CN104073634B - A kind of method of nickel minerals leachate or electrolytic anode liquid deironing - Google Patents
A kind of method of nickel minerals leachate or electrolytic anode liquid deironing Download PDFInfo
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- CN104073634B CN104073634B CN201410260055.6A CN201410260055A CN104073634B CN 104073634 B CN104073634 B CN 104073634B CN 201410260055 A CN201410260055 A CN 201410260055A CN 104073634 B CN104073634 B CN 104073634B
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Abstract
The invention discloses a kind of nickel minerals leachate or the method for electrolytic anode liquid deironing, the method comprises the following steps: adopt homogeneous crystallization process to prepare nano-magnetic crystal seed, induce the iron ion hydrolysis crystallization in leachate or electrolytic anode liquid with nano-magnetic crystal seed for seed crystal, grow up, and by the arrangement of externally-applied magnetic field induced crystal structure direction, crystallized product is made not only to have bigger granularity, and there is stronger magnetic, the separation of iron ion hydrolyzate is realized finally by magnetic separation technique.The method achieve quick, the high efficiency separation of iron ion in nickel minerals leachate or electrolytic anode liquid, be effectively increased resource utilization, and equipment and flow operations is simple, economical and efficient, meet industrialized production.
Description
Technical field
The invention belongs to technical field of resource comprehensive utilization, be specifically related to a kind of nickel minerals leachate or the method for electrolytic anode liquid deironing.
Background technology
In hydrometallurgy process, being frequently used acid solution leaching Ore, the ferrum in mineral is often enter solution with trivalent or divalent ion form.Owing to ferrum exists bigger harm when carrying out the subsequent techniques such as electro-deposition, therefore deironing is one procedure the most general and important in hydrometallurgy.For ferrum heavy in the solution high from iron content, since the end of the sixties in last century, jarosite process, goethite process, hematite process successively industrially obtain application as new heavy ferrum method.
Ihleite is a kind of sulfate mineral, and its crystal is only small and very rare, has glassy lustre.Ihleite is pure faint yellow or yellow, belongs to hexagonal crystal system, tabular or false cube Alumen stone-type structure, cell parameter a=0.721nm, e=1.703nm, Z=3.The molecular formula of ihleite can be write as A2[Fe6(S04)4(OH)12] or AFe3(S04)2(OH)6, or A20·3Fe203·4S03·6H20, monovalent cation A both can be K+, Na+, NH4 +, it is also possible to it is Ag+、Rb+、1/2Pb2+Deng.Such as: yellow ammonia siderotil:；Autunezite:；Sodium jarosite:；Carphosiderite:.When processing the nickelic scum of nickle electrolysis anode solution neutralizing hydrolysis deironing institute output, adopt the oxidation autunezite deironing of sulfuric acid dissolution sodium chlorate.Although siderotil class scum stable components, sedimentation, filtration and scourability are good, and solid-liquor separation easily carries out, good iron removal effect.But the autunezite quantity of slag is big, and sulfuric acid consumption is many, scum bulk deposition, takies a large amount of land resource, and environmental pollution is serious.
Goethite process starts from nineteen seventies, and by the development of balun factory of Laoshan company of Belgium and application, 1973, China proceeded by goethite process experimental study, and in nineteen ninety-five in smeltery of Shuikoushan Mining Bureau the 4th input commercial production.Goethite process has very big advantage compared to jarosite process, and first goethite process is suitable for multiple acid medium leachate (sulphuric acid, hydrochloric acid, nitric acid etc.), and secondly temperature and pressure are required relatively low by deironing operation.Iron ion its precipitation form in different systems is different, and in sulfate liquor, iron ion mainly precipitates with alpha-feooh form, and main with β-FeOOH form precipitation in hydrochloric acid medium.
Fe203-H20 balance chart being shows: goethitum is only at Fe3+Could generate when concentration is very low, therefore Fe3+Want to precipitate with goethitum alpha-feooh form, it is necessary to assure Fe3+Concentration maintains very low state all the time.The clearance of iron ion in wet-process metallurgy leachate, depends on formed resolution of precipitate degree, and sedimentary dissolubility depends on the dissolubility of eutectic mixture in mixture.Ferrum compound thermodynamic study shows: only as the Fe in solution3+When concentration is reduced to certain value, goethite precipitation is only possible to formation.
Hematite precipitation is with α-Fe203With γ-Fe203Two kinds of crystal forms exist.Natural hematite belongs to α-Fe in chemical composition and structure203, crystal belongs to trigonal system, is paramagnetic, and γ-Fe203It it is ferromagnetism.In iron ion hydrolytic precipitation process, what be initially formed is the compound of similar goethitum, continues and is transformed into turgite (α-Fe2030.5H20) third level product γ type bloodstone, is ultimately formed.Fe203-S03-H2In 0 system, the isothermal line under 200 DEG C of high temperature shows: under 200 DEG C of conditions, and iron ion major part is with Fe203Form Precipitation.
These methods, while the solid-liquid separation problem substantially solved in hydrometallurgy, the precipitated crystal of ferrum is good, and to dissolved ferric iron quantitative limitation when can cancel leaching.But all there is respective defect in them: the shortcoming of ihleite method is that the quantity of slag is big, and Iron grade is low, and sulfuric acid consumption is more；Goethite process is characterized by and makes ferric ion concentration in solution keep reduced levels in precipitation process, and as lower than lg/L, this process efficiency is relatively low, the feed liquid of filtration is relatively big, and power consumption is big, and acid balance is difficult to grasp, and acid, alkali consumption are relatively big, and equipment is complex；What hematite process deironing was the most attractive is that this method deironing scum amount is few, and iron content is higher, but needs higher ph, and energy consumption is the highest, and steam consumption quantity accounts for full factory 60%.
Therefore, accelerate the separation of ferrum in leachate, the utilization rate improving precipitation slag to work out a kind of to the effective method of separation of iron ion in nickel minerals leachate, electrolytic anode liquid and technique targetedly, makes environmental benefit, economic benefit and social benefit three unified.
Summary of the invention
The technical problem to be solved be provide for above-mentioned deficiency of the prior art a kind of energy quickly, iron ion obtains high-grade scum in high efficiency separation nickel minerals leachate or electrolytic anode liquid method, the method process is simple, easy to operate, meets industrialized production.
Technical problem for solving the present invention adopts the following technical scheme that
A kind of method of nickel minerals leachate or electrolytic anode liquid deironing, comprises the following steps:
Step 1:
Prepare nano-magnetic crystal seed
It is dissolved in distilled water after Fe (II) salt and Fe (III) salt are weighed mixing for the ratio of 1:1 in molar ratio, stirring and dissolving, the solution after dissolving adds rare H2SO4Solution makes pH value of solution less than 3.0, is subsequently adding surfactant polyethylene, and the mixed solution obtained fully is dissolved in stirring, the mixed solution obtained is put in 50-60 DEG C of water-bath, using NaOH solution or ammonia as nertralizer, making pH value of solution is 11, continues to keep mixed solution at 50-60 DEG C, high-speed stirred reacts 0.5-1h, then obtaining solid particle with magnetic field separation, solid particle is dry 3-4h in vacuum drying oven, grinds, encapsulation, namely obtains nano-magnetic crystal seed；
Step 2:
Magnetic field and crystal seed induction crystallization
Nickel minerals leachate or electrolytic anode liquid is added in the crystallization reaction still being covered with the vertical magnetic field of 800-1200GS, nickel minerals leachate or electrolytic anode liquid temp control at 80-90 DEG C, it is subsequently adding the magnetic crystal seed that step 1 obtains to be stirred, the addition weight of described magnetic crystal seed is identical with iron ion weight in leachate or electrolytic anode liquid, oxidant is added again in crystallization reaction still, making the mol ratio of Fe (II) and Fe (III) in nickel minerals leachate or electrolytic anode liquid is 1:2, the most backward described nickel minerals leachate or electrolytic anode liquid add sodium carbonate, sodium bicarbonate, nickelous carbonate, sodium hydroxide, a kind of neutralization in nickel hydroxide, making pH is 3.0-4.0, iron ion is promoted at magnetic seed surface crystallization and to align, the time of reaction is that 1-2h obtains ore pulp；
Step 3:
The magnetic flocculation of non magnetic or sub magnetic debris
Flocculant is added in the ore pulp of step 2 gained, the addition weight of described flocculant is every liter of nickel minerals leachate or electrolytic anode liquid addition 10-100mg so that the non magnetic or weak magnetic subparticle that hydrolytic process produces and magnetic-particle flocculation, coalescence formation magnetic floc sedimentation；
Step 4:
The magnetic separation of scum separates
The ore pulp of step 3 gained is proceeded in magnetic separator, it is achieved being separated efficiently and rapidly of scum.
Raw material Fe (II) salt of nano-magnetic crystal seed and Fe (III) salt respectively FeSO in described step 14And Fe2(SO4)3, described Fe (II) salt and Fe (III) salt are 10:10:1 with surfactant polyethylene mol ratio.
The oxidant of described step 2 is the one in hydrogen peroxide, air, oxygen, ozone, sodium peroxydisulfate.
In described step 3, flocculant is non-ionic polyacrylamide or aluminium polychlorid or bodied ferric sulfate.
In described step 4, magnetic separator separation magnetic field intensity is 400-600GS.
Beneficial effects of the present invention: magnetic field and magnetic crystal seed are induced iron ion hydrolysis crystallization technique to be incorporated in nickel hydrometallurgy purification technique by the technique of the present invention first, hydrolyzate is not only made to have bigger granularity, and there is stronger magnetic, in conjunction with flocculant or flocculation aid, sub magnetic debris and non-magnetic particle are carried out net and catch flocculation, realize intergranular magnetic coagulation, by magnetic field separation ferrum slag, gained scum has higher grade, and clear liquid iron content is low, valuable metal is almost without loss, what be truly realized in nickel minerals leachate or electrolytic anode liquid iron ion is quick, high efficiency separation, it is effectively increased resource utilization.The magnetic crystal seed preparation method that the present invention adopts easily, inexpensively economical, equipment, flow process, simple to operate, economical and efficient, meet industrialized production.
Detailed description of the invention
Following example are further intended to present invention is described, rather than limit the scope of the invention.
Embodiment 1
This process is utilized to process Fe2+Mass concentration is the nickel minerals leachate of 5.6g/L.
Prepare nano-magnetic crystal seed: weigh 1molFeSO respectively4And 1molFe2(SO4)3It is dissolved in 1L distilled water and mixes, stirring and dissolving, add appropriate rare H2SO4Solution, make pH value of solution less than 3.0, add surfactant polyethylene 0.1mol, stirring 5min fully dissolves, the mixed solution obtained is put in 60 DEG C of water-baths, using NaOH solution as nertralizer, being slowly dropped into pH value of solution=ll with dropper, continue to keep solution at 60 DEG C, high-speed stirred reacts 1h, mixing speed is 800r/min, then obtaining solid particle with the magnetic field separation that magnetic field intensity is 500GS, solid particle is dry 3h in vacuum drying oven, grinds, encapsulation, namely obtains nano-magnetic crystal seed.
1L nickel minerals leachate is added in deironing crystallization reaction still, add 5.6g nano-magnetic crystal seed, the air passing into compression in nickel minerals leachate makes the mol ratio of Fe (II) and Fe (III) in nickel minerals leachate be 1:2, controlling nickel minerals leachate temperature is 85 DEG C, regulating the crystallization reaction still internal magnetic field intensity being covered with vertical magnetic field is 1000GS, mixing speed 800r/min, the nertralizer sodium hydroxide solution that molar concentration is 4mol/L slowly it is continuously added in reactor, controlling reaction pH is 4.0, reaction 1h, reaction adds 10mg non-ionic polyacrylamide after terminating and carries out magnetic flocculation, non magnetic or the weak magnetic subparticle that hydrolytic process produces is flocculated with magnetic-particle, coalescence forms magnetic floc sedimentation, by magnetic separator separation scum that magnetic field intensity is 500GS after having flocculated.
Table 1 is the present embodiment nickel minerals leachate deironing result of the test
Embodiment 2:
This process is utilized to process Fe2+Content is the nickel minerals leachate of 15.56g/L.
Prepare nano-magnetic crystal seed: weigh 1molFeSO respectively4And 1molFe2(SO4)3It is dissolved in 1L distilled water and mixes, stirring and dissolving, add appropriate rare H2SO4Solution, make pH value of solution less than 3.0, add surfactant polyethylene 0.1mol, stirring 5min fully dissolves, the mixed solution obtained is put in 50 DEG C of water-baths, using ammonia as nertralizer, being slowly dropped into pH value of solution=ll with dropper, continue to keep solution at 50 DEG C, high-speed stirred reacts 0.5h, mixing speed is 1000r/min, then obtaining solid particle with the magnetic field separation of magnetic field intensity 600GS, solid particle is dry 4h in vacuum drying oven, grinds, encapsulation, namely obtains nano-magnetic crystal seed.
1L nickel minerals leachate is added in deironing crystallization reaction still, add 15.56g nano-magnetic crystal seed, adding the hydrogen peroxide that mass fraction is 30% in nickel minerals leachate makes the mol ratio of Fe (II) and Fe (III) in nickel minerals leachate be 1:2, controlling nickel minerals leachate temperature is 80 DEG C, regulating the crystallization reaction still internal magnetic field intensity being covered with vertical magnetic field is 800GS, mixing speed 800r/min, nertralizer sodium carbonate liquor slowly it is continuously added in reactor, controlling reaction pH is 3.0, , reaction 2h, reaction adds 50mg aluminium polychlorid after terminating and carries out magnetic flocculation, non magnetic or the weak magnetic subparticle that hydrolytic process produces is flocculated with magnetic-particle, coalescence forms magnetic floc sedimentation, by magnetic separator separation scum that magnetic field intensity is 600GS after having flocculated.
Table 2 is the present embodiment nickel minerals leachate deironing result of the test
Embodiment 3:
This process is utilized to process Fe2+The nickel minerals electrolytic anode liquid of content 0.54g/L.
Prepare nano-magnetic crystal seed: weigh 1molFeSO respectively4And 1molFe2(SO4)3It is dissolved in 1L distilled water and mixes, stirring and dissolving, add appropriate rare H2SO4Solution, make pH value of solution less than 3.0, add surfactant polyethylene 0.1mol, stirring 5min fully dissolves, the mixed solution obtained is put in 50 DEG C of water-baths, using ammonia as nertralizer, being slowly dropped into pH value of solution=ll with dropper, continue to keep solution at 50 DEG C, high-speed stirred reacts 0.5h, mixing speed is 1000r/min, then obtaining solid particle with the magnetic field separation of magnetic field intensity 600GS, solid particle is dry 4h in vacuum drying oven, grinds, encapsulation, namely obtains nano-magnetic crystal seed.
1L nickel minerals electrolytic anode liquid is added in deironing crystallization reaction still, add 0.54g nano-magnetic crystal seed, passing into oxygen in nickel minerals electrolytic anode liquid makes the mol ratio of Fe (II) and Fe (III) in nickel minerals electrolytic anode liquid be 1:2, controlling nickel minerals electrolytic anode liquid temp is 90 DEG C, regulating the crystallization reaction still internal magnetic field intensity being covered with vertical magnetic field is 1200GS, mixing speed 800r/min, slowly it is continuously added to neutralize sodium bicarbonate solution in reactor, controlling reaction pH is 4.0, reaction 2h, reaction adds bodied ferric sulfate 100mg after terminating and carries out magnetic flocculation, non magnetic or the weak magnetic subparticle that hydrolytic process produces is flocculated with magnetic-particle, coalescence forms magnetic floc sedimentation, by magnetic separator separation scum that magnetic field intensity is 600GS after having flocculated.
Table 3 is the present embodiment nickel minerals electrolytic anode liquid deironing result of the test
Embodiment 4:
This process is utilized to process Fe2+The nickel minerals electrolytic anode liquid of content 0.30g/L.
Prepare nano-magnetic crystal seed: weigh 1molFeSO respectively4And 1molFe2(SO4)3It is dissolved in 1L distilled water and mixes, stirring and dissolving, add appropriate rare H2SO4Solution, make pH value of solution less than 3.0, add surfactant polyethylene 0.1mol, stirring 5min fully dissolves, the mixed solution obtained is put in 50 DEG C of water-baths, using ammonia as nertralizer, being slowly dropped into pH value of solution=ll with dropper, continue to keep solution at 50 DEG C, high-speed stirred reacts 0.5h, mixing speed is 1000r/min, then obtaining solid particle with the magnetic field separation of magnetic field intensity 600GS, solid particle is dry 4h in vacuum drying oven, grinds, encapsulation, namely obtains nano-magnetic crystal seed.
1L nickel minerals electrolytic anode liquid is added in deironing crystallization reaction still, add 0.30g nano-magnetic crystal seed, passing into ozone in nickel minerals electrolytic anode liquid makes the mol ratio of Fe (II) and Fe (III) in nickel minerals electrolytic anode liquid be 1:2, controlling nickel minerals electrolytic anode liquid temp is 90 DEG C, regulating the crystallization reaction still internal magnetic field intensity being covered with vertical magnetic field is 1000GS, mixing speed 800r/min, nertralizer nickelous carbonate solution slowly it is continuously added in reactor, controlling reaction pH is 4.0, reaction 1.5h, reaction adds bodied ferric sulfate 100mg after terminating and carries out magnetic flocculation, non magnetic or the weak magnetic subparticle that hydrolytic process produces is flocculated with magnetic-particle, coalescence forms magnetic floc sedimentation, by magnetic separator separation scum that magnetic field intensity is 400GS after having flocculated.
Table 4 is the present embodiment nickel minerals electrolytic anode liquid deironing result of the test
Embodiment 5:
This process is utilized to process Fe2+The nickel minerals electrolytic anode liquid of content 0.86g/L.
Prepare nano-magnetic crystal seed: weigh 1molFeSO respectively4And 1molFe2(SO4)3It is dissolved in 1L distilled water and mixes, stirring and dissolving, add appropriate rare H2SO4Solution, make pH value of solution less than 3.0, add surfactant polyethylene 0.1mol, stirring 5min fully dissolves, the mixed solution obtained is put in 55 DEG C of water-baths, using ammonia as nertralizer, being slowly dropped into pH value of solution=ll with dropper, continue to keep solution at 55 DEG C, high-speed stirred reacts 0.5h, mixing speed is 1000r/min, then obtaining solid particle with the magnetic field separation of magnetic field intensity 600GS, solid particle is dry 4h in vacuum drying oven, grinds, encapsulation, namely obtains nano-magnetic crystal seed.
1L nickel minerals electrolytic anode liquid is added in deironing crystallization reaction still, add 0.86g nano-magnetic crystal seed, adding the sodium peroxydisulfate that molar concentration is 1mol/L in nickel minerals electrolytic anode liquid makes the mol ratio of Fe (II) and Fe (III) in nickel minerals electrolytic anode liquid be 1:2, controlling nickel minerals electrolytic anode liquid temp is 90 DEG C, regulating the crystallization reaction still internal magnetic field intensity being covered with vertical magnetic field is 900GS, mixing speed 800r/min, slowly it is continuously added to neutralize nickel hydroxide solution in reactor, controlling reaction pH is 4.0, reaction 1h, reaction adds non-ionic polyacrylamide 10mg after terminating, carry out magnetic flocculation, non magnetic or the weak magnetic subparticle that hydrolytic process produces is flocculated with magnetic-particle, coalescence forms magnetic floc sedimentation, by magnetic separator separation scum that magnetic field intensity is 500GS after having flocculated.
Table 5 is the present embodiment nickel minerals electrolytic anode liquid deironing result of the test
Claims (5)
1. the method for a nickel minerals leachate or electrolytic anode liquid deironing, it is characterised in that comprise the following steps:
Step 1:
Prepare nano-magnetic crystal seed
It is dissolved in distilled water after Fe (II) salt and Fe (III) salt are weighed mixing for the ratio of 1:1 in molar ratio, stirring and dissolving, the solution after dissolving adds rare H2SO4Solution makes pH value of solution less than 3.0, is subsequently adding surfactant polyethylene, and the mixed solution obtained fully is dissolved in stirring, the mixed solution obtained is put in 50-60 DEG C of water-bath, using NaOH solution or ammonia as nertralizer, making pH value of solution is 11, continues to keep mixed solution at 50-60 DEG C, high-speed stirred reacts 0.5-1h, then obtaining solid particle with magnetic field separation, solid particle is dry 3-4h in vacuum drying oven, grinds, encapsulation, namely obtains nano-magnetic crystal seed；
Step 2:
Magnetic field and crystal seed induction crystallization
Nickel minerals leachate or electrolytic anode liquid is added in the crystallization reaction still being covered with the vertical magnetic field of 800-1200GS, nickel minerals leachate or electrolytic anode liquid temp control at 80-90 DEG C, it is subsequently adding the magnetic crystal seed that step 1 obtains to be stirred, the addition weight of described magnetic crystal seed is identical with iron ion weight in leachate or electrolytic anode liquid, oxidant is added again in crystallization reaction still, making the mol ratio of Fe (II) and Fe (III) in nickel minerals leachate or electrolytic anode liquid is 1:2, the most backward described nickel minerals leachate or electrolytic anode liquid add sodium carbonate, sodium bicarbonate, nickelous carbonate, sodium hydroxide, a kind of neutralization of nickel hydroxide, making pH is 3.0-4.0, iron ion is promoted at magnetic seed surface crystallization and to align, the time of reaction is that 1-2h obtains ore pulp；
Step 3:
The magnetic flocculation of non magnetic or sub magnetic debris
Flocculant is added in the ore pulp of step 2 gained, the addition weight of described flocculant is every liter of nickel minerals leachate or electrolytic anode liquid addition 10-100mg so that the non magnetic or weak magnetic subparticle that hydrolytic process produces and magnetic-particle flocculation, coalescence formation magnetic floc sedimentation；
Step 4:
The magnetic separation of scum separates
The ore pulp of step 3 gained is proceeded in magnetic separator, it is achieved being separated efficiently and rapidly of scum.
2. the method for a kind of nickel minerals leachate according to claim 1 or electrolytic anode liquid deironing, it is characterised in that: raw material Fe (II) salt of nano-magnetic crystal seed and Fe (III) salt respectively FeSO in described step 14And Fe2(SO4)3, described Fe (II) salt and Fe (III) salt are 10:10:1 with surfactant polyethylene mol ratio.
3. the method for a kind of nickel minerals leachate according to claim 1 and 2 or electrolytic anode liquid deironing, it is characterised in that: the oxidant of described step 2 is the one in hydrogen peroxide, air, oxygen, ozone, sodium peroxydisulfate.
4. the method for a kind of nickel minerals leachate according to claim 3 or electrolytic anode liquid deironing, it is characterised in that: in described step 3, flocculant is non-ionic polyacrylamide or aluminium polychlorid or bodied ferric sulfate.
5. the method for a kind of nickel minerals leachate according to claim 1 or 3 or electrolytic anode liquid deironing, it is characterised in that: in described step 4, magnetic separator separation magnetic field intensity is 400-600GS.
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| CN110129773A (en) * | 2019-06-19 | 2019-08-16 | 宁波中科纬诚新材料科技有限公司 | A kind of method of chemical nickeling ageing liquid circular regeneration |
| CN113666351B (en) * | 2021-08-31 | 2023-12-12 | 广东邦普循环科技有限公司 | Method for preparing ferric phosphate by recycling ferronickel slag |
| CN114031239B (en) * | 2022-01-10 | 2022-04-08 | 中南大学 | Method for separating multiple metals in plasma fused soot elution wastewater |
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