weight can be produced in the production process of neodymium iron boron magnetic body, it include turning block and
Oil immersion waste material etc..Rare earth element containing about 30% (wherein containing neodymium about 90%, remaining is terbium, dysprosium etc.) in neodymium iron boron waste material.In
Guo Shi NdFeB materials big producing country, accounts for the 80% of global total output.The yield for expecting China's neodymium iron boron in 2016 will exceed
300000 tons, and 20% growth rate will be kept, about 90,000 tons of neodymium iron boron waste material will be produced within 2016.In order to economize on resources, with
When reduce industrial refuse, environmental protection seems very necessary to neodymium iron boron waste material comprehensive utilization of resources, and can produce significant
Social benefit and considerable economic benefit.
At present, neodymium iron boron greasy filth waste recovery Application way mainly has：Sulphuric acid-double salt precipitation method, the fluoride sedimentation method, adopt
With complete molten method, oxidizing roasting-dissolving with hydrochloric acid method that hydrochloric acid is solvent, production technology is then mostly using being produced by below operation：Burn
→ grinding → oxidizing roasting → acid is molten → remove impurity → extract and separate → precipitation → calcination, wherein from burning oxidizing roasting for from pre-
Science and engineering sequence, although this technology processes ratio more thoroughly to neodymium iron boron waste material, the operating cost of actual recovered production technology is high and controls
Difficulty processed is larger, and these recoverying and utilizing methods are in process of production, all there are industrial chemicals and consumes big, high cost, consolidates
Liquid garbage is more, problem that is can causing secondary pollution to environment.
Content of the invention
It is contemplated that being directed to the deficiencies in the prior art, there is provided a kind of neodymium iron boron greasy filth waste material oxidoreduction full constituent is reclaimed
Method, the method can not only make chip oil in waste material effectively removing fully recovering, and chip waste material energy therein
It is transformed into simple rare-earth products, its rare earth yield and purity are high, and avoids during closed processes environment is made
Into pollution, ensure that greasy filth harmless resource utilization reclaim, therefore, the technical matters have good economic benefit, environment
Benefit and social benefit.
The invention provides reduction, acid are molten realizing neodymium iron boron greasy filth waste material reuse new technique after a kind of first removing oil.Specifically
Comprise the following steps：First to neodymium iron boron greasy filth waste material under anaerobic, react 100min at a temperature of 350 550 DEG C
180min, carries out pyrolysis deoiling treatment, obtains residual solid product and gaseous product, is then added with residual solid product as raw material
Enter oxidant direct oxidation reduction, then through gravity treatment, sour molten, extract and separate production rare-earth products.
The greasy filth waste material that described neodymium iron boron greasy filth waste material is produced after being preferably Nd-Fe-B permanent magnet chip.To the gas
Pyrolytic behavior and pyrolysis gas are obtained after product is condensed.
Oil-water separation is carried out to the pyrolytic behavior, the oil recovery for obtaining（Resource product）Can produce as the oil of high value
Product are sold.
The pyrolysis gas are the higher combustible gas of calorific value, can be used as the fuel of heat supply in pyrolytic process, i.e.,：Released by burning
Thermal discharge is pyrolysis system heat supply, realizes that the inner loop of system capacity is utilized.
Described residual solid product is neodymium iron boron powder and coke mixture, with residual solid product as the direct oxygen of raw material
Change reduction, then through gravity treatment, sour molten, extract and separate production rare-earth products, which at least comprises the following steps：
The first step, the powder that residual solid product is ground to form 200-400 mesh in an inert atmosphere, optimal mesh number are 300 mesh.
Second step, powder ground for the first step is placed in tube furnace, adds oxidant, closed appearance after mix homogeneously
Device, carries out oxidoreduction after being passed through protective gas, described oxidant can be in iron sesquioxide or diboron trioxide
At least one, its oxidoreduction temperature are 1000-1400 DEG C, and preferable reaction temperature is 1300 DEG C, and its response time is that 2-4 is little
When, preferred reaction time is 2.5 hours.
3rd step, grinds to form 50-150 purposes in noble gases the reactant mixture of gained after second step reaction completely
Powder, preferably 100 mesh, are then classified with gravity separation method, obtain the powder particle of Different Weight level, its powder particle weight
Predominantly ferroboron granule, the light predominantly rare earth solid impurity particle of powder particle.
4th step, the rare earth solid impurity particle deionized water dissolving obtained by gravity treatment by the 3rd step, then be added thereto to
The dilute hydrochloric acid of 0.1-0.5mol/L, preferably dilute hydrochloric acid concentration are 0.2mol/L, and its liquid-solid ratio remains 1:6 L/kg, Ran Hou
Isothermal reaction 1-2 hours at 65-75 DEG C, after reaction completely, its solution is diluted to PH=3-7 or so, preferably PH by deionized water
For 5, so that the most of impurity in earth solution can be precipitated completely.
5th step, the acid solution that the 4th step is obtained is filtered, the filter of predominantly ferric hydroxide precipitate and boron is obtained
Slag, and gained filtrate is mainly rare-earth chloride solution.
6th step, carries out Rare Earth Separation to the rare-earth chloride solution that the 5th step is obtained by extraction separation method, obtains single
Pure rare-earth products, its extraction system are P507 systems.
Further, the protective gas described in second step can be argon.
Compared with prior art, the present invention produces the method for greasy filth waste material with as follows after processing Nd-Fe-B permanent magnet chip
Beneficial effect.
（1）, using pyrolysis removing oil technology, simple to operate, production procedure is short, using total enclosing production technology, energy-conservation for the present invention
Environmental protection, can realize the zero-emission for being thoroughly kept completely separate recovery, really realizing the three wastes of neodymium iron boron powder and oil, thoroughly avoid
Smoke pollution problem produced by conventional incineration method oil removing, is truly realized harmless resource utilization high efficiente callback using greasy filth waste material
Purpose.
（2）The present invention simple to operate, do not introduce new impurity, through oil removal treatment after clean neodymium iron boron waste material composition do not occur
Any change, does not only interfere with neodymium iron boron partition, and oil removing operation straight yield of rare earth >=99%.
（3）Compared with traditional long flow processing technique, the oil removing of neodymium iron boron greasy filth waste incineration need not be generated by the present invention
Oxide, again sour molten, precipitation, calcination only need to be produced with the pyrolysis residual solid of neodymium iron boron greasy filth waste material into rare earth oxide
Thing be raw material oxidoreduction, obtain ferroboron and rare earth oxide mixture, then by Gravity separation obtain ferroboron and
Two kinds of materials of rare earth oxide, rare earth oxide is molten through peracid and extract and separate is obtained single high pure rare earth product.This
Technique achieves the full resource reuse of short route of neodymium iron boron greasy filth waste material, and the yield of gained rare-earth products and purity are high, and
By a relatively large margin reduce energy consumption and production cost.
Specific embodiment
Neodymium iron boron greasy filth waste material oxidoreduction full constituent reclaim method through the following steps that realize.
(1) pour neodymium iron boron greasy filth waste material into pyrolysis oven first, stop under anaerobic, 350 550 DEG C of temperature conditionss
100min 180min, in the process, there are pyrolysis in oil content in neodymium iron boron waste material, obtain residual solid product and
Gaseous product.When temperature is too low, the part mink cell focus in greasy filth does not react, and pyrolysis is not exclusively；When temperature is too high, generation
Pyrolysis oil yield can reduce, and be unfavorable for reclaiming pyrolysis oil.When time is too short, reaction is carried out not exclusively；During overlong time, then can make
Waste into unnecessary production.
(2) tubulation indirect condenser, isolated pyrolytic behavior and pyrolysis gas are flowed through by the gas that pyrolysis oven is separated out.Pyrolytic behavior
Subsequently in oil water separator, 2-4h is stopped, realizes that oil-water separation, isolated pyrolysis oil reach oil product fuel oil
Prescription.Containing a certain amount of water solublity oils in the water that isolates, the sewage disposal system for entering oil field is needed to process.
(3) the condensed pyrolysis gas for obtaining afterwards, rich in CH4And H2, the higher combustible gas of calorific value, can be used as be pyrolyzed heat supply
Fuel, is system heat supply by combustion heat release amount, realizes that the inner loop of system capacity is utilized, and the heat smoke of generation is finally passed through
Qualified discharge after process.
(4) the residual solid product that body of heater is discharged is ground to form in an inert atmosphere the powder of 200-400 mesh, milling time
For 20-30min.In the process, it should be ensured that the powder for being ground can pass through the mesh screen of 200 mesh, to ensure oxidoreduction mistake
Fully carrying out for journey, is preferably milled to the powder of 300 mesh.
(5) ground powder is placed in tubular type furnace temperature highest region, adds oxidant, closed appearance after mix homogeneously
Device, carries out oxidoreduction after being passed through argon, and its Redox Condition is to react 2-4 hours at 1000-1400 DEG C, and preferably 2.5
Hour.Residual solid product is neodymium iron boron powder and coke mixture, in the process, residual solid product as reducing agent with
Oxidant reaction, oxidant are iron sesquioxide or at least one in diboron trioxide.Metal in powder and coke, oxidation
There is redox reaction in agent, obtain the reactant mixture of Different Weight level.And temperature too low when, oxidation-reduction process can not
Fully carry out, reaction not exclusively, affects operation below；When temperature is too high, it is unfavorable for the reactant mixture point of Different Weight level
From the yield of rare-earth products can be substantially reduced.
The equation of redox reaction is as follows：
In formulaAFerrum or boron element is represented,MeRepresent carbon or rare earth element.
(6) solid mixture obtained after reaction completely is ground to form the powder of 50-150 mesh in noble gases, preferably
For 100 mesh, then abrasive flour is classified with the jigging machine in gravity separation method, the powder weight granule of gained is mainly ferrum boron and closes
Gold grain, light particle are then mainly rare earth solid impurity particle.
(7) in the rare earth solid impurity particle of gravity treatment gained, add deionized water to be dissolved, be subsequently adding 0.1-0.5mol/L
Dilute hydrochloric acid, preferably dilute hydrochloric acid concentration is 0.2mol/L, and keeps liquid-solid ratio to be always 1:6, then anti-as constant temperature at 65-75 DEG C
Answer 1-2 hours, the completely rear deionized water of question response that its solution is diluted to PH=3-5 or so, preferably PH is 4, regulates solution
After PH, a period of time is stood, so that the most of impurity in earth solution can be precipitated completely, and allow precipitation particle growth.
(8) acid solution obtained in above-mentioned steps is carried out sucking filtration twice with vacuum filter, obtains predominantly hydrogen-oxygen
Change the filtering residue of ferrum precipitation and boron, its recoverable；And gained filtrate is mainly rare-earth chloride solution.
(9) rare-earth chloride solution for obtaining is carried out extract and separate under P507 extraction systems, obtains simple rare earth
Product.The technique of extraction separation method production rare earth is very ripe, does not just add here to repeat.
Greasy filth waste resource recovery processing method is produced after the Nd-Fe-B permanent magnet cutting can realize neodymium iron boron waste material with oil
Be kept completely separate, utilize purpose so as to reach pollution-free and full component resource high efficiente callback, oil that can be in high efficiente callback greasy filth
Resource, realizes that the high efficiente callback from heat supply with energy of system is utilized, while the innoxious of oil-sludge treatment is reached, and in oxidation
During reduction, new impurity is not introduced, effectively eliminate useless composition.Compared with other treatment technologies, the technology tool
Have the advantages that stable and reliable operation, oily resource recovery height, strong adaptability, secondary pollution are little, be a kind of neodymium ferrum being worthy to be popularized
Boron greasy filth waste resource recovery treatment technology.
The method of the present invention is illustrated below by specific embodiment, but the invention is not limited in this.Following realities
Experimental technique described in example is applied, if no special instructions, conventional method is；The reagent and material, if no special instructions,
Obtain from commercial channels.
Embodiment 1.
（1）Certain Nd-Fe-B permanent magnet cutting greasy filth waste material 500g is chosen, neodymium iron boron powder therein, oil with water quality ratio are
28：69：21.By greasy filth waste material in 550 DEG C of temperature, 3 hours oxygen free condition lower time of staying were pyrolyzed；Bubbing is condensed
After obtain pyrolytic behavior and pyrolysis gas, pyrolytic behavior obtains oil through oil-water separation, and pyrolysis gas can be carried for greasy filth hot resolution of waste material as fuel
Energizing quantity, the efficient heat for producing that burns are sufficient for the needs being pyrolyzed, and system can be realized from heat supply, are not required to extra interpolation combustion
Material.After processed by the invention, pyrolysis gas 8.6%, oil recovery 34.3%, residual solid product 57.1% is obtained；In residual solid product
Neodymium iron boron waste material is 40 with the ratio of coke quality：60, oil content 0.25%.
（2）Will（1）Step pyrolysis gained residual solid product takes 100g and grinds 30min in an inert atmosphere so as to powder
Granule is maintained at 250 mesh or so；Oxidoreduction experiment is carried out in tube furnace, and reaction tube is internal diameter 25mm, a length of 1000mm
Alundum tube, selection iron sesquioxide are oxidant, and iron sesquioxide enough with 80g for the powder of 250 mesh of grinding gained is mixed
Close uniform after as porcelain boat in, and which is positioned over highest temperature zone in stove, tubular type under the protection of argon after hermetic container
Stove is warmed up to 1300 DEG C, question response 2.5 hours, and collects the carbon dioxide for producing with sodium hydroxide solution, finally in argon
Room temperature is cooled under the protection of gas, is taken out porcelain boat, is obtained reacted solid mixture.
（3）?（2）The solid mixture that step reaction is obtained completely afterwards grinds to form the powder of 100 mesh or so in noble gases
End, is then classified abrasive flour with the jigging machine in gravity separation method, and the powder weight granule of gained is mainly ferroboron
Grain, light particle are then mainly rare earth solid impurity particle.
（4）?（3）The rare earth slag powder of step gravity treatment gained is put in beaker, is subsequently adding the dilute hydrochloric acid of 0.2mol/L,
Liquid-solid ratio 1:6, will react 1.5 hours in constant temperature water bath of the beaker as 70 DEG C, after reaction completely, deionized water is molten by which
Liquid is diluted to PH=4 or so, stands a period of time, makes precipitation particle growth.
（5）?（4）Acid solution after step dilution carries out sucking filtration twice with vacuum filter, the earth solution of gained
Rare-earth products are obtained by extraction technique.The composition of its earth solution see the table below 1.
1 earth solution composition catalog of table
| Element term | Al | Co | Dy | Nd | Ni | Pr | SUM |
| Content/% | 0.287 | 1.017 | 8.665 | 64.11 | 0.013 | 15.187 | 89.279 |
Embodiment 2.
（1）Certain Nd-Fe-B permanent magnet cutting greasy filth waste material 500g is chosen, neodymium iron boron waste material therein, oil with water quality ratio are
28：69：21.By greasy filth waste material in 350 DEG C of temperature, 2 hours oxygen free condition lower time of staying were pyrolyzed；Bubbing is condensed
After obtain pyrolytic behavior and pyrolysis gas；Pyrolytic behavior obtains oil through oil-water separation；Pyrolysis gas make fuel, burn
Energizing quantity, the efficient heat for producing that burns are sufficient for the needs for being pyrolyzed, and system can be realized from heat supply, are not required to extra interpolation
Fuel.After processed by the invention, pyrolysis gas 10.9%, oil recovery 43.5%, residual solid product 45.6% is obtained；Residual solid is produced
In thing, neodymium iron boron waste material is 30 with the ratio of coke quality：70, oil content 0.21%.
（2）Will（1）The residual solid product of step pyrolysis gained takes 100g and grinds 30min in an inert atmosphere so as to powder
Last granule is maintained at 250 mesh or so；Oxidoreduction experiment is carried out in tube furnace, and reaction tube is internal diameter 25mm, a length of 1000mm
Alundum tube, selection diboron trioxide is oxidant, powder and the enough diboron trioxides of 85g of 250 mesh of grinding gained
After mix homogeneously as porcelain boat in, and which is positioned over highest temperature zone in stove, pipe under the protection of argon after hermetic container
Formula stove is warmed up to 1300 DEG C, treats fully reaction 2.5 hours, and collects the carbon dioxide for producing with sodium hydroxide solution, most
It is cooled to room temperature afterwards under the protection of argon, takes out porcelain boat, obtain reacted solid mixture.
（3）Will（2）The solid mixture that step reaction is obtained completely afterwards grinds to form the powder of 100 mesh in noble gases,
Then abrasive flour is classified with the jigging machine in gravity separation method, the powder weight granule of gained is mainly ferroboron granule,
Light particle is then mainly rare earth solid impurity particle.
（4）?（3）The rare earth slag powder of step gravity treatment gained is put in beaker, is subsequently adding the dilute hydrochloric acid of 0.2mol/L,
Liquid-solid ratio 1:6, will react 1.5 hours in constant temperature water bath of the beaker as 70 DEG C, after reaction completely, deionized water is molten by which
Liquid is diluted to PH=4 or so, stands a period of time, makes precipitation particle growth.
（5）Will（4）Acid solution after step dilution carries out sucking filtration twice with vacuum filter, obtains predominantly boron carbide
Filtering residue, its recoverable is obtained rare-earth products the earth solution of gained by extraction technique.Its earth solution into
Part see the table below 2.
2 earth solution composition catalog of table
| Element term | Al | Co | Dy | Nd | Ni | Pr | B | SUM |
| Content/% | 0.217 | 1.112 | 8.365 | 62.11 | 0.023 | 13.187 | 0.014 | 85.028 |
Embodiment 3.
（1）Certain Nd-Fe-B permanent magnet cutting greasy filth waste material 500g is chosen, neodymium iron boron waste material therein, oil with water quality ratio are
28：69：21.By greasy filth waste material in 450 DEG C of temperature, 3 hours oxygen free condition lower time of staying were pyrolyzed；Bubbing is condensed
After obtain pyrolytic behavior and pyrolysis gas；Pyrolytic behavior obtains oil through oil-water separation；Pyrolysis gas make fuel, burn
Energizing quantity, the efficient heat for producing that burns are sufficient for the needs for being pyrolyzed, and system can be realized from heat supply, are not required to extra interpolation
Fuel.After processed by the invention, pyrolysis gas 10.9%, oil recovery 34.5%, residual solid product 54.6% is obtained；Residual solid is produced
In thing, neodymium iron boron waste material is 35 with the ratio of coke quality：65, oil content 0.23%.
（2）Will（1）The solid residue of step gained takes 100g and grinds 30min in an inert atmosphere so as to which powder particle is protected
Hold between 250 mesh；Oxidoreduction experiment carry out in tube furnace, reaction tube be internal diameter 25mm, the alundum tube of a length of 1000mm,
Iron sesquioxide is selected to compare 1 with the matter of diboron trioxide:1 mixture be oxidant, grinding gained 250 mesh powder with
As for highest temperature zone in stove is positioned in porcelain boat and which after the enough oxidant mix homogeneously of 80g, in argon after hermetic container
Tube furnace is warmed up to 1300 DEG C under the protection of gas, treats fully reaction 2.5 hours, and two for producing are collected with sodium hydroxide solution
Carbon oxide gas, are finally cooled to room temperature under the protection of argon, take out porcelain boat, obtain reacted solid mixture.
（3）Will（2）The completely rear solid mixture for being obtained of step reaction grinds to form the powder of 100 mesh in noble gases
End, is then classified abrasive flour with the jigging machine in gravity separation method, and the powder weight granule of gained is mainly ferroboron
Grain, light particle are then mainly rare earth solid impurity particle.
（4）?（3）The rare earth slag powder of step gravity treatment gained is put in beaker, is subsequently adding the dilute hydrochloric acid of 0.2mol/L,
Liquid-solid ratio 1:6, will react 1.5 hours in constant temperature water bath of the beaker as 70 DEG C, after reaction completely, deionized water is molten by which
Liquid is diluted to PH=4 or so, stands a period of time, makes precipitation particle growth.
（5）?（4）Acid solution after step dilution carries out sucking filtration twice with vacuum filter, then the rare earth of gained
Solution is obtained rare-earth products by extraction technique.The composition of its earth solution see the table below 3.
3 earth solution composition catalog of table
| Element term | Al | Co | Dy | Nd | Ni | Pr | SUM |
| Content/% | 0.187 | 1.012 | 9.365 | 68.11 | 0.031 | 12.187 | 90.892 |
Claims (10)
1. a kind of method that neodymium iron boron greasy filth waste material oxidoreduction full constituent is reclaimed, it is characterised in that first useless to neodymium iron boron greasy filth
Material reacts 30min 180min under anaerobic, at a temperature of 350 550 DEG C, carries out pyrolysis deoiling treatment, obtains remaining solid
Body product and gaseous product, the residual solid product are neodymium iron boron powder and coke mixture, then with the residual solid
Product is raw material addition oxidant direct oxidation reduction, then through gravity treatment, sour molten, extract and separate production rare-earth products, concrete bag
Include following steps：
The first step, the powder that residual solid product is ground to form 200-400 mesh in an inert atmosphere；
Second step, powder ground for the first step is placed in tube furnace, adds oxidant, hermetic container after mix homogeneously to lead to
Oxidoreduction is carried out after entering protective gas, and described oxidant is at least one in iron sesquioxide or diboron trioxide,
Its oxidoreduction temperature is 1000-1400 DEG C, and the response time is 2-4 hours；
3rd step, the powder that the reactant mixture of gained after second step reaction completely is ground to form 50-150 mesh in noble gases
End, is then classified with gravity separation method, obtains the powder particle of Different Weight level, the predominantly ferroboron of its powder particle weight
Granule, the light predominantly rare earth solid impurity particle of powder particle；
4th step, the rare earth solid impurity particle deionized water dissolving obtained by gravity treatment by the 3rd step, then it is added thereto to 0.1-
The dilute hydrochloric acid of 0.5mol/L, its liquid-solid ratio remain 1:6 L/kg, then isothermal reaction 1-2 hours at 65-75 DEG C, have reacted
After complete, its solution is diluted to PH=3-5 or so by deionized water；
5th step, the acid solution that the 4th step is obtained is filtered, and gained filtrate is mainly rare-earth chloride solution；
6th step, carries out Rare Earth Separation to the rare-earth chloride solution that the 5th step is obtained by extraction separation method, obtains simple
Rare-earth products, its extraction system are P507 systems.
2. method according to claim 1, it is characterised in that described neodymium iron boron greasy filth waste material is cut for Nd-Fe-B permanent magnet
The greasy filth waste material produced after bits.
3. method according to claim 1, it is characterised in that residual solid product is ground to form 300 in an inert atmosphere
Purpose powder.
4. method according to claim 1, it is characterised in that the oxidoreduction temperature is 1300 DEG C, the response time is
2.5 hour.
5. method according to claim 1, it is characterised in that the protective gas is argon.
6. method according to claim 1, it is characterised in that the reactant mixture of gained after second step reaction completely is existed
The powder of 100 mesh is ground to form in noble gases.
7. method according to claim 1, it is characterised in that the rare earth solid impurity particle that the 3rd step is obtained by gravity treatment is spent
Ion water dissolution, then the dilute hydrochloric acid of 0.2mol/L is added thereto to, its liquid-solid ratio remains 1:6 L/kg, then at 65-75 DEG C
Lower isothermal reaction 1-2 hours, after reaction completely, its solution is diluted to PH=4 or so by deionized water.
8. method according to claim 1, it is characterised in that obtain pyrolytic behavior and heat after condensed to the gaseous product
Vent one's spleen.
9. method according to claim 8, it is characterised in that oil-water separation is carried out to the pyrolytic behavior, oil is recycled,
Can sell as the oil product of high value.
10. method according to claim 8, it is characterised in that the pyrolysis gas are the higher combustible gas of calorific value, can be used as
Fuel of heat supply in pyrolytic process.
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| CN107794373A (en) * | 2017-11-06 | 2018-03-13 | 王志勇 | The integrated conduct method of the useless magnetic material of neodymium iron boron |
| CN109338113A (en) * | 2018-11-28 | 2019-02-15 | 北京工业大学 | A kind of method of Ca- chloride vat blue RS technology recycling neodymium iron boron sets of holes greasy filth waste material |
| FR3142921A1 (en) * | 2022-12-13 | 2024-06-14 | Caremag | PROCESS FOR RECYCLING USED OR WASTED PERMANENT MAGNETS |
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| CN109338113A (en) * | 2018-11-28 | 2019-02-15 | 北京工业大学 | A kind of method of Ca- chloride vat blue RS technology recycling neodymium iron boron sets of holes greasy filth waste material |
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| CN106498166B (en) | 2018-04-17 |
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Effective date of registration: 20230620 Address after: 341000 No. 10, Gaoxin Avenue, Ganzhou high tech Industrial Development Zone, Ganxian District, Ganzhou City, Jiangxi Province Patentee after: Ganzhou Rare Earth Youli Technology Development Co.,Ltd. Address before: 341000 No. 86 Hongqi Avenue, Jiangxi, Ganzhou Patentee before: Jiangxi University of Science and Technology |