CN106834757A - A kind of 14 kinds of methods of rare earth element of Sync enrichment in roasted ore from rare earth sulfuric acid - Google Patents
A kind of 14 kinds of methods of rare earth element of Sync enrichment in roasted ore from rare earth sulfuric acid 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
- 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
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/28—Amines
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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
14 kinds of methods of rare earth element of Sync enrichment in a kind of roasted ore from rare earth sulfuric acid of present invention offer, belong to rare-earth enrichment field.The method is with N, N, N ', the oxygen glutaramide abbreviation TODGA of four octyl groups of N ' 3 is extractant, with kerosene as diluent, it is enriched with while 14 kinds of rare earth ions during rare earth sulfuric acid roasted ore is realized by way of liquid-liquid extraction using dissolubility property of the rare earth element under different extraction acidity, extractant concentration, extraction volume ratio, extraction time, extraction times.The method that the present invention is provided can be realized being enriched with while lanthanum, cerium, praseodymium, neodymium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, 14 kinds of rare earth elements of yttrium in rare earth sulfuric acid roasted ore, practicality simple to operate, required separation equipment is few, not corrosive equipment, is adapted to sulphuric acid environment needed for industrial production, drug dosage, required energy consumption are substantially reduced, extraction efficiency is high, and TODGA can be recycled, and waste liquid is pollution-free, discharge is reduced, and meets the demand of environmental protection.
Description
Technical field
The present invention relates to a kind of Extraction and enrichment method of various rare earth elements in roasted ore to rare earth sulfuric acid, belong to rare earth rich
Collection field.
Background technology
Rare earth be countries in the world today rebuild traditional industry, developing high-tech and the indispensable weight of national defence sophisticated technology
Want strategic resource.With the continuous breakthrough of the continuous progressive and application technology of science and technology, the value of single rare earth oxide is increasingly
Greatly.Rare earth element is obtained in fields such as oil, chemical industry, metallurgy, weaving, ceramics, glass, permanent-magnet materials and is widely applied.
Many extract and separates of method P204, P205 more than the comparing of current industrial rare-earth separating, but extraction efficiency is low, in order to change
Enter technique, improve the utilization ratio of rare earth resources, a kind of simple, efficient mischmetal method for separating and concentrating of exploration is isolated dilute
Earth elements seem and its necessary, are that we probe into using new rare-earth extractant N, N, N this ', the octyl group -3- oxygen glutaryls of N '-four
Amine abbreviation TODGA is enriched with rare earth under sulphuric acid environment, can not only separate 4 kinds of light rare earths from mixing sample ore well rich
Collection, additionally it is possible to remaining 10 kinds of heavy rare earth is also extracted, highly desirable effect has been obtained.
Solvent extraction is the wide process for separation and purification of an application field, be widely used in hydrometallurgy, petrochemical industry,
The industrial circles such as non-ferrous metal metallurgy, nuclear fuel extraction purification, pharmacy and environmental protection, have become rare earth, non-ferrous metal work
Industry separates the important means for producing simple metal.Chemical-process is pursuing high efficiency, environment-friendly and zero-emission, solvent extraction point all the time
It is no exception from flow.Therefore, probing into new more efficient, more environmentally friendly, the more simple solvent extraction and separation method of technique will make
Chemical reagent acid and alkali consumption declines, and industrial discharge is reduced, beneficial to environmental protection.
The content of the invention
The invention solves the problems that optimization of the rare-earth industry to the demand, solvent selection and extraction conditions of the environment of rare earth extraction
Etc. technical problem, therefore provide a kind of use TODGA abstraction techniques Sync enrichment rare earth element from rare earth sulfuric acid roasted ore
Method.
To achieve the above object, the technical scheme is that：One kind Sync enrichment from rare earth sulfuric acid roasted ore
14 kinds of methods of rare earth element, it is characterised in that in sulphuric acid environment, TODGA is extractant reality by way of liquid-liquid extraction
Now Sync enrichment lanthanum, cerium, praseodymium, neodymium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, 14 kinds of rare earths of yttrium from rare earth sulfuric acid roasted ore
Element, comprises the following steps：
(1)：The preparation of rare earth sulfate leaching liquid：Rare earth sulfuric acid roasted ore is measured in container, with certain mass ratio with
Deionized water mixes, and adds moderate amount of sulfuric acid, is heated for a period of hours under leaching temperature and is allowed to dissolve, and collects clear liquid and obtains final product rare earth sulfuric acid
Salt leaching liquid；
(2)：The preparation of extraction agent solution, solution to be separated and back extraction mixed acid solution：A solution：Take TODGA diluents
Dilution, obtains extracting agent solution；B solution：The rare earth sulfate leaching liquid for preparing is taken, cooling is placed after adjusting acidity with sulfuric acid
It is standby, obtain solution to be separated；C solution：Hydrochloric acid and the mixed acid solution of nitric acid needed for preparing back extraction, place cooling standby
With, obtain be stripped mixed acid solution；
(3)：Extract and separate：Using liquid-liquid extraction method, by a solution and b solution in step (2) with certain volume than mixing
In separatory funnel, vibration shakes up, and rare earth ion is complexed to organic phase, separates organic phase and water phase；
(4)：Back extraction enrichment：The organic phase in step (3) is taken in separatory funnel, with the c solution in step (2) and gone
Ionized water is extracted to organic phase successively as two kinds of water phases, and two kinds of water are not fixed using order, using liquid-liquid extraction method
Rare earth ion is transferred in water phase, that is, realize and rare earth unit is enriched with from rare earth sulfuric acid roasted ore using TODGA abstraction techniques
Element.
Step (1) the middle rare earth sulfuric acid baking ore deposit is 1 with the mass ratio of deionized water:(30~150)；Rare earth sulfuric acid is roasted
The mass ratio for burning ore deposit with sulfuric acid (with 98% sulphur acid meter) is 1：(0.5~3), leaching temperature is 30~100 DEG C；Leaching time is 1
~10 hours；Leaching liquid rare earth ion total concentration is 4.0~20.0g/L.
The diluent of a solution is kerosene in the step (2), and its density is the quality of 0.8g/mL, TODGA and diluent
Than being 1：(15~60).
B solution is sulfate liquor in the step (2), is 2.0 with sulfuric acid concentration in its solution after sulfuric acid regulation acidity
~9.0mol/L；C solution is aqueous phase solution in step (2), and it is nitric acid and hydrochloric acid mixed solution, wherein concentration of hydrochloric acid be 0.5~
5.0mol/L, nitric acid is with the molar concentration rate of hydrochloric acid：1：(1~10).
A solution mixes with b solution and shaken up vibration, in b solution Rare Earth Ion and a solution in the step (3)
The mass concentration ratio of TODGA is 1：(1~13), duration of oscillation is 3 minutes/time, and extraction times are 1~9 time, organic phase and water phase
Extraction volume ratio is 1：(0.3~3).
In the step (4) the back extraction condition of stripping process be c solution with it is organic collected by extraction in step (3)
The volume ratio of phase is 1：(0.3~3), minute/time of duration of oscillation 3, back extraction number of times is 1~9 time；Deionized water and step (3)
The volume ratio of the organic phase collected by middle extraction is (0.5~3)：1, minute/time of duration of oscillation 3, back extraction number of times is 1~4
It is secondary.Order is used not fix as the c solution and deionized water of water phase.
Overall recovery according to all rare earth ions in rare earth sulfuric acid roasting ore leaching liquid after above method treatment reaches
82%~95%.
Above-mentioned technical proposal of the invention has the beneficial effect that：
The enrichment method of above-mentioned mixed rare earth ions meets industrial requirement, and practicality simple to operate, extraction efficiency is high, and the party
Method is environmentally safe, and the selectivity to rare earth element is high, can meet current social and Novel Extractant is utilized under sulfuric acid system
To the extraction demand of rare earth ion.
Specific embodiment
To make the technical problem to be solved in the present invention, technical scheme and advantage clearer, below in conjunction with specific implementation
Example is described in detail.
Technical scheme provided by the present invention is explained in detail with reference to embodiment, but not as to the claims in the present invention
The limitation of protection domain.A kind of 14 kinds of methods of rare earth element of Sync enrichment in roasted ore from rare earth sulfuric acid, specific implementation is for example
Under：
Embodiment 1
(1)：The preparation of rare earth sulfate leaching liquid：100 DEG C of 90mL deionized waters heated for controlling temperature is taken, lower addition is stirred continuously
3g rare earth sulfuric acid roasted ores, add the 9g concentrated sulfuric acids, continue to stir 1h after charging.After cooling, infusion, now, water are filtrated to get
The rare earth ion concentration of immersion liquid is about 20.0g/L.
(2)：The preparation of extraction agent solution, solution to be separated and back extraction mixed acid solution：A solution：Pipette 2mLTODGA dilute
Release and agent solution is extracted in 88mL kerosene.B solution：The solution that 5mL steps (1) treatment is obtained is taken, 3.3mL concentrated sulfuric acids use is measured
21.7mL deionized waters dilute, and mix with 5mL rare earth sulfuric acid solutions after cooling and obtain final product solution to be separated.C solution：Measure 11.3mL
Concentrated hydrochloric acid, 9mL concentrated nitric acids are diluted with water after mixing as 270mL is stripped mixed acid solution.
(3)：Extract and separate：The b solution 30mL that step (2) is obtained are taken, is mixed in separatory funnel with a solution of 90mL and shaken
Extraction is swung, duration of oscillation is extracted 1 time for 3 minutes, obtains 90mL organic phase raffinates.
(4)：Back extraction enrichment：(3) are collected the 90mL organic phase raffinates for obtaining to pour into separatory funnel, c solution is used
Be stripped, c solution usages be each 30mL, duration of oscillation 3 minutes, back extraction 9 times after, the water that will be obtained mutually is depressurized
Concentrated by rotary evaporation, carries out ICP measure.Sample ore leaching liquid Rare Earth Ion extraction rate reached is to more than 83%.
Embodiment 2
(1)：The preparation of rare earth sulfate leaching liquid：65 DEG C of 200mL deionized waters heated for controlling temperature is taken, lower addition is stirred continuously
3g rare earth concentrated sulfuric acid roasting ore deposits, continue to stir 4h after charging, and the 6g concentrated sulfuric acids are added in stirring.After cooling, water logging is filtrated to get
Liquid, now, the rare earth ion concentration of infusion is about 9.0g/L.
(2)：The preparation of extraction agent solution, solution to be separated and back extraction mixed acid solution：A solution：Pipette 2.5mLTODGA
It is diluted in 87.5mL kerosene and extracts agent solution.B solution：The solution that 5mL steps (1) treatment is obtained is taken, the dense sulphur of 15mL is measured
Acid is diluted with 10mL deionized waters, is mixed with 5mL rare earth sulfuric acid solutions after cooling and is obtained final product solution to be separated.C solution：Measure
113mL concentrated hydrochloric acids, 9mL concentrated nitric acids are diluted with water after mixing as 270mL is stripped mixed acid solution.
(3)：Extract and separate：The b solution 30mL that step (2) is obtained are taken, is mixed in separatory funnel with a solution of 45mL and shaken
Extraction is swung, duration of oscillation 3 minutes is extracted 2 times, obtain 90mL organic phases extraction and close liquid.
(4)：Back extraction enrichment：(3) are collected the 90mL organic phases extraction conjunction liquid for obtaining to pour into separatory funnel, c solution is used
It is stripped, c solution usages are each 45mL, organic phase after being stripped 6 times, is added 270mL by duration of oscillation 3 minutes
Deionized water oscillation extraction, duration of oscillation 3 minutes will obtain all water and mutually merge, and carry out vacuum rotary steam concentration, carry out ICP surveys
It is fixed.Sample ore leaching liquid Rare Earth Ion extraction rate reached is to more than 92%.
Embodiment 3
(1)：The preparation of rare earth sulfate leaching liquid：45 DEG C of 300mL deionized waters heated for controlling temperature is taken, lower addition is stirred continuously
3g rare earth concentrated sulfuric acid roasting ore deposits, continue to stir 7h after charging, and the 3g concentrated sulfuric acids are added in whipping process.After cooling, water is filtrated to get
Immersion liquid, now, the rare earth ion concentration of infusion is 6.0g/L.
(2)：The preparation of extraction agent solution, solution to be separated and back extraction mixed acid solution：A solution：Pipette 1.3mLTODGA
It is diluted in 88.7mL kerosene and extracts agent solution.B solution：The solution that 5mL steps (1) treatment is obtained is taken, the dense sulphur of 10mL is measured
Acid is diluted with 15mL deionized waters, is mixed with 5mL rare earth sulfuric acid solutions after cooling and is obtained final product solution to be separated.C solution：Measure
56.5mL concentrated hydrochloric acids, 9mL concentrated nitric acids are diluted with water after mixing as 270mL is stripped mixed acid solution.
(3)：Extract and separate：The b solution 30mL that step (2) is obtained are taken, is mixed in separatory funnel with a solution of 30mL and shaken
Extraction is swung, duration of oscillation 3 minutes is extracted 3 times, obtain 90mL organic phases extraction and close liquid.
(4)：Back extraction enrichment：(3) are collected the 90mL organic phases extraction conjunction liquid for obtaining to pour into separatory funnel, c solution is used
Be stripped, c solution usages be each 54mL, duration of oscillation 3 minutes, back extraction 4 times after, organic phase add 45mL go from
Sub- water oscillation extraction, duration of oscillation 3 minutes, is repeated twice, then is stripped once with the c solution of 54mL, all water that will be obtained
Mutually merge, carry out vacuum rotary steam concentration, carry out ICP measure.Sample ore leaching liquid Rare Earth Ion extraction rate reached is to more than 95%.
Embodiment 4
(1)：The preparation of rare earth sulfate leaching liquid：30 DEG C of 450mL deionized waters heated for controlling temperature is taken, lower addition is stirred continuously
3g rare earth concentrated sulfuric acid roasting ore deposits, continue to stir 10h after charging, and the 1.5g concentrated sulfuric acids are added in stirring.After cooling, water logging is filtrated to get
Liquid, now, the rare earth ion concentration of infusion is 4.0g/L.
(2)：The preparation of extraction agent solution, solution to be separated and back extraction mixed acid solution：A solution：Pipette 5mLTODGA dilute
Release and agent solution is extracted in 85mL kerosene.B solution：The solution that 5mL steps (1) treatment is obtained is taken, the 8.00mL concentrated sulfuric acids are measured
Diluted with 17.00mL deionized waters, mix with 5mL rare earth sulfuric acid solutions after cooling and obtain final product solution to be separated.C solution：Measure
79mL concentrated hydrochloric acids, 9mL concentrated nitric acids are diluted with water after mixing as 270mL is stripped mixed acid solution.
(3)：Extract and separate：The b solution 30mL that step (2) is obtained are taken, is mixed in separatory funnel with a solution of 18mL and shaken
Extraction is swung, duration of oscillation 3 minutes is extracted 5 times, obtain 90mL organic phases extraction and close liquid.
(4)：Back extraction enrichment：(3) are collected the 90mL organic phases extraction conjunction liquid for obtaining to pour into separatory funnel, c solution is used
It is stripped, c solution usages are 90mL, duration of oscillation 3 minutes is stood after dividing liquid, and organic phase 90mL deionized waters vibrate
Extraction, duration of oscillation 3 minutes stands a point liquid.By aforesaid operations order, organic phase is alternately extracted with c solution and deionized water,
Each extraction 3 times, all water that will be obtained mutually merge, and carry out vacuum rotary steam concentration, carry out ICP measure.Sample ore leaching liquid middle rare earth
The ion extraction rate reaches more than 92%.
Embodiment 5
(1)：The preparation of rare earth sulfate leaching liquid：80 DEG C of 330mL deionized waters heated for controlling temperature is taken, lower addition is stirred continuously
3g rare earth concentrated sulfuric acid roasting ore deposits, continue to stir 6h after charging, and the 4.5g concentrated sulfuric acids are added in stirring.After cooling, water logging is filtrated to get
Liquid, now, the rare earth ion concentration of infusion is 5.4g/L.
(2)：The preparation of extraction agent solution, solution to be separated and back extraction mixed acid solution：A solution：Pipette 3.8mLTODGA
It is diluted in 86.2mL kerosene and extracts agent solution.B solution：The solution that 5mL steps (1) treatment is obtained is taken, the dense sulphur of 12mL is measured
Acid is diluted with 13mL deionized waters, is mixed with 5mL rare earth sulfuric acid solutions after cooling and is obtained final product solution to be separated.C solution：Measure
56.5mL concentrated hydrochloric acids, 9mL concentrated nitric acids are diluted with water after mixing as 270mL is stripped mixed acid solution.
(3)：Extract and separate：The b solution 30mL that step (2) is obtained are taken, is mixed in separatory funnel with a solution of 10mL and shaken
Extraction is swung, duration of oscillation 3 minutes is extracted 9 times, obtain 90mL organic phases extraction and close liquid.
(4)：Back extraction enrichment：(3) are collected the 90mL organic phases extraction conjunction liquid for obtaining to pour into separatory funnel, c solution is used
It is stripped, c solution usages are 270mL, duration of oscillation 3 minutes is stood after dividing liquid, and organic phase 67mL deionized waters vibrate
Extraction, duration of oscillation 3 minutes is extracted 4 times, and all water that will be obtained mutually merge, and carry out vacuum rotary steam concentration, carry out ICP measure.
Sample ore leaching liquid Rare Earth Ion extraction rate reached is to more than 82%.
The above is the preferred embodiment of the present invention, it is noted that for those skilled in the art
For, on the premise of principle of the present invention is not departed from, some improvements and modifications can also be made, these improvements and modifications
Should be regarded as protection scope of the present invention.
Claims (6)
1. a kind of 14 kinds of methods of rare earth element of Sync enrichment in roasted ore from rare earth sulfuric acid, it is characterised in that in sulphuric acid environment
In, realized by way of liquid-liquid extraction with TODGA as extractant from rare earth sulfuric acid roasted ore Sync enrichment lanthanum, cerium, praseodymium,
Neodymium, europium, gadolinium, terbium, dysprosium, holmium, erbium, thulium, ytterbium, lutetium, 14 kinds of rare earth elements of yttrium, comprise the following steps：
(1)：The preparation of rare earth sulfate leaching liquid：Rare earth sulfuric acid roasted ore is measured in container, with certain mass ratio with go from
Sub- water mixing, adds moderate amount of sulfuric acid, is heated for a period of hours under leaching temperature and is allowed to dissolve, and collects clear liquid and obtains final product rare earth sulfate leaching
Take liquid；
(2)：The preparation of extraction agent solution, solution to be separated and back extraction mixed acid solution：A solution：Take TODGA dilute with diluent
Release, obtain extracting agent solution；B solution：The rare earth sulfate leaching liquid for preparing is taken, placement cooling is standby after adjusting acidity with sulfuric acid
With obtaining solution to be separated；C solution：The mixed acid solution of hydrochloric acid and nitric acid needed for preparing back extraction, placement cooling is standby,
Obtain being stripped mixed acid solution；
(3)：Extract and separate：Using liquid-liquid extraction method, a solution and b solution in step (2) are mixed in point with certain volume ratio
In liquid funnel, vibration shakes up, and rare earth ion is complexed to organic phase, separates organic phase and water phase；
(4)：Back extraction enrichment：The organic phase in step (3) is taken in separatory funnel, with c solution and deionization in step (2)
Water is extracted to organic phase successively as two kinds of water phases, and two kinds of water are not fixed using order, are made using liquid-liquid extraction method dilute
In native ion-transfer to water phase, that is, realize using TODGA abstraction techniques enrichment of rare earth elements from rare earth sulfuric acid roasted ore.
2. 14 kinds of methods of rare earth element of Sync enrichment in a kind of roasted ore from rare earth sulfuric acid according to claim 1, its
It is characterised by, step (1) the middle rare earth sulfuric acid baking ore deposit is 1 with the mass ratio of deionized water:(30~150)；Rare earth sulfuric acid
The mass ratio of roasted ore and 98% sulfuric acid is 1：(0.5~3), leaching temperature is 30~100 DEG C；Leaching time is 1~10 hour；
Leaching liquid rare earth ion total concentration is 4.0~20.0g/L.
3. 14 kinds of methods of rare earth element of Sync enrichment in a kind of roasted ore from rare earth sulfuric acid according to claim 1, its
It is characterised by, the diluent of a solution is kerosene in the step (2), its density is the quality of 0.8g/mL, TODGA and diluent
Than being 1：(15~60).
4. 14 kinds of methods of rare earth element of Sync enrichment in a kind of roasted ore from rare earth sulfuric acid according to claim 1, its
It is characterised by, b solution is sulfate liquor in the step (2), is 2.0 with sulfuric acid concentration in its solution after sulfuric acid regulation acidity
~9.0mol/L；C solution is aqueous phase solution in step (2), and it is nitric acid and hydrochloric acid mixed solution, wherein concentration of hydrochloric acid be 0.5~
5.0mol/L, nitric acid is with the molar concentration rate of hydrochloric acid：1：(1~10).
5. 14 kinds of methods of rare earth element of Sync enrichment in a kind of roasted ore from rare earth sulfuric acid according to claim 1, its
It is characterised by, a solution mixes with b solution and shaken up vibration in the step (3), in b solution Rare Earth Ion and a solution
The mass concentration ratio of TODGA is 1：(1~13), duration of oscillation is 3 minutes/time, and extraction times are 1~9 time, organic phase and water phase
Extraction volume ratio is 1：(0.3~3).
6. 14 kinds of methods of rare earth element of Sync enrichment in a kind of roasted ore from rare earth sulfuric acid according to claim 1, its
It is characterised by, the back extraction condition of stripping process is c solution and having collected by extraction in step (3) in the step (4)
The volume ratio of machine phase is 1：(0.3~3), minute/time of duration of oscillation 3, back extraction number of times is 1~9 time；Deionized water and step
(3) volume ratio of the organic phase in collected by extraction is (0.5~3)：1, minute/time of duration of oscillation 3, back extraction number of times is 1
~4 times, order is used not fix as c solution and the deionized water of water phase.
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Application publication date: 20170613 |