CN101760654B - Method for recovering indium from indium-containing waste - Google Patents
Method for recovering indium from indium-containing waste Download PDFInfo
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- CN101760654B CN101760654B CN2008102414843A CN200810241484A CN101760654B CN 101760654 B CN101760654 B CN 101760654B CN 2008102414843 A CN2008102414843 A CN 2008102414843A CN 200810241484 A CN200810241484 A CN 200810241484A CN 101760654 B CN101760654 B CN 101760654B
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Abstract
The invention relates to a method for extracting indium from indium-containing waste and is characterized in that as the process of adding nitric acid is adopted for the acid leaching process, the leaching rate and extraction rate of indium are improved. The invention includes the steps of acid leaching, reduction, sedimentation, hydrochloric acid dissolving, replacement, secondary replacement and ingot casting. The indium-containing waste is processed through the steps and can be cast into crude indium ingots.
Description
Technical field
The present invention relates to a kind of method of from indium-containing wastes such as secondary zinc oxide, plumbous mud, flue dust, extracting indium.
Technical background
Big quantity research has been carried out in the separation and the enrichment of scattered metals indium in the smelting zinc waste residue both at home and abroad.Wherein extraction process, ion exchange method, liquid-film method etc. can separate and the enrichment indium from the utilising zinc containing waste residue leach liquor effectively.
Extracting indium method commonly used mainly contains following several:
(1) low acidleach goes out～solvent extraction
This method is directly leached the raw material slag with the sulfuric acid of lower concentration, and leaching liquid extracts with extraction agent, extracts scattered metals indium.In sulfuric acid, add sodium-chlor and Manganse Dioxide and can reduce the leaching rate that impurity disturbed and improved indium, contain the feed liquid of indium leaching liquid after the leaching as extraction of indium.It is of a great variety, wherein comparatively commonly used with the P204 extraction agent to be used for the extraction agent of extraction of indium, and therefore, low acidleach goes out～and extraction process is also referred to as P204 solvent (dialkyl group phosphoric acid, D2EHPA) extraction process.In hydrochloric acid medium, TBP (tributyl phosphate) has good extraction ability to indium; Extration resin N503 (N, N～DOAA di sec octylacetamide) extraction of indium effectively in hydrochloric acid, Hydrogen bromide or sulfuric acid～Sodium Bromide system.Test shows that in hydrochloric acid system, the N503 extration resin reaches 76% to the suction collection rate maximum of indium, in the Hydrogen bromide system, when Hydrogen bromide concentration during at 2mol/L, resin to the suction collection rate of indium near 100%.P570～P350 mixed extractant is the good extraction agent of separation and concentration Trace Indium, is applicable to separate indium, iron, and effect is better; Aminoresin and N235 are used for that the separation and concentration of indium is also had report or the like.Because indium is in the loss of the links such as washing, reextraction of extraction, load organic phases, the total yield of indium is about about 80%.
(2) indium is reclaimed in vacuum distilling
It is one of processing method of the direct comprehensive reutilization hard zinc fast of comparison that indium is reclaimed in vacuum distilling.Distill out zinc and zinc lead alloy with vacuum oven from plumbous zinc ore, the indium in the plumbous zinc is enriched in the distillation residue, is called the vacuum slag, contains the indium of high level in the vacuum slag.Vacuum distillating hard-zinc is at vacuum tightness 66～106Pa, 1000 ℃ of temperature, and constant temperature distillation 40～100min, the concentration ratio of indium in residue is greater than 915 times, and direct yield is greater than 90%.Adopt the alkali fusion slag making to capture indium, wash the technology of removing alkali, nitration mixture leaching indium, the rate of recovery can reach 85%.Adopt sulfuric acid slaking leaching, iron powder replacement removal of impurities, P204 extracting and enriching technology from the reverberatory furnace flue dust, to reclaim indium, indium recovery about 85%.This technology has the multiple valuable metal characteristics of a step enrichment simultaneously, carries zinc and enrichment indium, silver etc. are finished simultaneously, the short direct yield height of flow process; Advanced technology is polluted gently, consumes and lacks, and cost is low.
(3) liquid-film method separation and concentration scattered metals indium
The liquid film separate substance is a kind of efficient, quick, energy-conservation high-new isolation technique.With P291 is that the emulsion liquid film that flowing carrier prepares can promptly move the enrichment indium.Be that flowing carrier, L113A are that tensio-active agent, whiteruss are that toughener, the kerosene of film is the solvent of film with P291, the sulfuric acid and the hydrazonium sulfate aqueous solution are the Liquid Membrane System of interior phase reagent, the acidity of foreign minister's test solution (or feed liquid) is pH3～4, migration enrichment indium, and effect is fairly good.Test shows that the migration accumulation rate of indium can reach 99.5%.With P507 is the emulsion liquid membrane extracting indium of flowing carrier, and the good rate of recovery is also arranged.Test-results show the emulsion liquid film system of P507～L113A～kerosene can be at a high speed, move indium effectively, to containing In
3+0.2g/L analog material liquid, the indium extraction yield can reach more than 99%.With P350 (methyl acid phosphate diformazan fat in heptan), be moving phase with the 1.0mol/L Hydrogen bromide, silica gel is made carrier, and extraction chromatography separates indium, can realize and highly selective Quantitative Separation such as a large amount of galliums, copper, iron, cobalt, nickel and aluminium.
(4) other reclaims the method for indium
Alkali fusion～soda boiling～acidleach indium-extracting process has that flow process and equipment are simple, advantages such as less investment, the rate of recovery height of indium, processing ease, production cost are low, remarkable in economical benefits, and indium recovery is about 90%, and this method weak point is that alkaline consumption is bigger.In addition, also have synthetic method to carry indium, adopt technologies such as two sections leachings (first neutrality leaches to such an extent that contain the indium slag, and acidity leaches again) and displacement, reach the purpose of separation of Zinc, lead and enrichment indium; The oxidative slagging method is carried indium, utilizes principle that indium is much higher than plumbous affinity to oxygen to the affinity of oxygen to realize separating of indium and lead etc., must contain the indium scum silica frost through oxidative slagging.Neutral earlier the leaching removed most of zinc, leaches with the vitriol oil again, and the leach liquor that contains indium is directly replaced with zinc; Sulfurization roasting water logging technology is carried indium, and raw material is equipped with the vitriol oil and carries out roasting, and indium and heavy metal oxide almost all change into vitriol, and major part in roasting process such as impurity arsenic, selenium, fluorine, chlorine is volatilized and removed.The calcining of output is after water logging goes out, and the leach liquor that contains indium is as the extraction of indium feed liquid.
On the whole, the at present domestic secondary zinc oxide that utilizes is mainly used in hydrometallurgy and manufacturing zinc salt.Its technology is: acidleach → neutrality leaches (pH＜5) → acidleach.What take is neutral leach liquor.Because Fe with this understanding
3+Be hydrolyzed to Fe (OH)
3, simultaneously Sb, As are brought in the slag.Though zinc leaches not exclusively, still have acidleach to reclaim zinc.Neutral again leaching goes round and begins again.PH=5 when leaching because of neutrality, indium, bismuth etc. remains in the slag entirely, and slag is mainly lead, producer sells pyrometallurgical smelting of lead factory.Though plumbous factory can be in reclaiming flue dust recovery part, can only reclaim 40% in the ash, cause 60% indium waste, and indium is a rare metal, is important material for preparedness against war, the reserves in the earth have only 10
-7, waste is real like this is unfortunate.
In these methods, the rate of recovery of indium often depends on the leaching yield of indium.For indium complicated and changeable being separated and extracting, on the principles of chemistry, must make the indium compound that is insoluble in acid, alkali and water be converted into the indium of solubility.When adopting routine techniques and technology to carry out the indium recovery and utilize, mainly adopt the method for high-temperature roasting, make the compound transformation of indium and enter gas phase, after gathering dust, indium is carried out enrichment once more.Adopt two to three sections acidleach to go out method to indium enrichment material,, adopt method of extraction that indium is separated with other metallic elements again, after the back extraction of extraction liquid knot, adopt the method for metal replacement to generate thick indium the compound dissolution of indium.This wherein, the leaching yield of indium is to the final extraction yield important influence of indium.
Adopt appropriate solvent, valuable constituent is extracted from solid, the process that the solution of gained is separated from unwanted raw material is referred to as leaching or leaching process.Leaching is the complicated heterogeneous reaction process of solvent and solid state reaction.In conventional zinc hydrometallurgy production process, traditional indium process of enriching is the zinc oxide extract technology.The zinc hydrometallurgy factory of China, zinc oxide leaches and adopts two sections leachings usually, and one section is neutral the leaching, and one section is acid the leaching.In the zinc oxide leaching process that extracts indium, the neutral leaching as first section, indium iron is present in neutrality and soaks in the slag, the acid leaching as second section.
Roasted ore (ZnO) extract technology can be divided into conventional acid the leaching and two kinds of technologies of hot acid leaching again.In conventional acid the leaching, the acid purpose that leaches is to guarantee that as far as possible the zinc in the calcining dissolves to greatest extent, also will avoid a large amount of impurity dissolvings simultaneously, and the terminal point sulfuric acid content of general control is 1～5g/l, is applicable to that the few roasted ore of iron content leaches.This method zinc ferrite can not dissolve, and the leaching yield of zinc is low, and the leaching yield of indium is also low, improves the leaching that terminal point acidity helps indium.
Adopt present sulfuric acid to soak indium technology and from secondary zinc oxide, soak indium, the leaching rate of indium is lower than 70%, and pickling liquor can obtain thick sponge indium through the operation of multisteps such as iron filings removal of impurities, clarification filtration, extraction, reextraction, zine plate displacement, total yield is less than 60%, and a large amount of indiums run off in process of production.No matter from economically, or on the environmental benefit, all bring loss, and foreign matter content height in the thick indium product of gained, therefore,, have great importance to how improving the research of the leaching rate of indium in the secondary zinc oxide.The major cause that indium recovery is not high is that leaching rate is not high, accounts for 60～70% of total number of dropouts, at present not about the research to leaching indium in the secondary zinc oxide.Have experiment to show: the existence of acidity, solid-to-liquid ratio, temperature, reaction times, granular size and some oxygenant, all have influence on the leaching rate of indium, control under suitable condition, the leaching rate of indium can reach more than 97%.
The speed of leaching is represented with the amount of substance of transferring in the unit time in the solution (or amount of the reactive material that is consumed in the unit time).It is relevant with many factors such as surface-area of concentration of reactants, temperature, stirring velocity and solid phase, and these factors may change in leaching process.Process comprised with the next stage:
1. pass through the liquid film layer on the solid surface, the reactant in the liquid phase is to the diffusion mass transfer process of solid phase surface;
2. reactant is through solid product layer or the residual material bed diffusion mass transfer process that is not leached;
3. leached the lip-deep chemical reaction process of thing;
4. dissolved thing through the solid product layer by the outside diffusion process of reaction surface;
5. the liquid film layer on the dissolved thing process solid phase surface is to the solution diffusion process.
In liquid and solid phase reaction, owing to be reflected on the phase interface and carry out, whole process comprises diffusion process and chemical reaction two parts, the factor of influence process speed also has the influence of factors such as viscosity, liquid-solid ratio, solid granularity, specific surface utilization ratio and rate of diffusion except that temperature, concentration with the reaction times.To a certain definite liquid-solid system, same whipping device, when temperature of reaction was not added control by autothermal equilibrium, the principal element that influences the indium leaching rate was reaction times, leaching agent concentration, grain graininess, stirring velocity and liquid-solid ratio L/S.
Summary of the invention
Purpose of the present invention just provides a kind of leaching method of uniqueness, improves the leaching rate of indium, reaches the rate of recovery that improves indium.
For achieving the above object, the invention provides following technical scheme:
(1) acidleach
Liquid-solid mass ratio 1: 2～4 times, Xian Jiashui under agitation adds raw materials such as secondary zinc oxide slag or plumbous mud, stirs out that to add concentration behind the solid material be 10～15% sulfuric acid, adds concentration behind about 1～2h and is 20～50% nitric acid and stir 30～40min again, reaction terminating.
In
2O
3+3H
2SO
4＝In
2(SO
4)
3+3H
2O
In
2O
3+6HNO
3＝2In(NO
3)
3+3H
2O
(2) reduction
Solution in (1) filtered and for several times with distilled water wash.It is 10～30% oxalic acid that filtrate adds concentration, with Fe
3+Be reduced into Fe
2+
2Fe
3++C
2O
4 2～＝2Fe
2++2CO
2↑
(3) precipitation
Add a certain amount of Na again
3PO
4, make In be converted into InPO
4, because of InPO
4PH reduces during hydrolysis, can not reduce the grade of indium because of the Zn hydrolysis.
In
3++PO
4 3+＝InPO
4
Solution stirring 30～the 40min of gained transfers pH=3～5 with NaOH solution, filters, washs.Slag is mainly In (OH)
3
In
3++3OH
～＝In(OH)
3
(4) dissolving with hydrochloric acid
With this In (OH)
3Slag concentration is 30% dissolving with hydrochloric acid.
In(OH)
3+3HCl＝InCl
3+3H
2O
Fe(OH)
2+2HCl＝FeCl
2+2H
2O
Zn(OH)
2+2HCl＝ZnCl
2+2H
2O
(5) displacement
Carry out the displacement first time through the solution behind the dissolving with hydrochloric acid,, can cement out than zinc, the positive element in ferroelectric position with the iron plate displacement.
2In
3++3Fe→2In+3Fe
2+
(6) twice replaced
Slag after the displacement is used dissolving with hydrochloric acid again, obtains thick indium with the zine plate displacement afterwards.
2In+6HCI＝2InCl
3+3H
2↑
2InCI
3+3Zn＝2In+3ZnCl
2
(7) this thick indium is used the removal of impurities of molten sheet alkali again, can get thick indium ingot by ingot casting.
Better scheme of the present invention is: add the vitriol oil earlier in step (1), add nitric acid again, will not be dissolved in H
2SO
4In indium dissolving, the leaching yield of indium is brought up to more than 80%.Produce small amount of N O in this process
2, can on reactor, add a belt air-suction cover, with absorbing in the plastic fan suction alkali lye.
Better scheme of the present invention also can be: in step (2), add oxalic acid and reduce, when solution colour by the brown green that changes into, can think Fe
3+Be reduced into Fe fully
2+, stop to add oxalic acid.Because of Fe
3+The pH value and the In of hydrolysis
3+The pH value scope of hydrolysis exists intersects, and can influence the grade of indium, so earlier with Fe
3+Be converted into Fe
2+
Description of drawings
Accompanying drawing is the process flow sheet of this invention.
Specific embodiment
Below in conjunction with specific examples the present invention is described in more details, protection scope of the present invention includes but not limited to following example.
Example 1:
Claim 200g to contain the secondary zinc oxide slag of indium 0.0421%, wherein contain the 84.2mg indium, at first add 1030ml water in container, stir 10min, the back adds 110ml 98%H
2SO
4Reaction 80min adds 1mlHNO
3React 30min again, filtration, washing obtain leach liquor 1100ml, and this leach liquor contains indium 0.07034g/L, reclaims indium 77.37mg altogether, leaching yield 91.90%.
Example 2:
Claim 100g to contain the secondary zinc oxide slag of indium 0.0421%, at first add 515ml water in container, stir 10min, the back adds 55ml 98%H
2SO
4Reaction 80min adds 0.5mlHNO
3React 30min again, filtration, washing obtain leach liquor 736.5ml, contain indium 0.05698g/L, reclaim indium 41.9mg altogether, leaching yield 99.28%.
Example 3:
Claim 200g to contain the secondary zinc oxide slag of indium 0.0421%, at first add 1030ml water in container, stir 10min, the back adds 110ml 98%H
2SO
4Reaction 80min adds 1mlHNO
3React 30min again, obtain leach liquor 1200ml, contain indium 0.0648g/L, get indium 77.76mg, leaching yield 92.35%.
Example 4:
Above-mentioned leach liquor is total to 3036.5ml, contains Fe9.22g/L, add water-soluble H earlier
2C
2O
4.2H
2O 65g, reaction times 30min is with Fe
3+Be reduced into Fe
2+, after add 1gNa
3PO
4Reaction 30min uses liquid caustic soda key pH=3～5 again, gets In (OH)
3Precipitation, color is faint yellow, the precipitation oven dry is 2.78g altogether, indium content 7.55%.
Claims (1)
1. method of from indium-containing waste, extracting indium, this method adopts following steps:
(1) acidleach; Liquid-solid mass ratio 1: 2～4 times, Xian Jiashui under agitation adds secondary zinc oxide slag or plumbous mud raw material, stirs out that to add concentration behind the solid material be 10～15% sulfuric acid, adds concentration behind 1～2h and be nitric acid restir 30～40min of 20～50%, reaction terminating;
(2) reduction; The solution that obtains in the step (1) filtered and for several times with distilled water wash; It is the reduction of 10～30% oxalic acid that filtrate adds concentration, with Fe
3+Be reduced into Fe
2+
(3) precipitation; In the solution that step (2) obtains, add Na
3PO
4, make In be converted into InPO
4, gained solution stirring 30～40min, regulating pH with NaOH solution is 3～5, filters, washs, slag is mainly In (OH)
3
(4) dissolving with hydrochloric acid; The In (OH) that step (3) is obtained
3Slag concentration is 30% dissolving with hydrochloric acid;
(5) displacement for the first time; Step (4) is replaced with iron plate through the solution behind the dissolving with hydrochloric acid;
(6) displacement for the second time; Slag after step (5) displacement is used dissolving with hydrochloric acid again, obtain thick indium with the zine plate displacement afterwards;
(7) molten sheet alkali removal of impurities; The thick indium that step (6) is obtained is with the removal of impurities of molten sheet alkali.
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| CN101760654B true CN101760654B (en) | 2011-05-04 |
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Families Citing this family (8)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN102534258B (en) * | 2012-02-22 | 2013-04-03 | 郴州丰越环保科技股份有限公司 | Method for preparing indium and bismuth from coarse bismuth-containing indium |
| CN104451205B (en) * | 2013-09-12 | 2017-01-25 | 汉能新材料科技有限公司 | Indium extraction method capable of efficiently removing iron |
| CN104593599A (en) * | 2014-12-26 | 2015-05-06 | 河南豫光锌业有限公司 | Indium refining slag treatment method and indium refining slag treatment device |
| CN104651617A (en) * | 2015-02-16 | 2015-05-27 | 广西德邦科技有限公司 | Method for extracting indium from alkaline residues |
| CN105018752B (en) * | 2015-07-27 | 2017-12-22 | 昆明理工大学 | A kind of method of separation and concentration and recovery indium in solution of indium from low-concentration sulfuric acid |
| CN105907978B (en) * | 2016-04-20 | 2018-06-29 | 武汉长海高新技术有限公司 | A kind of method of recovery indium in flue dust containing indium |
| CN106222454A (en) * | 2016-09-30 | 2016-12-14 | 西安建筑科技大学 | A kind of from the method containing indium flue dust recovery indium |
| CN109355508B (en) * | 2018-11-21 | 2021-03-26 | 湖南锐异资环科技有限公司 | Comprehensive recovery method of high-arsenic multi-metal indium-containing material |
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|---|---|---|---|---|
| CN101289712A (en) * | 2008-05-27 | 2008-10-22 | 株洲冶炼集团股份有限公司 | Process for recovering indium from indium-containing material |
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