CN105506313A - Dechlorination method of organic phase in indium extracting process - Google Patents
Dechlorination method of organic phase in indium extracting process Download PDFInfo
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- CN105506313A CN105506313A CN201510985718.5A CN201510985718A CN105506313A CN 105506313 A CN105506313 A CN 105506313A CN 201510985718 A CN201510985718 A CN 201510985718A CN 105506313 A CN105506313 A CN 105506313A
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- China
- Prior art keywords
- organic phase
- sulphuric acid
- dilute sulphuric
- sulfuric acid
- extraction process
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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
- C22B58/00—Obtaining gallium or indium
-
- 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
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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
The invention relates to the field of metal smelting, in particular to a dechlorination method of an organic phase in an indium extracting process. The dechlorination method comprises the following steps: (1) a regenerated organic phase I and dilute sulfuric acid are fed in a mixing chamber of a first-grade sulfuric acid washing tank for stirring; and then, the mixed liquid of the organic phase I and the dilute sulfuric acid is fed in a clarification chamber of the first-grade sulfuric acid washing tank for standing and layering to obtain an organic phase II and a dilute sulfuric acid phase I; 2) the organic phase II obtained in the step 1) is fed in a mixing chamber of a second-grade sulfuric acid washing tank; meanwhile, dilute sulfuric acid is fed in the mixing chamber of the second-grade sulfuric acid washing tank for stirring; and then, the mixed liquid of the organic phase II and the dilute sulfuric acid is fed in a clarification chamber of the second-grade sulfuric acid washing tank for standing and layering to obtain an organic phase III and a dilute sulfuric acid phase II; and 3) the organic phase III is returned to an indium extracting procedure for recycling. The dechlorination method reduces the content of chloride ions in raffinate, prevents corrosion of chloride to electrolytic polar plates, equipment and factory buildings in zinc smelting, purifies the organic phases, and improves the load rate.
Description
Technical field
The present invention relates to Metal smelting field, particularly relate to the dechlorination method of organic phase in a kind of indium extraction process.
Background technology
Indium is dissipated metal, has very unique and excellent process based prediction model, becomes one of most important propping material in modern electronics industry.The imbalance of production and supplyment has driven the unprecedented soaring of indium market value in recent years.Indium mineral resources is many with Pb-Zn deposits association, and indium output 90% reclaims from lead-zinc smelting byproduct in the world.The indium of zinc abstraction system reclaims and manyly to reclaim from zinc oxide, the mode taking the integrated indium slag of getting rich first leaching extraction again had, and what have directly directly extracts from the Weak-acid leaching liquid of zinc oxide.Generally all have following technological process, leaching-purification-extraction-displacement-founding-electrolysis-ingot casting etc., in extraction process, the sulphuric leachate of indium contacts with organic phase, and indium enters in organic phase, and residue aqueous phase is indium-raffinate.Organic phase carries out sulfuric acid scrubbing-hydrochloric acid back extraction again, and indium enters hydrochloric acid aqueous phase, and the deironing of organic phase oxalic acid regenerates.
Because stripping process organic phase contacts with hydrochloric acid, organic phase after back extraction carries a small amount of hydrochloric acid aqueous phase, organic phase after regeneration returns when reusing and contacts with feed liquid, the hydrochloric acid that organic phase is carried enters in raffinate, cause raffinate chloride at more than 1000mg/L, due to the composition containing recoverables such as zinc, indium, iron, acid in indium-raffinate, indium-raffinate is all returned zinc abstraction system by a lot of enterprise, reclaims zinc, indium, iron, acid etc. wherein.But chlorion in indium-raffinate, long-time use causes zinc abstraction system chlorion to raise, and affects Zn system electrolysis and normally produces, and quality product declines, and also has certain corrosion, shorten its work-ing life to Zn system equipment.
Dechlorination mode in current zinc metallurgy System Solution mostly is: the mode of chlorine removal from copper residue, invest relatively large, and cost is higher, also has a certain impact to the recycling of output copper ashes.
Summary of the invention
The present invention for overcoming the deficiencies in the prior art, and provides the dechlorination method of organic phase in a kind of indium extraction process.
The dechlorination method of organic phase in a kind of indium extraction process provided by the invention, comprises the following steps:
Step 1), by regeneration after organic phase I and dilute sulphuric acid pass in the mixing section of one-level sulfuric acid scrubbing groove, turn on agitator stirs, organic phase I and dilute sulphuric acid are mixed, then, organic phase I and the mixed solution of dilute sulphuric acid are passed in the clarifying chamber of one-level sulfuric acid scrubbing groove, leave standstill, layering, obtain organic phase II and dilute sulphuric acid phase I;
Step 2), the organic phase II obtained in step 1) is passed in the mixing section of secondary sulfuric acid scrubbing groove, in the mixing section of secondary sulfuric acid scrubbing groove, pass into dilute sulphuric acid simultaneously, turn on agitator stirs, organic phase II and dilute sulphuric acid are mixed, then, organic phase II and the mixed solution of dilute sulphuric acid are passed in the clarifying chamber of secondary sulfuric acid scrubbing groove, leave standstill, layering, obtains organic phase III and dilute sulphuric acid phase II;
Step 3), organic phase III return indium extraction process and recycle, and then reduce the chloride ion content in extraction process raffinate.
Step 2) in dilute sulphuric acid concentration used be 30g/L-80g/L, step 2) in the dilute sulphuric acid that obtains II return in step 1) mutually.
Step 1) and step 2) in whipping temp be 25 DEG C-35 DEG C.
Step 1) and step 2) in churning time be 1min-3min.
Step 1) and step 2) in the paddle wheel linear velocity 5m/s-6m/s of agitator, avoid excessive velocities organic phase and aqueous phase overmixing, occur profit unseparated third phase during clarification, then mixed effect is poor for mistake speed.
Step 1) and step 2) in time of repose be 10min-30min.
In step 1), organic phase I is 1:3-1:5 with the volume ratio of dilute sulphuric acid, step 2) in organic phase II be 1:3-1:5 with the volume ratio of dilute sulphuric acid.
Dilute sulphuric acid is mutually I when being less than or equal to 3000mg/L with chloride ion content in dilute sulphuric acid phase II, resume at step 1) or step 2) in; Its waste water, mutually I when being greater than 3000mg/L with chloride ion content in dilute sulphuric acid mutually II, with lime powder neutralization, press filtration, is beaten sewage works by dilute sulphuric acid, in it and slag send converter recovery valuable metal back to.
Beneficial effect:
1, the chloride ion content in organic phase is reduced, and then the chloride ion content reduced in extraction process raffinate, avoid raffinate return Zn system use time chlorine to the corrosion of electrolytic pole board, equipment and factory building in zinc abstraction, organic phase is purified, and load factor is improved.
2, utilize chlorion different from the mutual solubility in dilution heat of sulfuric acid at organic solvent, mixed with dilution heat of sulfuric acid by organic phase, make the part chlorion in organic solvent proceed to dilution heat of sulfuric acid, to reach the object of separation and concentrating chloride ions.Chloride high dilution heat of sulfuric acid lime powder neutralizes afterwards, in and slag send Rotary Kiln to reclaim valuable metal, waste water to send sewage plant process, chloride low organic solvent returns indium extraction process and recycles.
3, dilute sulphuric acid concentration is 30g/L-80g/L, when avoiding dilute sulphuric acid concentration too low and organic phase undercompounding, has impact during dilute sulphuric acid excessive concentration on organic phase stability, and then affects chlorine in organic phase and enter in dilution heat of sulfuric acid.
4, whipping temp is 25 DEG C-35 DEG C, and when avoiding low temperature, organic phase is clamminess, and both dilute sulphuric acid phase and organic phase mixing and clarification difficulty, produce third phase; Avoid high temperature that organic phase is volatilized, cause organic phase to lose.
5, churning time 1min-3min, avoids time long organic phase and aqueous phase overmixing, occurs profit unseparated third phase during clarification, and too short then mixed effect is poor.
6, step 1) and step 2) in the paddle wheel linear velocity 5m/s-6m/s of agitator, avoid excessive velocities organic phase and aqueous phase overmixing, occur profit unseparated third phase during clarification, then mixed effect is poor for mistake speed.
7, settling time 10min-30min, avoid time short organic phase and aqueous phase separation thorough, time length affects processing power.
Accompanying drawing explanation
Fig. 1 is the FB(flow block) of the dechlorination embodiment of the method for organic phase in a kind of indium extraction process of the present invention.
Embodiment
Embodiment: the dechlorination method of organic phase in a kind of indium extraction process provided by the invention, as shown in Figure 1, comprises the following steps:
Step 1), by regeneration after organic phase I and dilute sulphuric acid pass in the mixing section of one-level sulfuric acid scrubbing groove, turn on agitator stirs, organic phase I and dilute sulphuric acid are mixed, then, organic phase I and the mixed solution of dilute sulphuric acid are passed in the clarifying chamber of one-level sulfuric acid scrubbing groove, leave standstill, layering, obtain organic phase II and dilute sulphuric acid phase I;
Step 2), the organic phase II obtained in step 1) is passed in the mixing section of secondary sulfuric acid scrubbing groove, in the mixing section of secondary sulfuric acid scrubbing groove, pass into dilute sulphuric acid simultaneously, turn on agitator stirs, organic phase II and dilute sulphuric acid are mixed, then, organic phase II and the mixed solution of dilute sulphuric acid are passed in the clarifying chamber of secondary sulfuric acid scrubbing groove, leave standstill, layering, obtains organic phase III and dilute sulphuric acid phase II;
Step 3), organic phase III return indium extraction process and recycle, and then reduce the chloride ion content in extraction process raffinate.
Step 2) in dilute sulphuric acid concentration used be 30g/L-80g/L, step 2) in the dilute sulphuric acid that obtains II return in step 1) mutually, dilute sulphuric acid recycles, and saves dilute sulphuric acid consumption, reduces costs.
Step 1) and step 2) in whipping temp be 25 DEG C-35 DEG C.
Step 1) and step 2) in churning time be 1min-3min.
Step 1) and step 2) in the paddle wheel linear velocity 5m/s-6m/s of agitator.
Step 1) and step 2) in time of repose be 10min-30min.
In step 1), organic phase I is 1:3-1:5 with the volume ratio of dilute sulphuric acid, step 2) in organic phase II be 1:3-1:5 with the volume ratio of dilute sulphuric acid.
Dilute sulphuric acid is mutually I when being less than or equal to 3000mg/L with chloride ion content in dilute sulphuric acid phase II, resume at step 1) or step 2) in; Its waste water, mutually I when being greater than 3000mg/L with chloride ion content in dilute sulphuric acid mutually II, with lime powder neutralization, press filtration, is beaten sewage works by dilute sulphuric acid, in it and slag send converter recovery valuable metal back to.
Utilize chlorion different from the mutual solubility in dilution heat of sulfuric acid at organic solvent, mixed with dilution heat of sulfuric acid by organic phase, make the part chlorion in organic solvent proceed to dilution heat of sulfuric acid, to reach the object of separation and concentrating chloride ions.Chloride high dilution heat of sulfuric acid lime powder neutralizes afterwards, in and slag send Rotary Kiln to reclaim valuable metal, waste water to send sewage plant process, chloride low organic solvent returns indium extraction process and recycles.
Claims (7)
1. the dechlorination method of organic phase in indium extraction process, is characterized in that: comprise the following steps:
Step 1), by regeneration after organic phase I and dilute sulphuric acid pass in the mixing section of one-level sulfuric acid scrubbing groove, turn on agitator stirs, organic phase I and dilute sulphuric acid are mixed, then, organic phase I and the mixed solution of dilute sulphuric acid are passed in the clarifying chamber of one-level sulfuric acid scrubbing groove, leave standstill, layering, obtain organic phase II and dilute sulphuric acid phase I;
Step 2), the organic phase II obtained in step 1) is passed in the mixing section of secondary sulfuric acid scrubbing groove, in the mixing section of secondary sulfuric acid scrubbing groove, pass into dilute sulphuric acid simultaneously, turn on agitator stirs, organic phase II and dilute sulphuric acid are mixed, then, organic phase II and the mixed solution of dilute sulphuric acid are passed in the clarifying chamber of secondary sulfuric acid scrubbing groove, leave standstill, layering, obtains organic phase III and dilute sulphuric acid phase II;
Step 3), organic phase III return indium extraction process and recycle.
2. the dechlorination method of organic phase in indium extraction process according to claim 1, is characterized in that: step 2) in dilute sulphuric acid concentration used be 30g/L-80g/L, step 2) in the dilute sulphuric acid that obtains II return in step 1) mutually.
3. the dechlorination method of organic phase in indium extraction process according to claim 1, is characterized in that: step 1) and step 2) in whipping temp be 25 DEG C-35 DEG C.
4. the dechlorination method of organic phase in indium extraction process according to claim 1, is characterized in that: step 1) and step 2) in churning time be 1min-3min.
5. the dechlorination method of organic phase in indium extraction process according to claim 1, is characterized in that: step 1) and step 2) in time of repose be 10min-30min.
6. the dechlorination method of organic phase in indium extraction process according to claim 1, is characterized in that: in step 1), organic phase I is 1:3-1:5 with the volume ratio of dilute sulphuric acid, step 2) in organic phase II be 1:3-1:5 with the volume ratio of dilute sulphuric acid.
7. the dechlorination method of organic phase in indium extraction process according to claim 1, is characterized in that: dilute sulphuric acid is mutually I when being less than or equal to 3000mg/L with chloride ion content in dilute sulphuric acid phase II, resume at step 1) or step 2) in; Its waste water, mutually I when being greater than 3000mg/L with chloride ion content in dilute sulphuric acid mutually II, with lime powder neutralization, press filtration, being beaten sewage plant, is sent converter back in it with slag by dilute sulphuric acid.
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| CN201510985718.5A CN105506313A (en) | 2015-12-25 | 2015-12-25 | Dechlorination method of organic phase in indium extracting process |
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| CN201510985718.5A CN105506313A (en) | 2015-12-25 | 2015-12-25 | Dechlorination method of organic phase in indium extracting process |
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Citations (6)
| 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 |
| US5332420A (en) * | 1992-02-25 | 1994-07-26 | Zeneca Limited | Chemical process of separating metals from an organic complex |
| CN102978396A (en) * | 2012-12-06 | 2013-03-20 | 河南豫光锌业有限公司 | Organic phase washing method and device |
| CN102978421A (en) * | 2012-12-31 | 2013-03-20 | 株洲冶炼集团股份有限公司 | Indium extraction method of ferrous iron-rich zinc oxide acid supernatant |
| CN103014338A (en) * | 2013-01-18 | 2013-04-03 | 株洲冶炼集团股份有限公司 | Method for processing poor organic phase after solvent extraction indium extracting |
| CN103540766A (en) * | 2012-07-17 | 2014-01-29 | 陕西锌业有限公司 | Technology for recycling indium from zinc oxide material with high fluoride and chlorine contents and removing fluorine, chlorine and arsenic from raffinate |
-
2015
- 2015-12-25 CN CN201510985718.5A patent/CN105506313A/en active Pending
Patent Citations (6)
| 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 |
| US5332420A (en) * | 1992-02-25 | 1994-07-26 | Zeneca Limited | Chemical process of separating metals from an organic complex |
| CN103540766A (en) * | 2012-07-17 | 2014-01-29 | 陕西锌业有限公司 | Technology for recycling indium from zinc oxide material with high fluoride and chlorine contents and removing fluorine, chlorine and arsenic from raffinate |
| CN102978396A (en) * | 2012-12-06 | 2013-03-20 | 河南豫光锌业有限公司 | Organic phase washing method and device |
| CN102978421A (en) * | 2012-12-31 | 2013-03-20 | 株洲冶炼集团股份有限公司 | Indium extraction method of ferrous iron-rich zinc oxide acid supernatant |
| CN103014338A (en) * | 2013-01-18 | 2013-04-03 | 株洲冶炼集团股份有限公司 | Method for processing poor organic phase after solvent extraction indium extracting |
Non-Patent Citations (1)
| Title |
|---|
| 王锦鸿: "湿法系统除氯工艺技术研究及应用", 《湖南有色金属》 * |
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Application publication date: 20160420 |