CN106498166B - A kind of method of neodymium iron boron greasy filth waste material redox full constituent recycling - Google Patents
A kind of method of neodymium iron boron greasy filth waste material redox full constituent recycling Download PDFInfo
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- CN106498166B CN106498166B CN201610947146.6A CN201610947146A CN106498166B CN 106498166 B CN106498166 B CN 106498166B CN 201610947146 A CN201610947146 A CN 201610947146A CN 106498166 B CN106498166 B CN 106498166B
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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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- 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
- C22B7/006—Wet processes
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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
Abstract
The invention discloses a kind of method of neodymium iron boron greasy filth waste material redox full constituent recycling, following steps are specifically included：First to neodymium iron boron greasy filth waste material under anaerobic, at a temperature of 350-550 DEG C react 100min-180min, carry out pyrolysis deoiling treatment, obtain residual solid product and gaseous product, then oxidant direct oxidation reduction is added by raw material of residual solid product, then rare-earth products is produced by gravity treatment, sour molten, extract and separate.This method can not only make the effective removing of chip oil and fully recovering in waste material, 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, it can ensure that greasy filth harmless resource utilization recycles, therefore, the technical matters is with good economic efficiency, environmental benefit and social benefit.
Description
Technical field
The present invention relates to the processing of neodymium iron boron greasy filth waste material, the oil specially produced after a kind of chip to Nd-Fe-B permanent magnet
The processing method of mud waste material.
Background technology
Neodymium-iron-boron magnetic material, since it is referred to as " magnetic king " with excellent magnetism, 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..Contain about 30% rare earth element in neodymium iron boron waste material (wherein containing neodymium about 90%, remaining is terbium, dysprosium etc.).In
State is NdFeB material big producer, accounts for the 80% of global total output.Expecting the yield of China's neodymium iron boron in 2016 will exceed
300000 tons, and the growth rate that 20% will be kept, about 90,000 tons of neodymium iron boron waste material will be produced within 2016.In order to economize on resources, together
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：Sulfuric acid-double salt precipitation method, the fluoride precipitation method, adopt
With complete molten method that hydrochloric acid is solvent, oxidizing roasting-dissolving with hydrochloric acid method, production technology is then mostly using being produced by below process：Burn
→ grinding → oxidizing roasting → acid is molten → removal of impurities → extract and separate → precipitation → calcination, wherein from burning oxidizing roasting for from pre-
Science and engineering sequence, although this technology handles 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, and all there is industrial chemicals consumption is big, of high cost, solid
Liquid discarded object is more, the problem of causing secondary pollution to environment.
The content of the invention
It is contemplated that in view of the deficiencies of the prior art, there is provided a kind of neodymium iron boron greasy filth waste material redox full constituent recycling
Method, this method can not only make the effective removing of chip oil and fully recovering in waste material, and chip waste material energy therein
It is transformed into simple rare-earth products, its rare earth yield and purity are high, and are avoided during closed processes and environment is made
Into pollution, can ensure greasy filth harmless resource utilization recycle, therefore, the technical matters is with good economic efficiency, environment
Benefit and social benefit.
Neodymium iron boron greasy filth waste material reuse new technology is realized the present invention provides reduction after a kind of first de-oiling, acid are molten.Specifically
Comprise the following steps：First to neodymium iron boron greasy filth waste material under anaerobic, at a temperature of 350-550 DEG C react 100min-
180min, carries out pyrolysis deoiling treatment, obtains residual solid product and gaseous product, then adds using residual solid product as raw material
Enter oxidant direct oxidation reduction, then rare-earth products are produced by gravity treatment, sour molten, extract and separate.
The neodymium iron boron greasy filth waste material is preferably the greasy filth waste material produced after Nd-Fe-B permanent magnet chip.To the gas
Pyrolytic behavior and pyrolysis gas are obtained after product is condensed.
Water-oil separating, obtained oil recovery are carried out to the pyrolytic behavior（Recycling product）Can be as the oil production of high value
Product are sold.
The pyrolysis gas is 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 inside of system capacity recycles.
The residual solid product is neodymium iron boron powder and coke mixture, using residual solid product as the direct oxygen of raw material
Change reduction, then rare-earth products are produced by gravity treatment, sour molten, extract and separate, it includes at least following steps：
The first step, is ground into 200-400 mesh powders, optimal mesh number is 300 in an inert atmosphere by residual solid product
Mesh.
Second step, the ground powder of the first step is placed in tube furnace, adds oxidant, after mixing closed appearance
Device, carries out redox, the oxidant can be in di-iron trioxide or diboron trioxide after being passed through protective gas
At least one, its redox temperature are 1000-1400 DEG C, and preferable reaction temperature is 1300 DEG C, its reaction time is small for 2-4
When, when preferred reaction time is 2.5 small.
3rd step, second step after the reaction was complete the reaction mixture of gained 50-150 purposes are ground into inert gas
Powder, is preferably 100 mesh, is then classified with gravity separation method, obtains the powder particle of different weight level, its powder particle weight
Predominantly ferroboron particle, the light predominantly rare earth solid impurity particle of powder particle.
The rare earth solid impurity particle that 3rd step is obtained by gravity treatment, is spent ionized water dissolving by the 4th step, then is added thereto
The dilute hydrochloric acid of 0.1-0.5mol/L, preferably dilute hydrochloric acid concentration are 0.2mol/L, its liquid-solid ratio remains 1:6 L/kg, Ran Hou
When isothermal reaction 1-2 is small at 65-75 DEG C, its solution is diluted to PH=3-7 or so, preferably PH with deionized water after the reaction was complete
For 5, so that most of impurity in earth solution can precipitate completely.
5th step, the acid solution that the 4th step obtains is filtered, obtains the filter of predominantly ferric hydroxide precipitate and boron
Slag, and gained filtrate is mainly rare-earth chloride solution.
6th step, carries out Rare Earth Separation by extraction separation method to the rare-earth chloride solution that the 5th step obtains, obtains single
Pure rare-earth products, its extraction system are P507 systems.
Further, the protective gas described in second step can be argon gas.
Compared with prior art, the method for greasy filth waste material is produced after present invention processing Nd-Fe-B permanent magnet chip with as follows
Beneficial effect.
（1）For the present invention using pyrolysis de-oiling technology, easy to operate, production procedure is short, energy saving using totally-enclosed production technology
Environmental protection, can realize that neodymium iron boron powder is kept completely separate recycling with the thorough of oil, really realize the zero-emission of the three wastes, thoroughly avoid
Smoke pollution problem caused by conventional incineration method oil removing, is truly realized harmless resource utilization high efficiente callback and utilizes greasy filth waste material
Purpose.
（2）The present invention is easy to operate, does not introduce new impurity, the clean neodymium iron boron waste material component after oil removal treatment does not occur
Any change, does not interfere with neodymium iron boron partition, but also oil removing process straight yield of rare earth >=99% not only.
（3）Compared with the long flow processing technique of tradition, the present invention need not generate the oil removing of neodymium iron boron greasy filth waste incineration
Oxide, again sour molten, precipitation, calcination need to only produces with the pyrolysis residual solid of neodymium iron boron greasy filth waste material into rare earth oxide
Thing is raw material redox, obtains ferroboron and rare earth oxide mixture, then by Gravity separation obtain ferroboron and
Two kinds of materials of rare earth oxide, rare earth oxide can obtain single high pure rare earth product through peracid is molten with extract and separate.This
Technique realizes the full recycling reuse of short route of neodymium iron boron greasy filth waste material, and the yield and purity of gained rare-earth products are high, and
By a relatively large margin reduce energy consumption and production cost.
Embodiment
Neodymium iron boron greasy filth waste material redox full constituent recycling method through the following steps that realize.
(1) neodymium iron boron greasy filth waste material is poured into pyrolysis oven first, is stopped under anaerobic, 350-550 DEG C of temperature conditionss
Pyrolysis occurs for 100min -180min, in the process, 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 incomplete；When temperature is excessive, generation
Pyrolysis oil yield can reduce, and be unfavorable for recycling pyrolysis oil.When time is too short, reaction carries out incomplete；During overlong time, then it can make
Wasted into unnecessary production.
(2) gas separated out by pyrolysis oven flows through tubulation indirect condenser, isolated pyrolytic behavior and pyrolysis gas.Pyrolytic behavior
Then in oil water separator, 2-4h is stopped, realizes water-oil separating, isolated pyrolysis oil reaches oil product-fuel oil
Quality requirement.Containing a certain amount of water-soluble oils, it is necessary to which the sewage disposal system into oil field is handled in the water isolated.
(3) the condensed pyrolysis gas obtained afterwards, rich in CH4And H2, the higher combustible gas of calorific value, can be used as the heat supply of pyrolysis
Fuel, is system heat supply by combustion heat release amount, realizes that the inside of system capacity recycles, the heat smoke of generation finally passes through
Qualified discharge after processing.
(4) the residual solid product that furnace body is discharged is ground into 200-400 mesh powders, milling time in an inert atmosphere
For 20-30min.In the process, it should be ensured that the powder ground can be by the mesh screen of 200 mesh, to ensure redox
The abundant progress of journey, is preferably milled to 300 mesh powders.
(5) ground powder is placed in tubular type furnace temperature highest region, adds oxidant, after mixing closed appearance
Device, redox is carried out after being passed through argon gas, when its Redox Condition is that reaction 2-4 is small at 1000-1400 DEG C, 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 at least one of di-iron trioxide or diboron trioxide.Metal and coke, oxidation in powder
Redox reaction occurs for agent, obtains the reaction mixture of different weight level.And temperature it is too low when, oxidation-reduction process cannot
Fully carry out, reaction is incomplete, influences operation below；When temperature is excessive, it is unfavorable for the reaction mixture point of different weight level
From the yields of rare-earth products can be substantially reduced.
The equation of redox reaction is as follows：
In formulaARepresent iron or boron element,MeRepresent carbon or rare earth element.
(6) the reaction was complete, the rear solid mixture obtained is ground into 50-150 mesh powders in inert gas, preferably
For 100 mesh, then abrasive flour is classified with the jigging machine in gravity separation method, the powder weight particle of gained is mainly that iron boron closes
Gold grain, light particle are mainly then rare earth solid impurity particle.
(7) deionized water is added in the rare earth solid impurity particle obtained by gravity treatment to be dissolved, then add 0.1-0.5mol/L
Dilute hydrochloric acid, preferably dilute hydrochloric acid concentration is 0.2mol/L, and it is always 1 to keep liquid-solid ratio:6, then it is anti-as constant temperature at 65-75 DEG C
When answering 1-2 small, its solution is diluted to PH=3-5 or so with deionized water after complete reaction, preferably PH is 4, regulates solution
After PH, a period of time is stood, so that most of impurity in earth solution can precipitate completely, and allows and precipitates particle growth.
(8) acid solution obtained in above-mentioned steps is filtered twice with vacuum filter, obtains predominantly hydrogen-oxygen
Change the filter residue of iron precipitation and boron, its recoverable；And gained filtrate is mainly rare-earth chloride solution.
(9) rare-earth chloride solution of acquisition 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 to repeat here.
Neodymium iron boron waste material and oil can be realized by producing greasy filth waste resource recovery processing method after Nd-Fe-B permanent magnet cutting
Be kept completely separate so that reaching pollution-free and full component recycling high efficiente callback utilizes purpose, oil that can be in high efficiente callback greasy filth
Resource, realizes being utilized from heat supply and the high efficiente callback of energy for system, while reaches the innoxious of oil-sludge treatment, and is aoxidizing
During reduction, new impurity is not introduced, effectively eliminates useless component.Compared with other treatment technologies, technology tool
There is the advantages of stable and reliable operation, oily resource recovery is high, adaptable, secondary pollution is small, be a kind of neodymium iron 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 present invention is not limited thereto.Following realities
Experimental method described in example is applied, is conventional method unless otherwise specified；The reagent and material, unless otherwise specified,
Obtain from commercial channels.
Embodiment 1.
（1）Choose certain Nd-Fe-B permanent magnet cutting greasy filth waste material 500g, neodymium iron boron powder therein, oil are with water quality ratio
28：69：21.By greasy filth waste material in 550 DEG C of temperature, the oxygen free condition lower residence time 3 is pyrolyzed when small；Bubbing is condensed
After obtain pyrolytic behavior and pyrolysis gas, pyrolytic behavior obtains oil through water-oil separating, and pyrolysis gas can be that greasy filth hot resolution of waste material carries as fuel
For energy, the efficient heat for generation of burning is sufficient for the needs of pyrolysis, and system can be realized from heat supply, is not required to additionally addition combustion
Material.After processed by the invention, pyrolysis gas 8.6%, oil recovery 34.3%, residual solid product 57.1% are obtained；In residual solid product
The ratio between neodymium iron boron waste material and coke quality are 40：60, oil content 0.25%.
（2）Will（1）Step pyrolysis gained residual solid product takes 100g to grind 30min in an inert atmosphere, makes its powder
Particle is maintained at 250 mesh or so；Redox experiment carries out in tube furnace, and reaction tube is internal diameter 25mm, a length of 1000mm
Alundum tube, it is oxidant to select di-iron trioxide, and 250 mesh powders of the grinding gained di-iron trioxide enough with 80g is mixed
As in porcelain boat after closing uniformly, and it is positioned over highest temperature zone in stove, tubular type under the protection of argon gas after closed container
Stove is warming up to 1300 DEG C, when question response 2.5 is small, and the carbon dioxide produced is collected with sodium hydroxide solution, finally in argon
It is cooled to room temperature under the protection of gas, takes out porcelain boat, the solid mixture after being reacted.
（3）（2）The solid mixture that step reaction obtains afterwards completely is ground into the powder of 100 mesh or so in inert gas
End, is then classified abrasive flour with the jigging machine in gravity separation method, and the powder weight particle of gained is mainly ferroboron
Grain, light particle are mainly then rare earth solid impurity particle.
（4）（3）Rare earth slag powder obtained by step gravity treatment is put into beaker, then adds the dilute hydrochloric acid of 0.2mol/L,
Liquid-solid ratio 1:6, by beaker as in 70 DEG C of constant temperature water bath reaction 1.5 it is small when, it is with deionized water that its is molten after the reaction was complete
Liquid is diluted to PH=4 or so, stands a period of time, makes precipitation particle growth.
（5）（4）Acid solution after step dilution is filtered twice with vacuum filter, the earth solution of gained
Rare-earth products are made by extraction technique.The composition of its earth solution see the table below 1.
1 earth solution composition list 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）Choose certain Nd-Fe-B permanent magnet cutting greasy filth waste material 500g, neodymium iron boron waste material therein, oil are with water quality ratio
28：69：21.By greasy filth waste material in 350 DEG C of temperature, the oxygen free condition lower residence time 2 is pyrolyzed when small；Bubbing is condensed
After obtain pyrolytic behavior and pyrolysis gas；Pyrolytic behavior obtains oil through water-oil separating；Pyrolysis gas makees fuel, burns and is carried for greasy filth hot resolution of waste material
For energy, the efficient heat for generation of burning is sufficient for the needs for pyrolysis, and system can be realized from heat supply, be not required to additionally add
Fuel.After processed by the invention, pyrolysis gas 10.9%, oil recovery 43.5%, residual solid product 45.6% are obtained；Residual solid is produced
The ratio between neodymium iron boron waste material and coke quality are 30 in thing：70, oil content 0.21%.
（2）Will（1）The residual solid product of step pyrolysis gained takes 100g to grind 30min in an inert atmosphere, makes its powder
Last particle is maintained at 250 mesh or so；Redox experiment carries out in tube furnace, and reaction tube is internal diameter 25mm, a length of 1000mm
Alundum tube, it be oxidant to select diboron trioxide, 250 mesh powders and enough 85g diboron trioxide grinding gained
After mixing as in porcelain boat, and it is positioned over highest temperature zone in stove, pipe under the protection of argon gas after closed container
Formula stove is warming up to 1300 DEG C, when abundant reaction 2.5 is small, and the carbon dioxide produced is collected with sodium hydroxide solution, most
It is cooled to room temperature afterwards under the protection of argon gas, takes out porcelain boat, the solid mixture after being reacted.
（3）Will（2）The solid mixture that step reaction obtains afterwards completely is ground into 100 mesh powders in inert gas,
Then abrasive flour being classified with the jigging machine in gravity separation method, the powder weight particle of gained is mainly ferroboron particle,
Light particle is mainly then rare earth solid impurity particle.
（4）（3）Rare earth slag powder obtained by step gravity treatment is put into beaker, then adds the dilute hydrochloric acid of 0.2mol/L,
Liquid-solid ratio 1:6, by beaker as in 70 DEG C of constant temperature water bath reaction 1.5 it is small when, it is with deionized water that its is molten after the reaction was complete
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 is filtered twice with vacuum filter, obtains predominantly boron carbide
Filter residue, the earth solution of gained, is made rare-earth products by its recoverable by extraction technique.Its earth solution into
Part see the table below 2.
2 earth solution composition list 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）Choose certain Nd-Fe-B permanent magnet cutting greasy filth waste material 500g, neodymium iron boron waste material therein, oil are with water quality ratio
28：69：21.By greasy filth waste material in 450 DEG C of temperature, the oxygen free condition lower residence time 3 is pyrolyzed when small；Bubbing is condensed
After obtain pyrolytic behavior and pyrolysis gas；Pyrolytic behavior obtains oil through water-oil separating；Pyrolysis gas makees fuel, burns and is carried for greasy filth hot resolution of waste material
For energy, the efficient heat for generation of burning is sufficient for the needs for pyrolysis, and system can be realized from heat supply, be not required to additionally add
Fuel.After processed by the invention, pyrolysis gas 10.9%, oil recovery 34.5%, residual solid product 54.6% are obtained；Residual solid is produced
The ratio between neodymium iron boron waste material and coke quality are 35 in thing：65, oil content 0.23%.
（2）Will（1）Solid residue obtained by step takes 100g to grind 30min in an inert atmosphere, protects its powder particle
Hold between 250 mesh；Redox experiment carries out in tube furnace, and reaction tube is internal diameter 25mm, the alundum tube of a length of 1000mm,
The matter of di-iron trioxide and diboron trioxide is selected than 1:1 mixture is oxidant, grinding gained 250 mesh powders with
Oxidant enough 80g is after mixing as highest temperature zone in stove is positioned in porcelain boat and it, in argon after closed container
Tube furnace is warming up to 1300 DEG C under the protection of gas, when abundant reaction 2.5 is small, and two produced are collected with sodium hydroxide solution
Carbon oxide gas, are finally cooled to room temperature under the protection of argon gas, take out porcelain boat, the solid mixture after being reacted.
（3）Will（2）The completely rear solid mixture obtained of step reaction is ground into the powder of 100 mesh in inert gas
End, is then classified abrasive flour with the jigging machine in gravity separation method, and the powder weight particle of gained is mainly ferroboron
Grain, light particle are mainly then rare earth solid impurity particle.
（4）（3）Rare earth slag powder obtained by step gravity treatment is put into beaker, then adds the dilute hydrochloric acid of 0.2mol/L,
Liquid-solid ratio 1:6, by beaker as in 70 DEG C of constant temperature water bath reaction 1.5 it is small when, it is with deionized water that its is molten after the reaction was complete
Liquid is diluted to PH=4 or so, stands a period of time, makes precipitation particle growth.
（5）（4）Acid solution after step dilution is filtered twice with vacuum filter, then the rare earth of gained
Rare-earth products are made by extraction technique in solution.The composition of its earth solution see the table below 3.
3 earth solution composition list 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 (9)
- A kind of 1. method of neodymium iron boron greasy filth waste material redox full constituent recycling, it is characterised in that first give up to neodymium iron boron greasy filth Material under anaerobic, 30min-180min is reacted at a temperature of 350-550 DEG C, carry out pyrolysis deoiling treatment, it is solid to obtain remaining Body product and gaseous product, the residual solid product is neodymium iron boron powder and coke mixture, then with the residual solid Product adds oxidant direct oxidation reduction for raw material, then produces rare-earth products, specific bag by gravity treatment, sour molten, extract and separate Include following steps：The first step, 200-400 mesh powders are ground into by residual solid product in an inert atmosphere；Second step, the ground powder of the first step is placed in tube furnace, adds oxidant, after mixing closed container, is led to Entering and redox is carried out after protective gas, the oxidant is at least one of di-iron trioxide or diboron trioxide, Its redox temperature is 1000-1400 DEG C, when the reaction time is 2-4 small；3rd step, second step after the reaction was complete the reaction mixture of gained the powder of 50-150 mesh is ground into inert gas End, is then classified with gravity separation method, obtains the powder particle of different weight level, the predominantly ferroboron of its powder particle weight Particle, the light predominantly rare earth solid impurity particle of powder particle；The rare earth solid impurity particle that 3rd step is obtained by gravity treatment, is spent ionized water dissolving by the 4th step, then adds 0.1- thereto The dilute hydrochloric acid of 0.5mol/L, its liquid-solid ratio remain 1:6 L/kg, when then isothermal reaction 1-2 is small at 65-75 DEG C, have reacted Its solution is diluted to pH=3-5 with deionized water after complete；5th step, the acid solution that the 4th step obtains is filtered, gained filtrate is mainly rare-earth chloride solution；6th step, carries out Rare Earth Separation by extraction separation method to the rare-earth chloride solution that the 5th step obtains, obtains simple Rare-earth products, its extraction system are P507 systems.
- 2. according to the method described in claim 1, it is characterized in that, the neodymium iron boron greasy filth waste material is cut for Nd-Fe-B permanent magnet The greasy filth waste material produced after bits.
- 3. according to the method described in claim 1, it is characterized in that, residual solid product is ground into 300 in an inert atmosphere Mesh powder.
- 4. according to the method described in claim 1, it is characterized in that, the redox temperature is 1300 DEG C, the reaction time is 2.5 it is small when.
- 5. according to the method described in claim 1, it is characterized in that, the protective gas is argon gas.
- 6. according to the method described in claim 1, it is characterized in that, second step after the reaction was complete the reaction mixture of gained exist 100 mesh powders are ground into inert gas.
- 7. according to the method described in claim 1, it is characterized in that, the rare earth solid impurity particle that the 3rd step is obtained by gravity treatment is spent Ionized water dissolves, then adds the dilute hydrochloric acid of 0.2mol/L thereto, its liquid-solid ratio remains 1:6 L/kg, then at 65-75 DEG C When lower isothermal reaction 1-2 is small, its solution is diluted to pH=4 with deionized water after the reaction was complete.
- 8. according to the method described in claim 1, it is characterized in that, obtain pyrolytic behavior and heat after condensed to the gaseous product Vent one's spleen.
- 9. according to the method described in claim 8, it is characterized in that, to pyrolytic behavior progress water-oil separating, oil is recycled, It can be sold as the oil product of high value.
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| CN102899479A (en) * | 2012-10-20 | 2013-01-30 | 北京工业大学 | Pretreatment method of oil sludge obtained after neodymium-iron-boron material grinding through machine tool |
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| CN104690277A (en) * | 2015-03-08 | 2015-06-10 | 北京工业大学 | Method for recycling NdFeB oil sludge according to reduction-diffusion technology |
| CN104690270A (en) * | 2015-03-08 | 2015-06-10 | 北京工业大学 | Short-process method for preparing high-performance sintered NdFeB magnet by utilizing sintered NdFeB oil sludge waste material |
| JP2015120124A (en) * | 2013-12-24 | 2015-07-02 | 太平洋セメント株式会社 | Method for solidifying rare earth-containing residue |
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| CN102899479A (en) * | 2012-10-20 | 2013-01-30 | 北京工业大学 | Pretreatment method of oil sludge obtained after neodymium-iron-boron material grinding through machine tool |
| JP2015120124A (en) * | 2013-12-24 | 2015-07-02 | 太平洋セメント株式会社 | Method for solidifying rare earth-containing residue |
| CN103882234A (en) * | 2014-03-18 | 2014-06-25 | 北京工业大学 | Method for preparing regenerated neodymium iron boron magnetic powder by using neodymium iron boron oily sludge |
| CN104690277A (en) * | 2015-03-08 | 2015-06-10 | 北京工业大学 | Method for recycling NdFeB oil sludge according to reduction-diffusion technology |
| CN104690270A (en) * | 2015-03-08 | 2015-06-10 | 北京工业大学 | Short-process method for preparing high-performance sintered NdFeB magnet by utilizing sintered NdFeB oil sludge waste material |
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