CN110306071A - A kind of method for extraction and purification of dysprosia - Google Patents
A kind of method for extraction and purification of dysprosia Download PDFInfo
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- CN110306071A CN110306071A CN201810835319.4A CN201810835319A CN110306071A CN 110306071 A CN110306071 A CN 110306071A CN 201810835319 A CN201810835319 A CN 201810835319A CN 110306071 A CN110306071 A CN 110306071A
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- C—CHEMISTRY; METALLURGY
- C21—METALLURGY OF IRON
- C21B—MANUFACTURE OF IRON OR STEEL
- C21B15/00—Other processes for the manufacture of iron from iron compounds
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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
- C22B7/001—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
- 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
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- Y02P—CLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
- Y02P10/00—Technologies related to metal processing
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Abstract
The invention discloses a kind of method for extraction and purification of dysprosia, comprising the following steps: step 1, material selection；Step 2, break process；Step 3, acid is molten and filters；Step 4, P507Extraction and separation process；Step 5, precipitating and filtering, step 6, calcination.The present invention is by carrying out extraction processing to rare earth element, after earth solution and liquid alkaline are carried out saponification, by mixed rare earth chlorides through dimethyl phosphatic type (HL)2Extractant P507It extracts (Tb+Dy)3+Ion, then (Tb+Dy) is stripped with hydrochloric acid3+Ion, raffinate (Pr+Nd) Cl3With strip liquor (Tb+Dy) Cl3Into oxalic acid precipitation process, P507 can mainly first extract the heavy rare earth element in solution, remaining major part is light rare earth elements, then weight rare earth element is separated, then back extraction processing is carried out to heavy rare earth, and when carrying out extraction processing to rare earth element, mainly different elements are separated in the way of extraction chromatography, reach the separating effect of rare earth element.
Description
Technical field
The present invention relates to rare earth oxide purification technique field, in particular to a kind of method for extraction and purification of dysprosia.
Background technique
Rare earth has the laudatory title of " industrial vitamin ".Nowadays extremely important strategic resource is had become.Rare earth element oxidation
Object refer to period of element atom ordinal number be 57 to 71 15 kinds of lanthanide oxides, and with lanthanide series chemical property
The oxide of similar scandium (Sc) and yttrium (Y) totally 17 kinds of elements.Rare earth element is in petroleum, chemical industry, metallurgy, weaving, ceramics, glass
The fields such as glass, permanent-magnet material are all widely used.
When carrying out abstraction purification to rare earth element now, P204And P507It can be used as extraction solution, P204After extraction, very
Difficulty carries out back extraction processing, cannot carry out purification process to rare earth element well, and light rare earth and heavy rare earth can not be good
It is separated.
Therefore, it is necessary to solve the above problems to invent a kind of method for extraction and purification of dysprosia.
Summary of the invention
The purpose of the present invention is to provide a kind of method for extraction and purification of dysprosia, P507It can mainly first will be in solution
Heavy rare earth element is extracted, and remaining major part is light rare earth elements, is then separated weight rare earth element, then counterweight is dilute
Soil carries out back extraction processing, and when carrying out extraction processing to rare earth element, mainly in the way of extraction chromatography by different elements into
Row separation, reaches the separating effect of rare earth element, to solve the problems mentioned in the above background technology.
To achieve the above object, the invention provides the following technical scheme: a kind of method for extraction and purification of dysprosia, including with
Lower step:
Material selection: step 1 chooses neodymium iron boron waste material 30wt%, hydrochloric acid 40wt%, liquid alkaline 4.5wt%, P5071wt%,
Kerosene 1wt% and water 33.5wt%；
Break process: step 2 after neodymium iron boron waste material is put into casting furnace inside, the temperature inside casting furnace is risen to
700 DEG C, inside casting furnace then roasting is crushed the waste material after roasting by pulverizer with removing moisture content contained in waste material
Afterwards, to improve the rate of output of rare earth element, the dust of generation is crushed after bag collection, tail gas is discharged by exhaust tube；
Step 3, acid is molten and filters: smashed neodymium iron boron waste material is put into reaction pot, and water and hydrochloric acid solution is added to carry out
Stirring and dissolving heats reaction pot using steam when dissolution, controls 50 DEG C -60 DEG C of reaction temperature, reaction time 3h-5h；
Step 4, P507Extraction and separation process: to adjust P507Acidity and stickiness, need to be mixed with sulfonated kerosene,
Then after carrying out saponification with liquid alkaline, by mixed rare earth chlorides through dimethyl phosphatic type (HL)2Extractant P507Extract (Tb+
Dy)3+Ion, then (Tb+Dy) is stripped with hydrochloric acid3+Ion, raffinate (Pr+Nd) Cl3With strip liquor (Tb+Dy) Cl3Into oxalic acid
Precipitation process；
Its reaction principle is:
Saponification formula: (HL)2+ 2NaOH=(NaL)2+2H2O,
Extract reaction equation: RECl3+3(NaL)2=RE (NaL2)3+ 3NaCl,
It is stripped reaction equation: RE (NaL2)3+ 6HCl=3 (HL)2+RECl3+3NaCl；
Step 5, precipitating and filtering: it after industrial ethanedioic acid is modulated into 16wt%-20wt% oxalic acid solution with water, is added to
1h is reacted in mixed rare earth chlorides, reaction temperature is controlled at 50 DEG C -70 DEG C, and mixed rare earth chloridesization reaction is made to generate oxalic acid
Salt precipitating；
Key reaction formula: 3H2C2O4+2RECl3+6H2O=RE2(C2O4)3·6H2O↓+6HCl；
Step 6, calcination: the mixed rare earth chlorides come out by precipitation and separation are through 850 DEG C of -1000 DEG C of high temperature sintering 30h
Product mix rare earth oxide is generated afterwards；
Key reaction formula: 2RE2(C2O4)3·6H2O+3O2=2RE2O3+12H2O+12CO2↑。
Preferably, the water ratio that accounts for of hydrochloric acid is 31wt% in the step 1.
Preferably, in the step 2, waste material crush at 100-200 mesh.
Preferably, obtaining filtrate and filter residue, filter residue (main component Fe after solution filtering in the step 32O3) outside
It sells, Re is the abbreviation of rare earth element, and filtrate is pumped into the separation that rare earth element is carried out in extraction tank, key reaction formula: Re2O3+6HCL
===2ReCL3+3H2O。
Preferably, in the step 4, when carrying out extraction preparation to dysprosia, after saponification, P507Extraction
Work carries out, and the only metal ion with rare earth exchanged will not make the pH value of solution generate variation.
Technical effect and advantage of the invention:
1, the present invention is by carrying out extraction processing to rare earth element, will after earth solution and liquid alkaline are carried out saponification
Mixed rare earth chlorides are through dimethyl phosphatic type (HL)2Extractant P507It extracts (Tb+Dy)3+Ion, then (Tb+ is stripped with hydrochloric acid
Dy)3+Ion, raffinate (Pr+Nd) Cl3With strip liquor (Tb+Dy) Cl3Into oxalic acid precipitation process, P507 can mainly first will
Heavy rare earth element in solution is extracted, and remaining major part is light rare earth elements, is then separated weight rare earth element, so
It, mainly will not in the way of extraction chromatography when carrying out back extraction processing to heavy rare earth afterwards, and carrying out extraction processing to rare earth element
It is separated with element, reaches the separating effect of rare earth element；
2, the present invention between smashed neodymium iron boron waste material by dissolving, the efficiency that rare earth oxide is reacted with hydrochloric acid solution
Greater than iron oxide, therefore rare earth oxide can first be reacted with hydrochloric acid solution, and iron oxide can be purifying rare earth member after peddling
Element provides economic supply, and iron oxide can also purify as iron simple substance, to increase the utilizing status of metal.
Specific embodiment
Below in conjunction with the embodiment of the present invention, technical scheme in the embodiment of the invention is clearly and completely described,
Obviously, described embodiments are only a part of the embodiments of the present invention, instead of all the embodiments.Based in the present invention
Embodiment, every other embodiment obtained by those of ordinary skill in the art without making creative efforts, all
Belong to the scope of protection of the invention.
Below with reference to embodiment, the present invention is further described.
Embodiment 1
A kind of method for extraction and purification of dysprosia, comprising the following steps:
Material selection: step 1 chooses neodymium iron boron waste material 30wt%, hydrochloric acid 40wt%, liquid alkaline 4.5wt%, P5071wt%,
The water ratio that accounts for of kerosene 1wt% and water 33.5wt%, hydrochloric acid are 31wt%；
Break process: step 2 after neodymium iron boron waste material is put into casting furnace inside, the temperature inside casting furnace is risen to
700 DEG C, inside casting furnace then roasting is crushed the waste material after roasting by pulverizer with removing moisture content contained in waste material
Afterwards, to improve the rate of output of rare earth element, the dust of generation is crushed after bag collection, tail gas is discharged by exhaust tube, waste powder
It is broken at 100 mesh；
Step 3, acid is molten and filters: smashed neodymium iron boron waste material is put into reaction pot, and water and hydrochloric acid solution is added to carry out
Stirring and dissolving heats reaction pot using steam when dissolution, controls 50 DEG C of reaction temperature, reaction time 3h, solution filtering
Filtrate and filter residue, filter residue (main component Fe are obtained afterwards2O3) sell outside, Re is the abbreviation of rare earth element, and filtrate is pumped into extraction tank and carries out
The separation of rare earth element, key reaction formula: Re2O3+ 6HCL=2ReCL3+3H2O；
Step 4, P507Extraction and separation process: to adjust P507Acidity and stickiness, need to be mixed with sulfonated kerosene,
Then after carrying out saponification with liquid alkaline, by mixed rare earth chlorides through dimethyl phosphatic type (HL)2Extractant P507Extract (Tb+
Dy)3+Ion, then (Tb+Dy) is stripped with hydrochloric acid3+Ion, raffinate (Pr+Nd) Cl3With strip liquor (Tb+Dy) Cl3Into oxalic acid
Precipitation process；
Its reaction principle is:
Saponification formula: (HL)2+ 2NaOH=(NaL)2+2H2O,
Extract reaction equation: RECl3+3(NaL)2=RE (NaL2)3+ 3NaCl,
It is stripped reaction equation: RE (NaL2)3+ 6HCl=3 (HL)2+RECl3+ 3NaCl,
When carrying out extraction preparation to dysprosia, after saponification, P507It extracts work to carry out, with rare earth exchanged
Only metal ion, will not make solution pH value generate variation；
Step 5, precipitating and filtering: after industrial ethanedioic acid is modulated into 16wt% oxalic acid solution with water, it is added to mischmetal
1h is reacted in chloride, reaction temperature is controlled at 50 DEG C, and mixed rare earth chloridesization reaction is made to generate oxalate precipitation；
Key reaction formula: 3H2C2O4+2RECl3+6H2O=RE2(C2O4)3·6H2O↓+6HCl；
Calcination: step 6 generates after 850 DEG C of high temperature sintering 30h by the mixed rare earth chlorides that precipitation and separation comes out
Product mix rare earth oxide；
Key reaction formula: 2RE2(C2O4)3·6H2O+3O2=2RE2O3+12H2O+12CO2↑。
Embodiment 2
A kind of method for extraction and purification of dysprosia, comprising the following steps:
Material selection: step 1 chooses neodymium iron boron waste material 30wt%, hydrochloric acid 40wt%, liquid alkaline 4.5wt%, P5071wt%,
The water ratio that accounts for of kerosene 1wt% and water 33.5wt%, hydrochloric acid are 31wt%；
Break process: step 2 after neodymium iron boron waste material is put into casting furnace inside, the temperature inside casting furnace is risen to
700 DEG C, inside casting furnace then roasting is crushed the waste material after roasting by pulverizer with removing moisture content contained in waste material
Afterwards, to improve the rate of output of rare earth element, the dust of generation is crushed after bag collection, tail gas is discharged by exhaust tube, waste powder
It is broken at 200 mesh；
Step 3, acid is molten and filters: smashed neodymium iron boron waste material is put into reaction pot, and water and hydrochloric acid solution is added to carry out
Stirring and dissolving heats reaction pot using steam when dissolution, controls 60 DEG C of reaction temperature, reaction time 5h, solution filtering
Filtrate and filter residue, filter residue (main component Fe are obtained afterwards2O3) sell outside, Re is the abbreviation of rare earth element, and filtrate is pumped into extraction tank and carries out
The separation of rare earth element, key reaction formula: Re2O3+ 6HCL=2ReCL3+3H2O；
Step 4, P507Extraction and separation process: to adjust P507Acidity and stickiness, need to be mixed with sulfonated kerosene,
Then after carrying out saponification with liquid alkaline, by mixed rare earth chlorides through dimethyl phosphatic type (HL)2Extractant P507Extract (Tb+
Dy)3+Ion, then (Tb+Dy) is stripped with hydrochloric acid3+Ion, raffinate (Pr+Nd) Cl3With strip liquor (Tb+Dy) Cl3Into oxalic acid
Precipitation process；
Its reaction principle is:
Saponification formula: (HL)2+ 2NaOH=(NaL)2+2H2O,
Extract reaction equation: RECl3+3(NaL)2=RE (NaL2)3+ 3NaCl,
It is stripped reaction equation: RE (NaL2)3+ 6HCl=3 (HL)2+RECl3+ 3NaCl,
When carrying out extraction preparation to dysprosia, after saponification, P507It extracts work to carry out, with rare earth exchanged
Only metal ion, will not make solution pH value generate variation；
Step 5, precipitating and filtering: after industrial ethanedioic acid is modulated into 20wt% oxalic acid solution with water, it is added to mischmetal
1h is reacted in chloride, reaction temperature is controlled at 70 DEG C, and mixed rare earth chloridesization reaction is made to generate oxalate precipitation；
Key reaction formula: 3H2C2O4+2RECl3+6H2O=RE2(C2O4)3·6H2O↓+6HCl；
Calcination: step 6 generates after 1000 DEG C of high temperature sintering 30h by the mixed rare earth chlorides that precipitation and separation comes out
Product mix rare earth oxide；
Key reaction formula: 2RE2(C2O4)3·6H2O+3O2=2RE2O3+12H2O+12CO2↑。
Embodiment 3
A kind of method for extraction and purification of dysprosia, comprising the following steps:
Material selection: step 1 chooses neodymium iron boron waste material 30wt%, hydrochloric acid 40wt%, liquid alkaline 4.5wt%, P5071wt%,
The water ratio that accounts for of kerosene 1wt% and water 33.5wt%, hydrochloric acid are 31wt%；
Break process: step 2 after neodymium iron boron waste material is put into casting furnace inside, the temperature inside casting furnace is risen to
700 DEG C, inside casting furnace then roasting is crushed the waste material after roasting by pulverizer with removing moisture content contained in waste material
Afterwards, to improve the rate of output of rare earth element, the dust of generation is crushed after bag collection, tail gas is discharged by exhaust tube, waste powder
It is broken at 150 mesh；
Step 3, acid is molten and filters: smashed neodymium iron boron waste material is put into reaction pot, and water and hydrochloric acid solution is added to carry out
Stirring and dissolving heats reaction pot using steam when dissolution, controls 55 DEG C of reaction temperature, reaction time 4h, solution filtering
Filtrate and filter residue, filter residue (main component Fe are obtained afterwards2O3) sell outside, Re is the abbreviation of rare earth element, and filtrate is pumped into extraction tank and carries out
The separation of rare earth element, key reaction formula: Re2O3+ 6HCL=2ReCL3+3H2O；
Step 4, P507Extraction and separation process: to adjust P507Acidity and stickiness, need to be mixed with sulfonated kerosene,
Then after carrying out saponification with liquid alkaline, by mixed rare earth chlorides through dimethyl phosphatic type (HL)2Extractant P507Extract (Tb+
Dy)3+Ion, then (Tb+Dy) is stripped with hydrochloric acid3+Ion, raffinate (Pr+Nd) Cl3With strip liquor (Tb+Dy) Cl3Into oxalic acid
Precipitation process；
Its reaction principle is:
Saponification formula: (HL)2+ 2NaOH=(NaL)2+2H2O,
Extract reaction equation: RECl3+3(NaL)2=RE (NaL2)3+ 3NaCl,
It is stripped reaction equation: RE (NaL2)3+ 6HCl=3 (HL)2+RECl3+ 3NaCl,
When carrying out extraction preparation to dysprosia, after saponification, P507It extracts work to carry out, with rare earth exchanged
Only metal ion, will not make solution pH value generate variation；
Step 5, precipitating and filtering: after industrial ethanedioic acid is modulated into 18wt% oxalic acid solution with water, it is added to mischmetal
1h is reacted in chloride, reaction temperature is controlled at 60 DEG C, and mixed rare earth chloridesization reaction is made to generate oxalate precipitation；
Key reaction formula: 3H2C2O4+2RECl3+6H2O=RE2(C2O4)3·6H2O↓+6HCl；
Calcination: step 6 generates after 920 DEG C of high temperature sintering 30h by the mixed rare earth chlorides that precipitation and separation comes out
Product mix rare earth oxide；
Key reaction formula: 2RE2(C2O4)3·6H2O+3O2=2RE2O3+12H2O+12CO2↑。
Table is obtained according to embodiment 1-3 data:
According to table: when being extracted to the rare earth element in neodymium iron boron waste material, needing according to light rare earth and again
Different ionic radius is classified between rare earth, P507Mainly first the heavy rare earth element in solution can be extracted, it is remaining
Major part be light rare earth elements, then weight rare earth element is separated, back extraction processing then is carried out to heavy rare earth, and to rare earth
When element carries out extraction processing, mainly different elements are separated in the way of extraction chromatography, reach point of rare earth element
From effect, the metal oxide generated after neodymium iron boron waste material calcination can be peddled, reduce the warp to rare earths separation
Ji consumption.
Finally, it should be noted that the foregoing is only a preferred embodiment of the present invention, it is not intended to restrict the invention,
Although the present invention is described in detail referring to the foregoing embodiments, for those skilled in the art, still may be used
To modify the technical solutions described in the foregoing embodiments or equivalent replacement of some of the technical features,
All within the spirits and principles of the present invention, any modification, equivalent replacement, improvement and so on should be included in of the invention
Within protection scope.
Claims (5)
1. a kind of method for extraction and purification of dysprosia, which comprises the following steps:
Material selection: step 1 chooses neodymium iron boron waste material 30wt%, hydrochloric acid 40wt%, liquid alkaline 4.5wt%, P5071wt%, kerosene
1wt% and water 33.5wt%；
Step 2, break process: after neodymium iron boron waste material is put into casting furnace inside, rising to 700 DEG C for the temperature inside casting furnace,
Roasting is inside casting furnace to remove moisture content contained in waste material, then by the waste material after roasting after pulverizer crushes, with
The rate of output for improving rare earth element, crushes the dust of generation after bag collection, tail gas is discharged by exhaust tube；
Step 3, acid is molten and filters: smashed neodymium iron boron waste material is put into reaction pot, and water and hydrochloric acid solution is added to be stirred
Dissolution heats reaction pot using steam when dissolution, controls 50 DEG C -60 DEG C of reaction temperature, reaction time 3h-5h；
Step 4, P507Extraction and separation process: to adjust P507Acidity and stickiness, need to be mixed with sulfonated kerosene, then
After carrying out saponification with liquid alkaline, by mixed rare earth chlorides through dimethyl phosphatic type (HL)2Extractant P507It extracts (Tb+Dy)3+
Ion, then (Tb+Dy) is stripped with hydrochloric acid3+Ion, raffinate (Pr+Nd) Cl3With strip liquor (Tb+Dy) Cl3Into oxalic acid precipitation
Process；
Its reaction principle is:
Saponification formula: (HL)2+ 2NaOH=(NaL)2+2H2O,
Extract reaction equation: RECl3+3(NaL)2=RE (NaL2)3+ 3NaCl,
It is stripped reaction equation: RE (NaL2)3+ 6HCl=3 (HL)2+RECl3+3NaCl；
Step 5, precipitating and filtering: after industrial ethanedioic acid is modulated into 16wt%-20wt% oxalic acid solution with water, it is added to mixing
1h is reacted in rare earth-iron-boron, reaction temperature is controlled at 50 DEG C -70 DEG C, so that mixed rare earth chloridesization reaction is generated oxalates heavy
It forms sediment；
Key reaction formula: 3H2C2O4+2RECl3+6H2O=RE2(C2O4)3·6H2O↓+6HCl；
Step 6, calcination: raw after 850 DEG C of -1000 DEG C of high temperature sintering 30h by the mixed rare earth chlorides that precipitation and separation comes out
At product mix rare earth oxide；
Key reaction formula: 2RE2(C2O4)3·6H2O+3O2=2RE2O3+12H2O+12CO2↑。
2. a kind of method for extraction and purification of dysprosia according to claim 1, it is characterised in that: in the step 1, salt
The water ratio that accounts for of acid is 31wt%.
3. a kind of method for extraction and purification of dysprosia according to claim 1, it is characterised in that: in the step 2, give up
Feed powder is broken at 100-200 mesh.
4. a kind of method for extraction and purification of dysprosia according to claim 1, it is characterised in that: molten in the step 3
Filtrate and filter residue, filter residue (main component Fe are obtained after liquid filtering2O3) sell outside, Re is the abbreviation of rare earth element, and filtrate is pumped into extraction tank
The middle separation for carrying out rare earth element, key reaction formula: Re2O3+ 6HCL===2ReCL3+3H2O。
5. a kind of method for extraction and purification of dysprosia according to claim 1, it is characterised in that: in the step 4,
When carrying out extraction preparation to dysprosia, after saponification, P507It extracts work to carry out, the only metal with rare earth exchanged
Ion will not make the pH value of solution generate variation.
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN111485110A (en) * | 2020-06-05 | 2020-08-04 | 中国林业科学研究院林产化学工业研究所 | Method for improving utilization rate of valuable elements in rare earth |
| CN116043016A (en) * | 2022-07-19 | 2023-05-02 | 江苏南方永磁科技有限公司 | Preparation method and application of neodymium oxide |
| TWI819544B (en) * | 2022-03-28 | 2023-10-21 | 朝陽科技大學 | Methods for recovering and separating rare earth metals from rare earth waste |
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