CN102534212A - Method for separating low-concentration multiple metal ions through extraction and stepwise back-extraction - Google Patents
Method for separating low-concentration multiple metal ions through extraction and stepwise back-extraction Download PDFInfo
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- CN102534212A CN102534212A CN2010106152739A CN201010615273A CN102534212A CN 102534212 A CN102534212 A CN 102534212A CN 2010106152739 A CN2010106152739 A CN 2010106152739A CN 201010615273 A CN201010615273 A CN 201010615273A CN 102534212 A CN102534212 A CN 102534212A
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Abstract
The invention discloses a method for separating low-concentration multiple metal ions through extraction and stepwise back-extraction. By the method, once extraction and sequential stepwise back-extraction are adopted, a high multiple metal ion separating effect can be achieved, and an aim of purifying and enriching metal ions is fulfilled. By the method, indium, cadmium and zinc in zinc concentrate biologic leachate of Qinghai Province are separated, purified and enriched, and impurity iron metal ions are removed. A P2O4 extracting agent and sulfonated kerosene mixture is taken as an organic phase, the multiple metal ions are extracted into the organic phase at one time, and different stripping agents are adopted for stepwise back-extracting in turn, pure zinc, indium and cadmium ionic liquids are obtained, and excessive iron metal ions are removed. The method is easily applied industrially, a process flow is short, equipment configuration is simple, scale flexibility is high, cost is saved, profit is increased, the added value of ore development is improved and the competitive power of mine enterprises is enhanced. A technology for separating metal ions in a solution is a bottleneck for restricting the development of a wet metallurgical technology, and the perfection of the separation technology is powder for promoting the development of wet metallurgy.
Description
Technical field
The present invention relates to the method that a kind of utilization extraction-substep reextraction in hydrometallurgy field separates many metals ions.Simple, efficient, the easy row of this separation method realizes that many metals separate the purpose of comprehensive recovery simultaneously.
Background technology
Hydrometallurgy is characteristics such as short and environmentally friendly because of its reduced investment, instant effect, flow process, in industrial application, have obtained good economic benefit, social benefit and environmental benefit, obtain application more and more widely in field of metallurgy.Stripping technique and hydrometallurgy are closely related, and are the restraining factors of hydrometallurgy development, and GOLD FROM PLATING SOLUTION belongs to the feasibility that the ionic separation and purification has directly determined the hydrometallurgy scheme.This shows that stripping technique is the main impellent that hydrometallurgical technology advances.The landmark development of hydrometallurgy industrial applications all is because the development and the innovation of stripping technique.
Summary of the invention
The method that the purpose of this invention is to provide a kind of extraction and the many metals ions of separating low concentration of stripping step by step; Present method is succinct, efficient, be prone to row, plant factor is high; The easy realization of industrial application is a kind of novel method that the hydrometallurgy stripping technique is separated many metals ions.
For reaching the foregoing invention purpose, the present invention adopts following technical scheme:
Novel method adopts solvent extraction technology; Utilize extraction agent that different metal ionic binding ability is not waited; Thereby the extraction environmental system is required difference, and disposable valuable metal ions being extracted in the organic solvent that contains extraction agent adopted different reverse-extraction agent substep back extractions then; The different metal ion is transferred to respectively in the reverse-extraction agent from this organic solvent, realized the separation and the purifying of many metals ions.
Novel method is succinct, efficient, be prone to row, plant factor is high, and the easy realization of industrial application is a kind of novel method that the hydrometallurgy stripping technique is separated many metals ions.
Many metals ions of lower concentration leach liquor and the organic phase solution hybrid extraction that contains extraction agent, metals ion is transferred in the organic phase, and organic phase changes load organic phases into;
Leach liquor is extracted and becomes raffinate behind the metals ion and turn back to the leaching system;
Reverse-extraction agent of different nature is mixed respectively with load organic phases successively step by step, and substep is stripped and is obtained containing the strip liquor of corresponding metal ion solution respectively;
Metals ion in the load organic phases in the strip liquor that contains corresponding metals ion, is obtained different metal ionic purification enrichment solution by the reverse-extraction agent back extraction;
Load organic phases is stripped behind the metals ion, and the saponification of hydro-oxidation sodium solution changes the regeneration organic phase into after the homogeneous phase saponification;
The regeneration organic phase is returned extraction process and is continued cycle operation.
Waiting to separate many metal ion solutions is the zinc leaching residue biochemical lixivium, and iron content 4～4.1g/L, indium 5～5.5mg/L, cadmium 5～5.5mg/L, zinc 23～24g/L, pH are 1.5～2.0.
In the extraction process, the phase mixing time is 5min, compares (O/A) 2/10 (volume ratio).
The strip reverse-extraction agent of zinc and cadmium of substep is that concentration is the sulphuric acid soln of 150g/L.
The back extraction mixing time is 3min, and comparing (O/A) is 10/2 (volume ratio).
The reverse-extraction agent of substep back extraction indium is that concentration is the hydrochloric acid soln of 3mol/L.
A ferrous metal ion in the iron strip liquor.
For realizing the separation and purification of many metals ions in the low concentration solution, novel method is taked following plan (see figure 1):
1), shown in operation 1, will contain many metal ion solution and mix with the regeneration organic phase solution of 30%P204+70% sulfonated kerosene after the homogeneous phase saponification and extract, mixed phase is than (O/A) 2/10 (volume ratio), mixing time 5min.Organic phase is converted into load organic phases because of having obtained metals ion from aqueous phase, and water has lost metals ion and has been converted into raffinate, has accomplished the transfer of metals ion.
2), shown in operation 2, add reverse-extraction agent 1 in the load organic phases, mix 3min, compare (O/A) 10/2 (volume ratio).Zn and Cd be transferred to aqueous phase system, realized separating of Zn and Cd and other metals ion.
3), shown in operation 3.Add reverse-extraction agent 2 in the load organic phases of back extraction separation of Zn and Cd once more, mix 3min, compare (O/A) 10/2 (volume ratio).At this moment, dissipated metal In is transferred to aqueous phase system, has realized the separating of In and other metals ion, enrichment and purifying.
4), shown in operation 4.Through adding reverse-extraction agent 3 once more in the organic phase behind twice back extraction separating metal ion, mix 3min, compare (O/A)=10/2 (volume ratio).Fe is transferred to aqueous phase, has realized separation, the enrichment of Fe, and organic phase has obtained regeneration.
5), shown in operation (4), after stripping through substep, the metals ion in the load organic phases is all dissociated, organic phase has obtained regeneration, has accomplished metals ion separation and purification from aqueous phase solution, has shifted the once circulation of carrying.The regeneration organic phase turns back to the extraction link, and the separation and purification of beginning next round is carried with shifting.
The many metal ion solutions of above-described lower concentration are leached mud leach liquors after biology leaches of iron content, indium, cadmium and zinc, leach liquor iron content 4.07g/L, indium 5.29mg/L, cadmium 5.29mg/L, zinc 23.5g/L, and the pH value is 1.5～2.0.Organic phase is organic mixing solutions that 30% P204+70% sulfonated kerosene is formed, and organic phase is with the saponification of sodium hydroxide homogeneous phase, saponification degree 70%.Leach liquor mixes the back metals ion and is transferred in the organic phase by exchange with organic phase; Separate through clarification; Obtain more purified load organic phases; Different according to metals ion with the binding ability and the parsing separation condition of extraction agent, utilize different reverse-extraction agent substep back extractions to obtain comparatively purified metal ion solution, realize the separation and purification of metals ion.
Description of drawings
Fig. 1 is the FB(flow block) of the present invention's substep stripping method
Fig. 2 is a practical implementation FB(flow block) of the present invention
Embodiment
Embodiment 1:
This substep back extraction novel method is applied to useful metal ionic separation in the zinc ore concentrate biochemical lixivium behind the Xi Tieshan lead-zinc ore floating of Qinghai.Zinc ore concentrate after the flotation be plumbous zinc ore behind flotation operation, obtain contain zinc 47.62%, sulphur 30.77%, iron 13.07%, cadmium 0.34%, indium 0.0146% and plumbous 0.79% concentrate.For what effectively utilize association in this ore valency scattered metals indium and cadmium being arranged, reduce environmental pollution simultaneously, adopt biological leaching-out technique to handle this ore, can obtain good economic benefit and environmental benefit, is effective novel process that the type ore develops.
Below in conjunction with the practical implementation instance the present invention is described further.
(1) as shown in Figure 2, ore is carried out obtaining leach liquor A after bacterium leaching and the solid-liquid separation, iron content 4.07g/L, indium 5.29mg/L, cadmium 5.29mg/L, zinc 23.5g/L, pH are 1.8.
(2) operation 1. with through homogeneous phase saponified regeneration organic phase I hybrid extraction, mix 5min, compare (O/A) 2/10, the metals ion in the water leach liquor is extracted in the organic phase, regeneration organic phase I changes load organic phases F into.The water that loses metals ion changes raffinate B into.
(3) 2., join the reverse-extraction agent 1C of sulfur acid 150g/L among the load organic phases F, mix 3min, comparing is (O/A) 10/2 (volume ratio) in operation.Zinc among the load organic phases F, cadmium metal ion in Zn, Cd strip liquor, have been realized that zinc, cadmium separate with other metals ions by back extraction.
(4) 3., join the reverse-extraction agent 2D of hydrochloric 3mol/L among the load organic phases G, mix 3min, comparing is that (O/A) is 10/2 (volume ratio) in operation.Indium metal ion among the load organic phases G in the In strip liquor, has been realized separation, purifying and the enrichment of indium ion by back extraction.
(5) 4., join the reverse-extraction agent 3E of hydrochloric 6mol/L among the load organic phases H, mix 3min, comparing (O/A) is 10/2 (volume ratio) in operation.Ferrous metal ion among the load organic phases H in the Fe strip liquor, has been realized that the removal of impurities of iron ion separates by back extraction, and organic phase has obtained regeneration.
(6) 5.,, after washing, obtain regeneration organic phase I, accomplished the regeneration of organic phase, begun the extraction of next round sodium hydroxide solution and load organic phases H mixing 3min in operation.
Effect of the present invention is: adopt SX disposable with the low-concentration metallic ion extractuin in the aqueous phase solution in the organic phase that contains extraction agent; Substep is stripped the metals ion back extraction in the organic phase in the strip liquor that contains corresponding metals ion then, realizes separation, purifying and the enrichment of many metals ions.This invention is easy to realize industrial applications, and equipment is simple, and industrial scale is changeable, reduces investment outlay, and is a kind of novel method in the hydrometallurgy solution separating system.
Claims (11)
1. an extraction and the substep method of the many metals ions of separating low concentration of stripping, it is characterized in that: it may further comprise the steps:
1), many metals ions of lower concentration leach liquor with contain the organic phase solution hybrid extraction of extraction agent, metals ion is transferred in the organic phase, organic phase changes load organic phases into;
2), leach liquor is extracted and becomes raffinate behind the metals ion and turn back to the leaching system;
Reverse-extraction agent of different nature is mixed respectively with load organic phases successively step by step, and substep is stripped and is obtained containing the strip liquor of corresponding metal ion solution respectively;
3), the metals ion in the load organic phases in the strip liquor that contains corresponding metals ion, is obtained different metal ionic purification enrichment solution by the reverse-extraction agent back extraction;
4), load organic phases stripped behind the metals ion, the saponification of hydro-oxidation sodium solution changes the regeneration organic phase into after the homogeneous phase saponification;
5), the regeneration organic phase is returned extraction process continuation cycle operation.
2. the method for a kind of extraction according to claim 1 and the many metals ions of separating low concentration of stripping step by step; It is characterized in that: waiting to separate many metal ion solutions is the zinc leaching residue biochemical lixivium; Iron content 4～4.1g/L, indium 5～5.5mg/L, cadmium 5～5.5mg/L, zinc 23～24g/L, pH are 1.5～2.0.
3. the method for a kind of extraction according to claim 1 and the many metals ions of separating low concentration of stripping step by step, the organic phase that contains extraction agent is the mixed solution of 30%P204+70% sulfonated kerosene.
4. the method for a kind of extraction according to claim 3 and the many metals ions of separating low concentration of stripping step by step is characterized in that: the saponification degree of regeneration organic phase is 70%.
5. the method for a kind of extraction according to claim 2 and the many metals ions of separating low concentration of stripping step by step, in the extraction process, the phase mixing time is 5min, compares (O/A) 2/10 (volume ratio).
6. according to the method for claim 2 or the 5 described a kind of extractions and the many metals ions of separating low concentration of stripping step by step, it is characterized in that: the reverse-extraction agent of strip step by step zinc and cadmium is that concentration is the sulphuric acid soln of 150g/L.
7. according to the method for claim 1 or the 6 described a kind of extractions and the many metals ions of separating low concentration of stripping step by step, it is characterized in that: the back extraction mixing time is 3min, and comparing (O/A) is 10/2 (volume ratio).
8. the method for a kind of extraction according to claim 2 and the many metals ions of separating low concentration of stripping step by step is characterized in that: the reverse-extraction agent of substep back extraction indium is that concentration is the hydrochloric acid soln of 3mol/L.
9. the method for a kind of extraction according to claim 2 and the many metals ions of separating low concentration of stripping step by step is characterized in that: the reverse-extraction agent of substep back extraction iron is that concentration is the hydrochloric acid soln of 6mol/L.
10. according to the method for claim 1, it is characterized in that: change raffinate after the metals ion in the leach liquor is extracted into and turn back to the recycle of leaching operation with the 2 described a kind of extractions and the many metals ions of separating low concentration of stripping step by step.
11. the method for a kind of extraction according to claim 2 and the many metals ions of separating low concentration of stripping step by step is characterized in that: a ferrous metal ion in the iron strip liquor.
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Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104034718A (en) * | 2014-05-19 | 2014-09-10 | 宁波大学 | Method for determining content of cadmium in soil by ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) |
| CN105800819A (en) * | 2014-12-30 | 2016-07-27 | 北京有色金属研究总院 | Method for high-efficiency separation of valuable metal ions in complex solution containing heavy metals |
| CN109022810A (en) * | 2018-08-24 | 2018-12-18 | 肇庆市珈旺环境技术研究院 | A method of separating and recovering valuable metal iron, manganese and scandium from tungsten slag |
| CN114717415A (en) * | 2022-03-30 | 2022-07-08 | 有研资源环境技术研究院(北京)有限公司 | Method for separating multi-metal mixed solution |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN1031720A (en) * | 1987-09-04 | 1989-03-15 | 冶金工业部长沙矿冶研究院 | Process for recovering indium from high indium iron solution |
| CN1966745A (en) * | 2006-11-20 | 2007-05-23 | 深圳市中金岭南有色金属股份有限公司韶关冶炼厂 | Extraction and separation technology for reclaiming main impurity in indium in hydrochloric acid system |
| CN101451185A (en) * | 2007-11-28 | 2009-06-10 | 灵宝市金源矿业有限责任公司 | Comprehensive recovery method for ferro-sulphur ore containing copper, zinc and iron multi-metal |
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2010
- 2010-12-20 CN CN2010106152739A patent/CN102534212A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1031720A (en) * | 1987-09-04 | 1989-03-15 | 冶金工业部长沙矿冶研究院 | Process for recovering indium from high indium iron solution |
| CN1966745A (en) * | 2006-11-20 | 2007-05-23 | 深圳市中金岭南有色金属股份有限公司韶关冶炼厂 | Extraction and separation technology for reclaiming main impurity in indium in hydrochloric acid system |
| CN101451185A (en) * | 2007-11-28 | 2009-06-10 | 灵宝市金源矿业有限责任公司 | Comprehensive recovery method for ferro-sulphur ore containing copper, zinc and iron multi-metal |
Cited By (4)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104034718A (en) * | 2014-05-19 | 2014-09-10 | 宁波大学 | Method for determining content of cadmium in soil by ICP-AES (Inductively Coupled Plasma-Atomic Emission Spectrometry) |
| CN105800819A (en) * | 2014-12-30 | 2016-07-27 | 北京有色金属研究总院 | Method for high-efficiency separation of valuable metal ions in complex solution containing heavy metals |
| CN109022810A (en) * | 2018-08-24 | 2018-12-18 | 肇庆市珈旺环境技术研究院 | A method of separating and recovering valuable metal iron, manganese and scandium from tungsten slag |
| CN114717415A (en) * | 2022-03-30 | 2022-07-08 | 有研资源环境技术研究院(北京)有限公司 | Method for separating multi-metal mixed solution |
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Application publication date: 20120704 |