CN104928503A - Method for separating and extracting indium and gallium from indium-gallium solution - Google Patents
Method for separating and extracting indium and gallium from indium-gallium solution Download PDFInfo
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Abstract
The invention relates to a method for separating and extracting indium and gallium from an indium-gallium solution. The method comprises the steps that (1) extraction is carried out, i.e., organic phosphoric acid is adopted as an extraction agent, and diluents are added, so that an organic phase is obtained, and the organic phase is added to liquid to be extracted for extraction after pH value is adjusted; (2) reverse extraction of indium is carried out, i.e., reverse extraction is conducted on the extracted phase in the step (1) with concentrated hydrochloric acid, so that an indium-enriched aqueous phase is obtained; (3) reverse extraction of gallium is carried out, i.e., reverse extraction is conducted on the organic phase subjected to reverse extraction in the step (2) with an oxalic acid solution, so that a gallium-enriched aqueous phase is obtained; (4) zinc or aluminum is added into the indium-enriched aqueous phase obtained in the step (2) to obtain indium through replacement, or alkaline substances are added to obtain indium hydroxide sediment; (5) precipitants are added into the gallium-enriched water phase obtained in the step (3) to obtain calcium oxalate, filtration is carried out to remove calcium oxalate, and replacement is carried out on liquid obtained after filtration with zinc or aluminum to obtain the simple substance gallium, or alkaline substances are added to obtain gallium hydroxide sediment. According to the method, two elements are recovered by conducting extraction once and reverse extraction twice, separation is complete, the recovery rate is high, operation is easy, and production cost is reduced.
Description
Technical field
The invention belongs to field of hydrometallurgy, specifically relate to a kind of method of separation and Extraction indium and gallium in indium Gallium solution.
Background technology
Indium and gallium, as dissipated metal element, are important Industrial materials, are usually used in alloy, sensor and semi-conductor.Due to the scarcity of two kinds of elements, from some industrial wastes or electron wastes, recovery indium or gallium become important approach.Indium gallium is often present in some industrial waste simultaneously, as smelted cadmia, indium gallium alloy target waste material and discarded indium gallium arsenic detector etc., can relate to the separation of two elements in the process of recovery unavoidably.And indium and the gallium Nature comparison when solion state is close, separation and Extraction acquires a certain degree of difficulty, so become the ubiquitous problem of industry.
The method of existing separating indium gallium from solution mainly uses the first extraction of indium of P204 extraction agent, then from raffinate, reclaims gallium, but has part gallium during extraction of indium and extracted in organic phase altogether, causes the gallium rate of recovery low.Also have bibliographical information to be separated by hydrolytic precipitation in addition, but both hydrolysis pH value relatively, control difficulty large, easily carry secretly coprecipitated, cause that product is impure or the rate of recovery is low.
Summary of the invention
For current Problems existing, the invention provides the method for separation and Extraction indium gallium in a kind of indium Gallium solution, main with organic phosphoric acid reagent for extraction agent, undertaken by the technological process extracting indium gallium-back extraction indium-back extraction gallium completely altogether or extract indium gallium-back extraction gallium-back extraction indium completely altogether, then from respective strip liquor, hydrolysis or displacement obtain corresponding indium product or gallium product.
Technique of the present invention is followed successively by following steps:
1. extract: with one or more in organophosphorus acids reagent (P204, P507, P501, Cyanex272, Cyanex301, B312) for extraction agent, with the one in (sulfonated kerosene, benzene) for thinner, be made into organic phase, extractant concentration is 5% ~ 30%. treat that extraction liquid pH is adjusted in 1 ~ 2.5 scope, then add organic extractant phase, comparing O/W is 1:5 ~ 5:1 scope, and temperature remains within the scope of 5 ~ 50 DEG C, stir or centrifugal 2 ~ 30min, then separatory.
2. back extraction indium: with the concentrated hydrochloric acid of 6 ~ 12 mol/L for reverse-extraction agent, carries out back extraction to organic phase after the extraction in 1 step, and temperature remains within the scope of 5 ~ 50 DEG C, comparing O/W is 8:1 ~ 1:1 scope, stir or centrifugal 2 ~ 30min, obtain the aqueous phase being rich in indium ion, then separatory.
3. back extraction gallium: with the oxalic acid solution of 0.1 ~ 1mol/L for reverse-extraction agent, to the further back extraction of organic phase after the back extraction in 2 steps, temperature remains within the scope of 5 ~ 50 DEG C, comparing O/W is 8:1 ~ 1:1 scope, stir or centrifugal 2 ~ 30min, obtain the aqueous phase being rich in gallium ion, then separatory.
4. the aqueous phase being rich in indium ion in pairs 2 adds zinc or aluminium displacement obtains simple substance indium, or adds alkaloids as ammoniacal liquor, sodium hydroxide, calcium hydroxide etc., obtains indium hydroxide precipitation.
5. the aqueous phase being rich in gallium ion in pairs 3 adds the precipitation agent of theoretical amount 1 ~ 1.5 times, form caoxalate, wherein precipitation agent is one or more in (calcium chloride, calcium hydroxide, calcium oxide, nitrocalcite, calcium sulfate), temperature of reaction is 5 ~ 80 DEG C of scopes, then cross and filter caoxalate, after filter, liquid zinc or aluminium displacement obtain Metallic Gallium, or add alkaloids as ammoniacal liquor, sodium hydroxide, calcium hydroxide etc., obtain gallium hydroxide precipitation.
Technique back extraction order of the present invention is exchanged, and other processing parameter is constant also can be realized, and is followed successively by following steps:
1. extract: with one or more in organophosphorus acids reagent (P204, P507, P501, Cyanex272, Cyanex301, B312) for extraction agent, with the one in (sulfonated kerosene, benzene) for thinner, be made into organic phase, extractant concentration is 5% ~ 30%. treat that extraction liquid pH is adjusted in 1 ~ 2.5 scope, then add organic extractant phase, comparing O/W is 1:5 ~ 5:1 scope, and temperature remains within the scope of 5 ~ 50 DEG C, stir or centrifugal 2 ~ 30min, then separatory.
2. back extraction gallium: with the oxalic acid solution of 0.1 ~ 1mol/L for reverse-extraction agent, carries out back extraction to organic phase after the extraction in 1 step, and temperature remains within the scope of 5 ~ 50 DEG C, comparing O/W is 8:1 ~ 1:1 scope, stir or centrifugal 2 ~ 30min, obtain the aqueous phase being rich in gallium ion, then separatory.
3. back extraction indium: with the concentrated hydrochloric acid of 6 ~ 12 mol/L for reverse-extraction agent, to the further back extraction of organic phase after the back extraction in 2 steps, temperature remains within the scope of 5 ~ 50 DEG C, comparing O/W is 8:1 ~ 1:1 scope, stir or centrifugal 2 ~ 30min, obtain the aqueous phase being rich in indium ion, then separatory.
4. the aqueous phase being rich in gallium ion in pairs 2 adds the precipitation agent of theoretical amount 1 ~ 1.5 times, form caoxalate, wherein precipitation agent is one or more in (calcium chloride, calcium hydroxide, calcium oxide, nitrocalcite, calcium sulfate), temperature of reaction is 5 ~ 80 DEG C of scopes, then cross and filter caoxalate, after filter, liquid zinc or aluminium displacement obtain Metallic Gallium, or add alkaloids as ammoniacal liquor, sodium hydroxide, calcium hydroxide etc., obtain gallium hydroxide precipitation.
5. the aqueous phase being rich in indium ion in pairs 3 adds zinc or aluminium displacement obtains simple substance indium, or adds alkaloids as ammoniacal liquor, sodium hydroxide, calcium hydroxide etc., obtains indium hydroxide precipitation.
Feature of the present invention is:
(1) make full use of indium and the common extraction character of gallium in organic phosphoric acid kind of extractants, change unfavorable factor is favorable factor, completely extracts two kinds of elements into organic phase simultaneously, then distinguishes back extraction recovery indium and gallium, and be separated thoroughly, the rate of recovery is high.
(2) this technique single extraction adds twice back extraction and reclaims two kinds of elements, and is all simple process, without the complex steps such as multi-stage solvent extraction or flushing, makes simple to operate, and production cost reduces.
(3) although this technique with the addition of oxalic acid, can recycle with the form of caoxalate byproduct.
embodiment:
below the specific embodiment of the present invention is described, but the present invention is not subject to any restriction of embodiment below, in target of the present invention, can adds after suitably changing and implement.
Embodiment 1
(1) take P204 as extraction agent, sulfonated kerosene is thinner, is mixed with the extraction phase that concentration is 30%.
(2) will be 460ppm containing indium, containing the aqueous solution 200ml of gallium 356ppm, regulate pH=1.8. with sodium hydroxide solution
(3) extraction phase prepared by 100ml, joins in (2) in solution liquid, and 30 DEG C of thermostatic electromagnetics stir 10min.
(4) pour in separating funnel by the two-phase after stirring, leave standstill separatory 3 minutes, upper strata is rich indium gallium organic phase, and lower floor is raffinate.
(5) organic phase in (4) taken out, add the hydrochloric acid back extraction of 10mol/L, 30 DEG C of constant temperature stir 10min.
(6) pour in separating funnel by the two-phase after stirring, leave standstill 5 minutes, upper strata is rich gallium organic phase, and lower floor is liquid after rich indium back extraction.
(7) organic phase in (6) taken out, add the oxalic acid back extraction of 1mol/L, 30 DEG C of constant temperature stir 10min.
(8) pour in separating funnel by the two-phase after stirring, leave standstill separatory 3 minutes, upper strata is organic phase after back extraction, and lower floor is liquid after rich gallium back extraction.
(9) under normal temperature to liquid after the rich indium back extraction in (6) add theoretical amount 1.5 times zinc metal sheet displacement obtain simple substance indium.
(10) add the calcium chloride of theoretical amount 1.2 times to liquid after the rich gallium back extraction in (8) under normal temperature, form calcium oxalate precipitation, then cross and filter caoxalate, after filter, liquid adds sodium hydroxide, obtains gallium hydroxide precipitation.
Embodiment 2
(1) with 1 volume P204+0.2 volume Cyanex272 for extraction agent, sulfonated kerosene is thinner, is mixed with the extraction phase that concentration is 25%.
(2) will be 150ppm containing indium, containing the aqueous solution 200ml of gallium 210ppm, regulate pH=1.9. with sodium hydroxide
(3) extraction phase prepared by 100ml, joins in (2) in solution liquid, and 30 DEG C of thermostatic electromagnetics stir 10min.
(4) pour in separating funnel by the two-phase after stirring, leave standstill separatory 5 minutes, upper strata is rich indium gallium organic phase, and lower floor is raffinate.
(5) organic phase in (4) taken out, add the hydrochloric acid back extraction of 10mol/L, 30 DEG C of constant temperature stir 10min.
(6) pour in separating funnel by the two-phase after stirring, leave standstill 5 minutes, upper strata is rich gallium organic phase, and lower floor is liquid after rich indium back extraction.
(7) organic phase in (6) taken out, add the oxalic acid back extraction of 0.5mol/L, 30 DEG C of constant temperature stir 10min.
(8) pour in separating funnel by the two-phase after stirring, leave standstill separatory 5 minutes, upper strata is organic phase after back extraction, and lower floor is liquid after rich gallium back extraction.
(9) under normal temperature to liquid after the rich indium back extraction in (6) add theoretical amount 1.5 times zinc metal sheet displacement obtain simple substance indium.
(10) add the calcium chloride of theoretical amount 1.2 times to liquid after the rich gallium back extraction in (8) under normal temperature, form calcium oxalate precipitation, then cross and filter caoxalate, after filter, liquid adds ammoniacal liquor, obtains gallium hydroxide precipitation.
Claims (5)
1. the method for separation and Extraction indium and gallium from an indium Gallium solution comprises the steps:
(1) extract: with organophosphorus acids reagent for extraction agent, with the one in (sulfonated kerosene, benzene) for thinner, be made into finite concentration organic phase. treat that extraction liquid pH is adjusted to certain value, then add organic extractant phase certain hour, then separatory.
(2) back extraction indium: take concentrated hydrochloric acid as reverse-extraction agent, carries out back extraction to organic phase after the extraction in (1) step, obtains the aqueous phase being rich in indium ion, then separatory.
(3) back extraction gallium: take oxalic acid solution as reverse-extraction agent, to the further back extraction of organic phase after the back extraction in (2) step, obtains the aqueous phase being rich in gallium ion, then separatory.
(4) zinc is added to the aqueous phase being rich in indium ion in (2) or aluminium displacement obtains simple substance indium, or adds alkaloids as ammoniacal liquor, sodium hydroxide, calcium hydroxide etc., obtain indium hydroxide precipitation.
(5) precipitation agent is added to the aqueous phase being rich in gallium ion in (3), form caoxalate, then cross and filter caoxalate, after filter, liquid zinc or aluminium displacement obtain Metallic Gallium, or add alkaloids as ammoniacal liquor, sodium hydroxide, calcium hydroxide etc., obtain gallium hydroxide precipitation.
Back extraction order in the present invention is exchanged, and other processing parameter is constant also can realize technological effect, so also can be following steps:
(6) extract: with organophosphorus acids reagent for extraction agent, with the one in (sulfonated kerosene, benzene) for thinner, be made into finite concentration organic phase. treat that extraction liquid pH is adjusted to certain value, then add organic extractant phase certain hour, then separatory.
(7) back extraction gallium: take oxalic acid solution as reverse-extraction agent, carries out back extraction to organic phase after the extraction in (6) step, obtains the aqueous phase being rich in gallium ion, then separatory.
(8) back extraction indium: take concentrated hydrochloric acid as reverse-extraction agent, to the further back extraction of organic phase after the back extraction in (7) step, obtains the aqueous phase being rich in indium ion, then separatory.
(9) precipitation agent is added to the aqueous phase being rich in gallium ion in (7), form caoxalate, then cross and filter caoxalate, after filter, liquid zinc or aluminium displacement obtain Metallic Gallium, or add alkaloids as ammoniacal liquor, sodium hydroxide, calcium hydroxide etc., obtain gallium hydroxide precipitation.
(10) zinc is added to the aqueous phase being rich in indium ion in (8) or aluminium displacement obtains simple substance indium, or add alkaloids as ammoniacal liquor, sodium hydroxide, calcium hydroxide etc., obtain indium hydroxide precipitation.
2. by described in (1) or (6) in claim 1, extraction agent is one or more in organophosphorus acids reagent (P204, P507, P501, Cyanex272, Cyanex301, B312), thinner is the one in (sulfonated kerosene, benzene), extractant concentration is 5% ~ 30%, treat that extraction liquid pH is adjusted to 1 ~ 2.5, comparing O/W is 1:5 ~ 5:1, and temperature remains on 5 ~ 50 DEG C, stirs or centrifugal 2 ~ 30min.
3., by described in (2) or (8) in claim 1, concentrated hydrochloric acid concentration is 6 ~ 12 mol/L, and back extraction temperature is 5 ~ 50 DEG C, and comparing O/W is 8:1 ~ 1:1, stirs or centrifugal 2 ~ 30min.
4., by described in (3) or (7) in claim 1, oxalic acid solution concentration is 0.1 ~ 1mol/L, and temperature is 5 ~ 50 DEG C, and comparing O/W is 8:1 ~ 1:1, stirs or centrifugal 2 ~ 30min.
5. by described in (5) or (9) in claim 1, precipitation agent is one or more in (calcium chloride, calcium hydroxide, calcium oxide, nitrocalcite, calcium sulfate), addition is theoretical amount 1 ~ 1.5 times, temperature of reaction is 5 ~ 80 DEG C, alkaloids is one or more in ammoniacal liquor, sodium hydroxide, calcium hydroxide, and precipitation pH value is 2 ~ 11.
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Cited By (2)
| Publication number | Priority date | Publication date | Assignee | Title |
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| CN105420502A (en) * | 2015-11-27 | 2016-03-23 | 四川长虹格润再生资源有限责任公司 | Method for recovering indium from waste liquid crystal display screen panel |
| CN108300877A (en) * | 2017-12-29 | 2018-07-20 | 深圳市中金岭南有色金属股份有限公司丹霞冶炼厂 | The method of gallium germanium indium in extraction and recovery zinc replacement slag leachate |
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| CN105420502A (en) * | 2015-11-27 | 2016-03-23 | 四川长虹格润再生资源有限责任公司 | Method for recovering indium from waste liquid crystal display screen panel |
| CN105420502B (en) * | 2015-11-27 | 2018-08-14 | 四川长虹格润环保科技股份有限公司 | The method of recovery indium from waste LCD panel |
| CN108300877A (en) * | 2017-12-29 | 2018-07-20 | 深圳市中金岭南有色金属股份有限公司丹霞冶炼厂 | The method of gallium germanium indium in extraction and recovery zinc replacement slag leachate |
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