CN105624439A - Method for separating low-concentration rare earth ions by using magnetic fluid extraction agent - Google Patents
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Abstract
The invention discloses a method for separating low-concentration rare earth ions by using a magnetic fluid extraction agent. The method mainly comprises the following several steps: preparing the magnetic fluid extraction agent with super paramagnetism; building a magnetic fluid fixed bed device; and extracting and separating the low-concentration rare earth ions. The method has the following innovative points: the advantages of a solvent extraction separation mode and a fixed bed separation mode are integrated, the magnetic fluid extraction agent with super paramagnetism is prepared, a brand-new integrative innovation separation mode is disclosed, the separation mode overcomes the disadvantages of the solvent extraction and the fixed bed, the respective advantages are exerted, and the brand-new integrative innovation separation mode is a brand-new separation technology.
Description
Technical field
The invention belongs to separation method, a kind of method being specifically related to magnetic fluid extractant separating low concentration rare earth ion.
Background technology
The waste water middle rare earth concentration relatively low (5-200mg/L) of the leaching ore deposit tail washings of Rare-earth Mine, leachate and the discharge of Rare Earth Separation enterprise. along with riseing year by year of rare earth price, the loss of these low concentration of rare earth solution, not only waste the resource of preciousness, and cause serious environmental pollution. but, at present these large volumes, low concentration rare earth resources be effectively enriched with reclaim also highly difficult. conventional separation techniques separates and recovers the method for rare earth ion from aqueous phase mainly has liquid liquid solvent extraction (referring to XiaoweiHuang, HongweiLi, XiangxinXue, etal.Developmentstatusandresearchprogressinrareearthhydr ometallurgyinChina.JournalofRareEarths.24 (2): 129-133, 2006.), ion exchange and absorption are (referring to HalinaHubicka, DorotaKolcodynska.Separationofrare-earthelementcomplexes withtrans-1, 2-diaminocyclohexane-N, N, N ', N '-tetraaceticacidonpolyacrylateanionexchangers.Hydrometall urgy.71:343-350, 2004.) etc. solvent extraction loading capacity is big, mass transfer velocity is fast, obtains extensive use in hydrometallurgy industry, but when being used for processing low concentration of rare earth ion waste liquid, has that emulsifying is serious, solvent and an extractant loss and cause secondary pollution problems. solid phase particles is generally deposited in cylinder with absorption by ion exchange, lock out operation is realized by solid-liquid interface absorption in the way of fixing bed, but this method is due to the restriction by solid phase particles specific surface area, adsorption capacity is little, cycle length needs frequent elution action, and hole inner transmission matter speed causes that liquid handling amount is low slowly.
In recent years, many new methods being used for recycling metal ion waste liquid are suggested (referring to Li Jie, Jiang Shuanying, Dong Bin. low-concentration metallic ion waste water Processing Technology Research is in progress. and Treatment of Industrial Water .30 (2): 15-19,2010.), its attention is exactly magnetic separation technique. for liquid liquid solvent extraction, the clastotypes such as bed Problems existing in recycling is containing low concentration of rare earth metal ion waste liquid process is fixed in ion exchange with absorption, in magnetic fluid technology of preparing (referring to OdenbachStefan.Magneticfluids.AdvancesinColloidandInterf aceScience.46:263.1993.) and high gradient magnetic separation theorem (referring to WatsonJHP.MagneticFiltration.JournalofAppliedPhysics.44: 4209, 1973.) basis on, the present invention is in conjunction with the advantage of solvent extraction and two kinds of clastotypes of fixing bed, it is prepared for the magnetic fluid extractant with superparamagnetism, and propose a brand-new integrated innovation clastotype, i.e. " magnetic fluid fixes bed extract and separate ", this clastotype overcomes solvent extraction and the shortcoming of fixing bed, play respective advantage, it it is a brand-new isolation technics.
Summary of the invention
For the conventional separation techniques limitation to low concentration of rare earth ion processing aspect, the invention provides a kind of brand-new separation method for low concentration of rare earth ion.
A kind of method of magnetic fluid extractant separating low concentration rare earth ion, comprises the following steps:
1) being coated with the inorganic magnetic even particulate dispersion of coupling agent in the mixing organic facies of extractant and diluent, preparation has the magnetic fluid extractant of superparamagnetism;
2) being uniformly filled in inside magnetic separating device by ferrimagnet, then pour in magnetic separating device by described magnetic fluid extractant, under uniform high gradient background magnetic field, magnetic fluid extractant is magnetized and is fixed on ferrimagnet surface;
3) low concentration of rare earth solion is at the uniform velocity by inside magnetic separating device, and the rare earth ion in solution is extracted by magnetic fluid extractant and is enriched with.
Wherein, described step 1) in, described inorganic magnetic granule is Fe3O4����-Fe2O3��CoFe2O4��FexOne or more in N, specific saturation magnetization is 2��20emu/g; It is preferably Fe3O4��
Wherein, described step 1) in, described coupling agent is the one in linoleic acid, oleic acid, linolenic acid; It is preferably oleic acid.
Wherein, described step 1) in, described extractant is the one in P507, P204, TBP, aphthenic acids, and diluent is kerosene, and in mixing organic facies, extractant volume content is 10��60%.
Wherein, described step 2) in, described ferrimagnet is the one in steel wire, steel ball, steel nail.
Wherein, described step 2) in, the magnetic field intensity of described uniform high gradient background magnetic field is 1500��6000 Gausses.
Wherein, described step 3) in, described low concentration of rare earth solion Rare Earth Ion concentration is 1��2000mg/L; Preferred rare earth ion concentration is 5��500mg/L.
Wherein, described step 3) in, described low concentration of rare earth solion pH value is 1��7; Preferable ph is 2��5.
Wherein, described step 3) in, described low concentration of rare earth solion is 5��20mm/min in magnetic separating device internal flow linear velocity.
Wherein, described step 3) in, described low concentration of rare earth solion temperature is 10��60 DEG C; Preferable temperature is 20��40 DEG C.
Wherein, one or more in the waste water of the leaching ore deposit tail washings of Rare-earth Mine, leachate or the discharge of Rare Earth Separation enterprise of described low concentration of rare earth ion source.
Wherein, step 1) in the mass ratio of coupling agent and inorganic magnetic granule be 0.1��0.5.
Wherein, step 1) in the solid content of magnetic fluid extractant be 5��40wt%.
Wherein, step 2) in the filling rate of magnetic fluid extractant be 15��40%.
Rare earth ion handled by the present invention derives from the waste water of the leaching ore deposit tail washings of Rare-earth Mine, leachate and the discharge of Rare Earth Separation enterprise, the features such as it is relatively low that it has rare earth concentration, and impurity is more; The processing-waste that all the other numerous electrolysis waste solutions discharged in Course of Mining and processing of ornament factory discharge, the precious metal ion contained has bigger difference, and the two all has bigger difference in dopant species, content, solution ph etc.
The present invention character feature according to rare-earth ion solution, by adjusting solution ph, temperature, multiple parameter such as concentration and flowing velocity, optimum organization, advantage in combination with solvent extraction and two kinds of clastotypes of fixing bed, by regulating and controlling the material rate relation of the magnetic fluid extractant of preparation superparamagnetism, process magnetic field intensity, the parameters such as raw material type, it is prepared for the magnetic fluid extractant with superparamagnetism, and propose a brand-new integrated innovation clastotype, i.e. " magnetic fluid fixes bed extract and separate ", this clastotype overcomes solvent extraction and the shortcoming of fixing bed, play respective advantage, it it is a brand-new isolation technics.
Detailed description of the invention
Detailed description of the invention below in conjunction with the application, the technical scheme of the application is described in detail, but below embodiment is only understand the present invention, and the application can not be limited, embodiment in the application and the feature in embodiment can be mutually combined, and the multitude of different ways that the application can be defined by the claims and cover is implemented.
Embodiment 1
1) adopt coprecipitation to prepare Surface coating and have the Fe of oleic acid3O4Granule, wherein Fe3O4The specific saturation magnetization of granule is 9.5emu/g, is dispersed in the mixing organic facies of P507 and kerosene, prepares magnetic fluid extractant, and solid content is 5wt%, and wherein in organic facies, P507 volume content is 50%, wherein the addition of oleic acid and Fe3O4Mass ratio between granule is 0.1;
2) steel wire of string diameter 0.5mm, grid 4mm �� 4mm is filled at magnetic separating device inner homogeneous, then magnetic fluid extractant is poured into the uniform high gradient background magnetic field being placed in 3500 Gausses in magnetic separating device, magnetic fluid extractant is magnetized and is fixed on steel wire surface, and wherein the filling rate of magnetic fluid is 15%;
3) by pH=2.5, temperature be 30 DEG C, the La of 12mg/L3+Solution is at the uniform velocity by inside magnetic separating device, and solution linear rate of flow is 10mm/min, La in solution3+Extraction yield reach 95%.
Embodiment 2
1) adopt coprecipitation to prepare Surface coating and have the Fe of oleic acid3O4Granule, wherein Fe3O4The specific saturation magnetization of granule is 2emu/g, is dispersed in the mixing organic facies of P507 and kerosene, prepares magnetic fluid extractant, and solid content is 5wt%, and wherein in organic facies, P507 volume content is 10%, wherein the addition of oleic acid and Fe3O4Mass ratio between granule is 0.1;
2) steel wire of string diameter 0.5mm, grid 4mm �� 4mm is filled at magnetic separating device inner homogeneous, then magnetic fluid extractant is poured into the uniform high gradient background magnetic field being placed in 1500 Gausses in magnetic separating device, magnetic fluid extractant is magnetized and is fixed on steel wire surface, and wherein the filling rate of magnetic fluid is 15%;
3) by pH=1, temperature be 10 DEG C, the La of 1mg/L3+Solution is at the uniform velocity by inside magnetic separating device, and solution linear rate of flow is 5mm/min, La in solution3+Extraction yield reach 96%.
Embodiment 3
1) adopt coprecipitation to prepare Surface coating and have the Fe of oleic acid3O4Granule, specific saturation magnetization is 15emu/g, is dispersed in the mixing organic facies of P507 and kerosene, prepares magnetic fluid extractant, and solid content is 15wt%, and wherein in organic facies, P507 volume content is 30%, wherein the addition of oleic acid and Fe3O4Mass ratio between granule is 0.3;
2) steel wire of string diameter 0.5mm, grid 4mm �� 4mm is filled at magnetic separating device inner homogeneous, then magnetic fluid extractant is poured into the uniform high gradient background magnetic field being placed in 3500 Gausses in magnetic separating device, magnetic fluid extractant is magnetized and is fixed on steel wire surface, and wherein the filling rate of magnetic fluid is 30%;
3) by pH=4, temperature be 30 DEG C, the La of 100mg/L3+Solution is at the uniform velocity by inside magnetic separating device, and solution linear rate of flow is 10mm/min, La in solution3+Extraction yield reach 94%.
Embodiment 4
1) adopt coprecipitation to prepare Surface coating and have the Fe of oleic acid3O4Granule, specific saturation magnetization is 20emu/g, is dispersed in the mixing organic facies of P507 and kerosene, prepares magnetic fluid extractant, and solid content is 40wt%, and wherein in organic facies, P507 volume content is 60%, wherein the addition of oleic acid and Fe3O4Mass ratio between granule is 0.5;
2) steel wire of string diameter 0.5mm, grid 4mm �� 4mm is filled at magnetic separating device inner homogeneous, then magnetic fluid extractant is poured into the uniform high gradient background magnetic field being placed in 6000 Gausses in magnetic separating device, magnetic fluid extractant is magnetized and is fixed on steel wire surface, and wherein the filling rate of magnetic fluid is 40%;
3) by pH=7, temperature be 60 DEG C, the La of 2000mg/L3+Solution is at the uniform velocity by inside magnetic separating device, and solution linear rate of flow is 20mm/min, La in solution3+Extraction yield reach 95%.
Embodiment 5
1) adopt coprecipitation to prepare Surface coating and have the ��-Fe of oleic acid2O3Granule, specific saturation magnetization is 15emu/g, is dispersed in the mixing organic facies of P204 and kerosene, prepares magnetic fluid extractant, and solid content is 25wt%, and wherein in organic facies, P204 volume content is 30%, wherein the addition of oleic acid and ��-Fe2O3Mass ratio between granule is 0.3;
2) steel wire of string diameter 0.5mm, grid 4mm �� 4mm is filled at magnetic separating device inner homogeneous, then magnetic fluid extractant is poured into the uniform high gradient background magnetic field being placed in 3500 Gausses in magnetic separating device, magnetic fluid extractant is magnetized and is fixed on steel wire surface, and wherein the filling rate of magnetic fluid is 30%;
3) by pH=4, temperature be 30 DEG C, the La of 100mg/L3+Solution is at the uniform velocity by inside magnetic separating device, and solution linear rate of flow is 10mm/min, La in solution3+Extraction yield reach 94%.
Embodiment 6
1) adopt coprecipitation to prepare Surface coating and have linolenic ��-Fe2O3Granule, specific saturation magnetization is 15emu/g, is dispersed in the mixing organic facies of TBP and kerosene, prepares magnetic fluid extractant, and solid content is 30wt%, and wherein in organic facies, TBP volume content is 30%, wherein linolenic addition and ��-Fe2O3Mass ratio between granule is 0.3;
2) steel wire of string diameter 0.5mm, grid 4mm �� 4mm is filled at magnetic separating device inner homogeneous, then magnetic fluid extractant is poured into the uniform high gradient background magnetic field being placed in 3500 Gausses in magnetic separating device, magnetic fluid extractant is magnetized and is fixed on steel wire surface, and wherein the filling rate of magnetic fluid is 30%;
3) by pH=4, temperature be 30 DEG C, the La of 100mg/L3+Solution is at the uniform velocity by inside magnetic separating device, and solution linear rate of flow is 10mm/min, La in solution3+Extraction yield reach 97%.
Embodiment 7
1) adopt coprecipitation to prepare Surface coating and have linolenic CoFe2O4Granule, specific saturation magnetization is 15emu/g, is dispersed in the mixing organic facies of TBP and kerosene, prepares magnetic fluid extractant, and solid content is 35wt%, and wherein in organic facies, TBP volume content is 30%, wherein linolenic addition and CoFe2O4Mass ratio between granule is 0.3;
2) steel wire of string diameter 0.5mm, grid 4mm �� 4mm is filled at magnetic separating device inner homogeneous, then magnetic fluid extractant is poured into the uniform high gradient background magnetic field being placed in 3500 Gausses in magnetic separating device, magnetic fluid extractant is magnetized and is fixed on steel wire surface, and wherein the filling rate of magnetic fluid is 30%;
3) by pH=4, temperature be 30 DEG C, the La of 100mg/L3+Solution is at the uniform velocity by inside magnetic separating device, and solution linear rate of flow is 10mm/min, La in solution3+Extraction yield reach 96%.
Embodiment 8
1) adopt coprecipitation to prepare Surface coating and have linoleic FexN granule, specific saturation magnetization is 15emu/g, is dispersed in the mixing organic facies of aphthenic acids and kerosene, prepares magnetic fluid extractant, and solid content is 5wt%, and wherein in organic facies, aphthenic acids volume content is 30%, wherein linoleic addition and FexMass ratio between N granule is 0.3;
2) steel wire of string diameter 0.5mm, grid 4mm �� 4mm is filled at magnetic separating device inner homogeneous, then magnetic fluid extractant is poured into the uniform high gradient background magnetic field being placed in 3500 Gausses in magnetic separating device, magnetic fluid extractant is magnetized and is fixed on steel wire surface, and wherein the filling rate of magnetic fluid is 30%;
3) by pH=4, temperature be 30 DEG C, the La of 100mg/L3+Solution is at the uniform velocity by inside magnetic separating device, and solution linear rate of flow is 10mm/min, La in solution3+Extraction yield reach 93%.
Embodiment 9
1) adopt coprecipitation to prepare Surface coating and have linolenic Fe3O4Granule, specific saturation magnetization is 9.5emu/g, is dispersed in the mixing organic facies of TBP and kerosene, prepares magnetic fluid extractant, and solid content is 40wt%, and wherein in organic facies, TBP volume content is 50%, wherein linolenic addition and Fe3O4Mass ratio between granule is 0.1;
2) steel wire of string diameter 0.5mm, grid 4mm �� 4mm is filled at magnetic separating device inner homogeneous, then magnetic fluid extractant is poured into the uniform high gradient background magnetic field being placed in 3500 Gausses in magnetic separating device, magnetic fluid extractant is magnetized and is fixed on steel wire surface, and wherein the filling rate of magnetic fluid is 15%;
3) by pH=2.5, temperature be 30 DEG C, the La of 12mg/L3+Solution is at the uniform velocity by inside magnetic separating device, and solution linear rate of flow is 10mm/min, La in solution3+Extraction yield reach 94%.
Comparative example 1
1) adopt coprecipitation to prepare Surface coating and have the Fe of oleic acid3O4Granule, specific saturation magnetization is 15emu/g, is dispersed in the mixing organic facies of P507 and kerosene, prepares magnetic fluid extractant, and solid content is 5wt%, and wherein in organic facies, P507 volume content is 8%, wherein the addition of oleic acid and Fe3O4Mass ratio between granule is 0.3;
2) steel wire of string diameter 0.5mm, grid 4mm �� 4mm is filled at magnetic separating device inner homogeneous, then magnetic fluid extractant is poured into the uniform high gradient background magnetic field being placed in 3500 Gausses in magnetic separating device, magnetic fluid extractant is magnetized and is fixed on steel wire surface, and wherein the filling rate of magnetic fluid is 30%;
3) by pH=4, temperature be 30 DEG C, the La of 100mg/L3+Solution is at the uniform velocity by inside magnetic separating device, and solution linear rate of flow is 10mm/min, La in solution3+Extraction yield reach 74%.
Comparative example 2
1) adopt coprecipitation to prepare Surface coating and have the Fe of oleic acid3O4Granule, specific saturation magnetization is 15emu/g, is dispersed in the mixing organic facies of P507 and kerosene, prepares magnetic fluid extractant, and solid content is 5wt%, and wherein in organic facies, P507 volume content is 65%, wherein the addition of oleic acid and Fe3O4Mass ratio between granule is 0.3;
2) steel wire of string diameter 0.5mm, grid 4mm �� 4mm is filled at magnetic separating device inner homogeneous, then magnetic fluid extractant is poured into the uniform high gradient background magnetic field being placed in 3500 Gausses in magnetic separating device, magnetic fluid extractant is magnetized and is fixed on steel wire surface, and wherein the filling rate of magnetic fluid is 30%;
3) by pH=4, temperature be 30 DEG C, the La of 100mg/L3+Solution is at the uniform velocity by inside magnetic separating device, and solution linear rate of flow is 10mm/min, La in solution3+Extraction yield reach 70%.
Comparative example 3
1) adopt coprecipitation to prepare Surface coating and have the ��-Fe of oleic acid2O3Granule, specific saturation magnetization is 15emu/g, is dispersed in the mixing organic facies of P204 and kerosene, prepares magnetic fluid extractant, and solid content is 25wt%, and wherein in organic facies, P204 volume content is 30%, wherein the addition of oleic acid and ��-Fe2O3Mass ratio between granule is 0.05;
2) steel wire of string diameter 0.5mm, grid 4mm �� 4mm is filled at magnetic separating device inner homogeneous, then magnetic fluid extractant is poured into the uniform high gradient background magnetic field being placed in 3500 Gausses in magnetic separating device, magnetic fluid extractant is magnetized and is fixed on steel wire surface, and wherein the filling rate of magnetic fluid is 30%;
3) by pH=4, temperature be 30 DEG C, the La of 100mg/L3+Solution is at the uniform velocity by inside magnetic separating device, and solution linear rate of flow is 10mm/min, La in solution3+Extraction yield reach 83%.
Comparative example 4
1) adopt coprecipitation to prepare Surface coating and have the ��-Fe of oleic acid2O3Granule, specific saturation magnetization is 15emu/g, is dispersed in the mixing organic facies of P204 and kerosene, prepares magnetic fluid extractant, and solid content is 25wt%, and wherein in organic facies, P204 volume content is 30%, wherein the addition of oleic acid and ��-Fe2O3Mass ratio between granule is 0.6;
2) steel wire of string diameter 0.5mm, grid 4mm �� 4mm is filled at magnetic separating device inner homogeneous, then magnetic fluid extractant is poured into the uniform high gradient background magnetic field being placed in 3500 Gausses in magnetic separating device, magnetic fluid extractant is magnetized and is fixed on steel wire surface, and wherein the filling rate of magnetic fluid is 30%;
3) by pH=4, temperature be 30 DEG C, the La of 100mg/L3+Solution is at the uniform velocity by inside magnetic separating device, and solution linear rate of flow is 10mm/min, La in solution3+Extraction yield reach 80%.
By above-mentioned comparative example it can be seen that comparative example 1-2 and embodiment 3 are the same from situation in all the other conditions, in organic facies, P507 volume content is different, La in last solution3+Extraction yield difference relatively big, the extraction of embodiment 3 is substantially better than comparative example 1-2; Comparative example 3-4 and embodiment 5 are the same from situation in all the other conditions, the addition of oleic acid and ��-Fe2O3Mass ratio between granule is different, La in last solution3+Extraction yield difference relatively big, the extraction of embodiment 5 is substantially better than comparative example 3-4, it can be seen that, in mixing organic facies, last result is had more significant impact with the mass ratio of coupling agent with inorganic magnetic granule by extractant volume content.
These are only the preferred embodiments of the present invention, be not limited to the present invention, to those skilled in the art, the present invention can have various change and conversion. All within the spirit and principles in the present invention, any amendment of making, equivalent replacement, improvement etc., should be included within protection scope of the present invention.
Claims (14)
1. the method for a magnetic fluid extractant separating low concentration rare earth ion, it is characterised in that comprise the following steps:
1) being coated with the inorganic magnetic even particulate dispersion of coupling agent in the mixing organic facies of extractant and diluent, preparation has the magnetic fluid extractant of superparamagnetism;
2) being uniformly filled in inside magnetic separating device by ferrimagnet, then pour in magnetic separating device by described magnetic fluid extractant, under uniform high gradient background magnetic field, magnetic fluid extractant is magnetized and is fixed on ferrimagnet surface;
3) low concentration of rare earth solion is at the uniform velocity by inside magnetic separating device, and the rare earth ion in solution is extracted by magnetic fluid extractant and is enriched with.
2. method according to claim 1, it is characterised in that described step 1) in, described inorganic magnetic granule is Fe3O4����-Fe2O3��CoFe2O4��FexOne or more in N, specific saturation magnetization is 2��20emu/g; It is preferably Fe3O4��
3. according to the arbitrary described method of claim 1-2, it is characterised in that described step 1) in, described coupling agent is the one in linoleic acid, oleic acid, linolenic acid; It is preferably oleic acid.
4. according to the arbitrary described method of claim 1-3, it is characterised in that described step 1) in, described extractant is the one in P507, P204, TBP, aphthenic acids, and diluent is kerosene, and in mixing organic facies, extractant volume content is 10��60%.
5. according to the arbitrary described method of the claims, it is characterised in that described step 2) in, described ferrimagnet is the one in steel wire, steel ball, steel nail.
6. according to the arbitrary described method of the claims, it is characterised in that described step 2) in, the magnetic field intensity of described uniform high gradient background magnetic field is 1500��6000 Gausses.
7. according to the arbitrary described method of the claims, it is characterised in that described step 3) in, described low concentration of rare earth solion Rare Earth Ion concentration is 1��2000mg/L; Preferred rare earth ion concentration is 5��500mg/L.
8. according to the arbitrary described method of the claims, it is characterised in that described step 3) in, described low concentration of rare earth solion pH value is 1��7; Preferable ph is 2��5.
9. according to the arbitrary described method of the claims, it is characterised in that described step 3) in, described low concentration of rare earth solion is 5��20mm/min in magnetic separating device internal flow linear velocity.
10. according to the arbitrary described method of the claims, it is characterised in that described step 3) in, described low concentration of rare earth solion temperature is 10��60 DEG C; Preferable temperature is 20��40 DEG C.
11. according to the arbitrary described method of the claims, it is characterised in that one or more in the waste water of the leaching ore deposit tail washings of Rare-earth Mine, leachate or the discharge of Rare Earth Separation enterprise of described low concentration of rare earth ion source.
12. according to the arbitrary described method of the claims, it is characterised in that step 1) in the mass ratio of coupling agent and inorganic magnetic granule be 0.1��0.5.
13. according to the arbitrary described method of the claims, it is characterised in that step 1) in the solid content of magnetic fluid extractant be 5��40wt%.
14. according to the arbitrary described method of the claims, it is characterised in that step 2) in the filling rate of magnetic fluid extractant be 15��40%.
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| CN105624439B (en) | 2017-11-10 |
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