CN107955886A - A kind of method that indium is extracted from rich indium alkali oxidation scum - Google Patents
A kind of method that indium is extracted from rich indium alkali oxidation scum Download PDFInfo
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- CN107955886A CN107955886A CN201711292920.5A CN201711292920A CN107955886A CN 107955886 A CN107955886 A CN 107955886A CN 201711292920 A CN201711292920 A CN 201711292920A CN 107955886 A CN107955886 A CN 107955886A
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- indium
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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
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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
- C22B13/00—Obtaining lead
- C22B13/04—Obtaining lead by wet processes
- C22B13/045—Recovery from waste materials
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/001—Dry processes
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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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- 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
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/04—Working-up slag
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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
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Abstract
The present invention relates to a kind of method that indium is extracted from rich indium alkali oxidation scum.Process, leached mud washing step, leachate aluminium displacement process, sponge indium briquetting process, briquetting alkali fusion refining process and melting matter are leached except cadmium except thallium process obtains thick indium by rich indium alkali oxidation scum washing step, washing slag.The solvent that sulfuric acid and chloride are formed disposably leaches rich indium alkali oxidation scum, indium leaching rate can reach more than 99.5%, compared with traditional secondary dilute sulfuric acid counterflow leaching, it is short with technological process, leaching velocity is fast, and reaction temperature is low, easy to operate, many advantages, such as leachate impurity content is low, and the leaching rate of indium is high.Applied suitable for being extracted from rich indium lead bullion alkali oxidation scum in indium metal.
Description
Technical field
The present invention relates to non-ferrous metal metallurgy Comprehensive Recovery Technology, and in particular to one kind is extracted from rich indium alkali oxidation scum
The method of indium.
Background technology
During crude zinc rectifying, high boiling metal such as lead, indium are enriched in the liquation hearth of rectifying lead tower, are passed through
Liquate separates, and obtains indium-containing crude lead.At present, from rich indium lead bullion the valuable metal generally use such as recovery indium into the lead bullion of melting
Oxidant is added, carries out oxidative slagging.Since indium and most of impurity metallic elements are bigger than lead to the affinity ability of oxygen, these gold
Belong to element and slag making reaction preferentially occurs with oxygen, so as to fulfill effective enrichment of indium and the purpose of refined lead.The oxidation of generally use
Agent is compressed air, makees oxidant due to the use of air, reaction temperature is high, and the volatilization of lead is serious, the content of indium in rich indium scum silica frost
It is relatively low, it is only 2%-3% containing indium, flue dust mechanical loss is big.The shortcomings that for air oxidation process, someone is developed using nitric acid
The method that sodium replaces air oxidant Enrichment Indium, effectively overcomes the shortcomings of air oxidation.The scum silica frost that two kinds of oxidizing process are obtained
The thing phase of component differs greatly, even if the rich indium alkaline residue of sodium nitrate oxidation is leached using low, high concentrated acid second adverse current, leaching
Amount containing indium is still up to 1%-2% in slagging tap, and indium leaching rate is only 80%-85%.How from rich indium alkaline residue higher proportion is extracted
Indium be the problem of this area is anxious to be resolved.
The content of the invention
The problem of in order to overcome second adverse current sulfuric acid leaching indium efficiency low, the present invention propose a kind of from rich indium alkali oxidation scum
The method of middle extraction indium.This method extracts indium metal by the solvent that sulfuric acid and chloride form from rich indium alkali oxidation scum,
Solve the problems, such as the recovery technology of indium.
Scheme is used by the present invention solves technical problem：
1st, rich indium alkali oxidation scum washing step：By the alkali oxidation scum containing indium 30-100 DEG C of water washing, the mistake of washing
Mechanical agitation is carried out in journey, a part of sodium hydroxide and some water miscible impurity is washed off, then filters, carries out liquid and solid
Separation, filtrate are used to recycle alkali, and gained washing slag enters washing slag and leaches process；
2nd, washing slag leaches process：Washing slag is put into container, container is placed in micro-wave oven, is added in washing slag
Enter what aqueous sulfuric acid and concentration aqueous chloride solution 0.5-10mol/L between of the concentration between 1-6mol/L was formed
The mass ratio of solvent, washing slag and solvent is 1: 2-10, and washing slag is leached, and extraction temperature is leached at 30-100 DEG C
Time when 1-8 is small, then filters, and is allowed to liquid and is separated with solid portion, obtains leached mud and leachate；
3rd, leached mud washing step：Separated leached mud is washed after extraction, carries out liquid after washing again
Body is separated by filtration with solid portion, and the wash water of wherein liquid condition is transmitted back to washing slag and leaches process, and the solid washery slag of gained is used
In recycling lead；
4th, leachate aluminium displacement process：Aluminium is added in washing slag leaches the leachate isolated in process, aluminium is carried out and puts
Change, sponge indium is obtained after separation.
5th, sponge indium briquetting process：By it is separated go out sponge indium carry out briquetting, be allowed to density increase；
6th, briquetting alkali fusion refining process：Sponge indium Jing Guo briquetting is put into basic species, the alkali fusion refining of indium is carried out, obtains
Alkali melting matter；
7th, alkali melting matter removes thallium process except cadmium：In alkali melting matter, add potassium iodide or iodine and remove cadmium, add zinc chloride or
Ammonium chloride, removes thallium, obtains thick indium.
The beneficial effects of the invention are as follows：
The solvent that the present invention is formed using sulfuric acid and chloride disposably leaches rich indium alkali oxidation scum, indium leaching
Extracting rate can reach more than 99.5%, short with technological process compared with traditional secondary dilute sulfuric acid counterflow leaching, leaching velocity
It hurry up, many advantages, such as reaction temperature is low, easy to operate, and leachate impurity content is low, and the leaching rate of indium is high.The present invention be suitable for from
Indium metal is extracted in rich indium lead bullion alkali oxidation scum.
Embodiment
Below by specific embodiment, the present invention is described in detail.
1st, rich indium alkali oxidation scum washing step：By the alkali oxidation scum containing indium, with 30-100 DEG C of water washing 2-3 times, wash
Mechanical agitation is carried out during washing, washes a part of sodium hydroxide and some water miscible impurity off, then vacuum filter, is carried out
Solid is separated with liquid, and filtrate recycling sodium hydroxide, gained washing slag, which enters, leaches process.
2nd, washing slag leaches process：The obtained filter residue of washing will be passed through to be put into container, container is placed in micro-wave oven
In, solvent is added, washing slag is leached.After reaching extraction time, filtered, be allowed to liquid and separated with solid portion,
Obtain leached mud and leachate.
The mass ratio of washing slag and solvent is 1:2-10,30-100 DEG C of extraction temperature, when extraction time 1-8 is small.
During leaching, the impurity such as zinc, cadmium, tin, arsenic in rich indium alkali oxidation scum is leached entrance together with indium
In solution, and PbO and H2SO4Reaction generation PbSO4Precipitation, a small amount of Pb and PbSO4With Cl-Interaction generation PbCl2, enter
In solution.Indium is down to less than 0.05% in leached mud, and the leaching rate of indium reaches more than 99.5% in rich indium alkali oxidation scum.
It is prepared by solvent：In dilute H2SO4The chloride of addition setting concentration in solution, such as hydrochloric acid, sodium chloride, calcium chloride, chlorination
Ammonium and soluble chloride.Wherein hydrionic concentration between 1-6mol/L, the concentration of chlorion 0.5-10mol/L it
Between.
3rd, leached mud washing step：Separated leached mud is washed after extraction, carries out liquid after washing again
Body is separated by filtration with solid portion, and the wash water of wherein liquid condition is transmitted back to leaching process, and the solid washery slag of gained is used to recycle
Lead.
4th, leachate aluminium displacement process：Aluminium is added in washing slag leaches the leachate isolated in process, aluminium is carried out and puts
Change, its dosage is 1.2 times of theoretical amount, and sponge indium is obtained after separation.
5th, sponge indium briquetting process：By it is separated go out sponge indium carry out briquetting, be allowed to density increase.
6th, briquetting alkali fusion refining process：Sponge indium Jing Guo briquetting is put into caustic soda, the alkali fusion refining of indium is carried out, obtains alkali
Melting matter.
7th, alkali melting matter removes thallium process except cadmium：In alkali melting matter, add potassium iodide or iodine and remove cadmium, add zinc chloride or
Ammonium chloride, removes thallium, obtains thick indium.
Embodiment 1
500 grams of rich indium alkali oxidation scums are taken, the mass percent that its component is formed is：In 4.86%, Zn 5.33%, Pb
60.21 %, Cu 0.12%, Bi 0.59%, Sb 0.57%, Fe 0.20%, Sn 0.12%, surplus are alkali compound.Leach
When washing slag and solvent mass ratio be 1: 5.The concentration of sulfuric acid is 6mol/L in solvent, and the concentration of chloride (ion) is
0.5mol/L.60-70 DEG C of extraction temperature, when extraction time 5 is small.It is separated by filtration, wash, dry, weighs.Measure indium in leached mud
Mass percent be 0.018%, leaching process indium leaching rate be 99.70%.
Embodiment 2
500 grams of rich indium alkali oxidation scums are taken, the mass percent that its component is formed is：In 5.19%, Zn 2.76%, Pb
62.28 %, Cu 0.10%, Bi 0.50%, Sb 0.26%, Fe 0.18%, Sn 0.08%, surplus are alkali compound.Leach
When washing slag and the mass ratio of solvent be 1: 5, the concentration of sulfuric acid is 4mol/L in solvent, and the concentration of chloride is 1.5mol/L.
70-80 DEG C of extraction temperature, when extraction time 5 is small.It is separated by filtration, wash, dry, weighs.Measure the quality hundred of indium in leached mud
Divide than being 0.02%, leaching process indium leaching rate is 99.69%.
Embodiment 3
500 grams of rich indium alkali oxidation scums are taken, the mass percent that its component is formed is：In 8.53%, Zn 1.20%, Pb
58.26 %, Cu 0.11%, Bi 0.60%, Sb 0.65%, Fe 0.22%, Sn 0.08%, surplus are alkali compound.Leach
When washing slag and the mass ratio of solvent be 1: 5, the concentration of sulfuric acid is 3mol/L in solvent, and the concentration of chloride is 2mol/L.Leaching
Go out 80-90 DEG C of temperature, when extraction time 5 is small.It is separated by filtration, wash, dry, weighs.Measure the quality percentage of indium in leached mud
Than for 0.03%, leaching process indium leaching rate is 99.71%.
Embodiment 4
500 grams of rich indium alkali oxidation scums are taken, the mass percent that its component is formed is：In 7.65%, Zn 1.50%, Pb
59.35 %, Cu 0.12%, Bi 0.29%, Sb 0.30%, Fe 0.22%, Sn 0.12%, surplus are alkali compound.Leach
When washing slag and the mass ratio of solvent be 1: 5, the concentration of sulfuric acid is 2mol/L in solvent, and the concentration of chloride is 3mol/L.Leaching
Go out 60-70 DEG C of temperature, when extraction time 6 is small.It is separated by filtration, wash, dry, weighs.Measure the quality percentage of indium in leached mud
Than for 0.03%, leaching process indium leaching rate is 99.69%.
Embodiment 5
500 grams of rich indium alkali oxidation scums are taken, the mass percent that its component is formed is：In 9.63%, Zn 0.85%, Pb
62.56 %, Cu 0.08%, Bi 0.25%, Sb 0.20%, Fe 0.15%, Sn 0.06%, surplus are alkali compound.Leach
When washing slag and the mass ratio of solvent be 1: 5, the concentration of sulfuric acid is 2mol/L in solvent, and the concentration of chloride is 4mol/L.Leaching
Go out 90-100 DEG C of temperature, when extraction time 6 is small.It is separated by filtration, wash, dry, weighs.Measure the quality hundred of indium in leached mud
Divide than being 0.05%, leaching process indium leaching rate is 99.58%.
Claims (2)
- A kind of 1. method that indium is extracted from rich indium alkali oxidation scum, it is characterised in that be by process：1) rich indium alkali oxidation scum washing step：By the alkali oxidation scum containing indium with 30-100 DEG C of water washing, during washing Mechanical agitation is carried out, a part of sodium hydroxide and some water miscible impurity is washed off, then filters, carries out liquid and solid point From filtrate is used to recycle alkali, and gained washing slag enters washing slag and leaches process；2) washing slag leaches process：Washing slag is put into container, container is placed in micro-wave oven, is added in washing slag dense The aqueous chloride solution of aqueous sulfuric acid and concentration between 0.5-10mol/L spent between 1-6mol/L is formed molten The mass ratio of agent, washing slag and solvent is 1:2-10, leaches washing slag, and extraction temperature is at 30-100 DEG C, leaching Between when 1-8 is small, then filter, be allowed to liquid and separated with solid portion, obtain leached mud and leachate；3) leached mud washing step：Separated leached mud is washed after extraction, carried out again after washing liquid with Solid portion is separated by filtration, and the wash water of wherein liquid condition is transmitted back to washing slag and leaches process, and the solid washery slag of gained is used for back Receive lead；4) leachate aluminium displacement process：Aluminium is added in washing slag leaches the leachate isolated in process, carries out aluminium displacement, point From rear acquisition sponge indium；5) sponge indium briquetting process：By it is separated go out sponge indium carry out briquetting, be allowed to density increase；6) briquetting alkali fusion refining process：Sponge indium Jing Guo briquetting is put into basic species, the alkali fusion refining of indium is carried out, obtains alkali fusion Refine thing；7) alkali melting matter removes thallium process except cadmium：Potassium iodide is added in alkali melting matter or iodine removes cadmium, adds zinc chloride or chlorination Ammonium, removes thallium, obtains thick indium.
- 2. the method according to claim 1 that indium is extracted from rich indium alkali oxidation scum, it is characterised in that：The chloride For potassium chloride, sodium chloride, calcium chloride, ammonium chloride or hydrogen chloride.
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| Application Number | Priority Date | Filing Date | Title |
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| CN201711292920.5A CN107955886A (en) | 2017-12-08 | 2017-12-08 | A kind of method that indium is extracted from rich indium alkali oxidation scum |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115418501A (en) * | 2022-09-02 | 2022-12-02 | 合肥工业大学 | Method for recovering metal indium from waste ITO glass |
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| CN101660053A (en) * | 2009-09-22 | 2010-03-03 | 中南大学 | Method for recovering tin, antimony and lead and enriching indium from tin residue |
| CN101831550A (en) * | 2010-05-21 | 2010-09-15 | 葫芦岛锌业股份有限公司 | Method for extracting indium from alkali oxidation scum rich in indium |
| CN103436706A (en) * | 2013-08-14 | 2013-12-11 | 河池市津泰资源再生有限公司 | Method for processing low-grade waste zinc slag to recover zinc, silver, lead and indium |
| CN104131174A (en) * | 2014-07-29 | 2014-11-05 | 广西金山铟锗冶金化工有限公司 | Smelting method for comprehensive recovery of tin lead antimony silver zinc indium in bulk concentrate from ore dressing |
| CN104831077A (en) * | 2015-04-01 | 2015-08-12 | 郴州雄风环保科技有限公司 | Method for extracting and separating indium and tin from indium-containing leaching residues |
| CN106119550A (en) * | 2016-07-29 | 2016-11-16 | 上海交通大学 | The recovery method of indium in a kind of waste liquid crystal panel mechanical stripping product |
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2017
- 2017-12-08 CN CN201711292920.5A patent/CN107955886A/en not_active Withdrawn
Patent Citations (7)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101532091A (en) * | 2009-04-17 | 2009-09-16 | 深圳市中金岭南有色金属股份有限公司韶关冶炼厂 | Technology of extracting and separating valuable metals such as Pb, In, Sb, Cu and Sn from lead smelting converter slags |
| CN101660053A (en) * | 2009-09-22 | 2010-03-03 | 中南大学 | Method for recovering tin, antimony and lead and enriching indium from tin residue |
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| CN103436706A (en) * | 2013-08-14 | 2013-12-11 | 河池市津泰资源再生有限公司 | Method for processing low-grade waste zinc slag to recover zinc, silver, lead and indium |
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Cited By (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN115418501A (en) * | 2022-09-02 | 2022-12-02 | 合肥工业大学 | Method for recovering metal indium from waste ITO glass |
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Application publication date: 20180424 |