CN1420184A - Method for extracting refined indium from indium tin oxide waste material - Google Patents
Method for extracting refined indium from indium tin oxide waste material Download PDFInfo
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Abstract
The invention relates to a method for extracting refined indium from Indium Tin Oxide (ITO) waste materials. The method takes indium-containing substances such as indium tin oxide waste materials and the like as raw materials, and the raw materials are added into inorganic mixed acid for dissolution, oxidation and indium-tin separation; adding alkali solution and inorganic coprecipitator in the process of separating indium and tin to make impurities of tin and the like generate a compact precipitate which has high settling speed and is easy for solid-liquid separation, and then carrying out solid-liquid separation, replacement, casting anode and electrolysis on the solution to obtain refined indium. The method greatly improves the filtering performance of the precipitate in the indium-tin separation process, enables solid-liquid to be quickly separated, and has the advantages of good tin removal effect, simple process, low cost, indium recovery rate of more than 95 percent and refined indium purity of more than 99.994 percent.
Description
Technical field: the method that the present invention relates to from the indium tin oxide waste material, extract smart indium.
Technical background: the method for extracting indium from indium tin oxide waste material or indium tin mixture mainly is that ITO waste material chip is dissolved in the mineral acid, because the content of tin is higher in the solution, after generally in the extraction process of indium, carrying out the separation of indium tin, from the low solution of indium of stanniferous amount, adopt chemical refining method further to remove other metallic impurity again, make the compound of indium metal or indium.The isolating common method of indium tin is: generate halo stannate throw out in the aqueous solution that contains indium and tin of strong acid and halide-ions coexistence 1., tin is separated selectively (spy opens flat 3-82720, the 3-91838 communique), to contain solution of tin be highly acid but this method must make, if the concentration of acid is low, the halide-ions amount that then needs is big, the positively charged ion requirement of halo stannate ion pairing is also big, this is very uneconomic, and the precipitation growing amount of tin compound also reduces, want selective separation tin just relatively more difficult, sedimentary separation property worsens.2. the spy opens flat 3--91838 communique and has reported another method, is the ITO chip to be dissolved in nitric acid make tin be oxidized to the stannic acid gelatinous precipitate isolating with it method.Though this method need not carried out the separation of tin by the halo hydrochlorate, the dissolution rate of ITO target waste material in nitric acid is very slow, indium tin separation difficulty, and can not remove other metallic impurity in the original ITO target waste material simultaneously.Therefore, need to adopt alkylphosphonic acid carboxylic acid esters extractant and carboxylic acid extractant to carry out reextraction and secondary back extraction.The cyclical operation repeatedly of extraction and reextraction process, the process more complicated in addition, need to use the solvent of high price, so cost is also higher.3. the method according to Te Kaiping-2001-40436 number report is that the ITO chip is dissolved in hydrochloric acid, and with the alkali neutralization, control pH value is decided in the scope, makes tin generate the separation of tin glue throw out and removes.But, in this method, in adjustment pH scope,, realize the solid-liquid separation difficulty during filtration because of the throw out that generates is a colloidal particulate, use filtration auxiliarys such as fiber-like, diatom great soil group to carry out filter operation together usually, throw out is separated.When the filtration auxiliary that uses is the diatomite time-like, can cause the intrusion of elements such as Fe, Ca in order to prevent the diatom great soil group, in advance that its pickling is clean before using diatomite.Separate tin＞0.2g/l the indium-containing aqueous solution of back from the hydrochloric acid stripping to indium tin, the rate of recovery 72%～93% of indium.This shows that the detin effect of this method and the rate of recovery of indium are not satisfied.
Summary of the invention: the objective of the invention is to: provide a kind of and make impurity hydrolysis such as tin generate the throw out that a kind of densification, settling velocity are fast, be easy to remove, improve the rate of recovery of indium, extract the method for smart indium.
Technical scheme of the present invention is: ITO waste material powder is joined in the inorganic mixing acid dissolve, after dissolving, add hydrogen peroxide oxidation in the liquid, adding an amount of alkali in oxidated solution neutralizes, the pH value is controlled in 1～4 scope, and add inorganic coprecipitated dose simultaneously, make impurity hydrolysis such as tin generate the throw out that a kind of densification, settling velocity are fast, be easy to solid-liquid separation, solution makes the smart indium of purity＞99.994% through solid-liquid separation, displacement, founding anode, electrolysis subsequently.
The starting material that present method adopts are that the ITO waste material comprises that corner, smear metal, waste material and indium tin mixture etc. that the used target of sputter coating, target production process produce contain the indium material.Now that this technological process division is as follows:
With the fragmentation of ITO waste material, be finely ground to-200～-250 orders, powder is joined in the inorganic mix acid liquor dissolves, solid-to-liquid ratio 1: 5～10,70～90 ℃ of solvent temperatures, the H of inorganic mixing acid
+Ion initial concentration 2～5mol/l.
2. after dissolving, add hydrogen peroxide oxidation in the liquid, 50～80 ℃ of temperature, in 0.5～3 hour reaction times, the add-on of hydrogen peroxide is with Sn
2+Be oxidized to Sn
4+, 1～2 times of theoretical amount.
3. indium tin separates: this process adopts the automatic hierarchy of control of continuous permanent pH value, oxidated solution, alkaline solution and inorganic coprecipitated dose are joined in first section reactor by under meter respectively, oxidated solution and inorganic coprecipitated dose of velocity ratio are fixed, the flow velocity of alkaline solution is by the permanent pH value control of reaction system, make the pH value remain on certain interior certain value of 1～4 scope, 40～80 ℃ of temperature of reaction.Reaction soln is the complete required time of tin precipitin reaction from first section reactor to the time that overflows from second section reactor, and inorganic coprecipitated dose concentration is 4～13g/l.
4. solution obtains indium-containing aqueous solution through solid-liquid separation subsequently, and indium-containing aqueous solution makes the smart indium of purity＞99.994% through displacement, founding anode, electrolysis.
More than said inorganic mixing acid can be the mixing acid of any two or two or more acid in the acid such as sulfuric acid, nitric acid, phosphoric acid, hydrofluoric acid, hydrochloric acid, Hydrogen bromide.
Alkaline solution can be in the bases such as ammoniacal liquor, sodium hydroxide, potassium hydroxide any.Coprecipitated dose can be villaumite, vitriol or the nitrate of basic metal or alkaline-earth metal.
The advantage of this method is: improved sedimentary strainability in the sepn process of indium tin greatly, made solid-liquid separation easy, detin is effective, indium recovery is high, technology is simple, cost is low.
Embodiment 1: with the fragmentation of ITO waste material, be finely ground to-200～-250 orders, 330 these powder of gram are joined in hydrochloric acid, the nitric acid mixing acid the initial H of mixing acid
+Concentration is 2.65mol/l, solid-to-liquid ratio 1: 10, the liquor capacity of reactor is 3 liters, 80 ℃ of following stirring and dissolving 3 hours, obtain dissolving back liquid, dissolving back liquid adds 157 milliliters of hydrogen peroxide, 50 ℃ of following oxidations 1 hour, obtain oxidated solution, with oxidated solution, 8.3 the potassium sulfate solution of grams per liter concentration is respectively with 22.9ml/min, 17.8ml/min flow velocity add in first section reactor by under meter, 10% sodium hydroxide solution is controlled by the pH value of reaction system, join in first section reactor by under meter, reaction system adopts the control automatically of two sections permanent pH values, and control pH is 1.0,50 ℃ of temperature of reaction; The time that reaction soln overflows from first section reactor to the second section reactor is 30 minutes, and what overflow contains throw out solution after solid-liquid separation, obtains indium-containing aqueous solution, the decreasing ratio 99.21% of tin; Making purity through displacement, founding anode, electrolysis is 99.997% indium metal (impurity component sees Table 1), and the rate of recovery of indium is 95.20%.
Embodiment 2: embodiment 1 same powder 125 grams are joined in sulfuric acid, the mixed in hydrochloric acid acid the initial H of mixing acid
+Concentration is 2.7mol/l, solid-to-liquid ratio 1: 8, and the liquor capacity of reactor is 1 liter, 70 ℃ of following stirring and dissolving 2.5 hours, obtains dissolving back liquid, dissolving back liquid adds 50 milliliters of hydrogen peroxide, 60 ℃ of following oxidations 3 hours, obtains oxidated solution; The Adlerika of oxidated solution, 10.2g/l concentration is joined in the first step reactor by under meter with the flow velocity of 14.1ml/min, 11.7ml/min respectively, the flow velocity of 15% sodium hydroxide solution is by the pH value control of reaction system, join in first section reactor by under meter, reaction system is the controls automatically of two sections permanent pH values, control pH is 1.5,70 ℃ of temperature of reaction; The time that reaction soln overflows from first section reactor to the second section reactor is 25 minutes, and what overflow contains throw out solution after solid-liquid separation, the decreasing ratio 99.17% of tin; It is 99.997% indium metal (impurity component sees Table 1) that indium-containing aqueous solution makes purity through displacement, founding anode, electrolysis, and the rate of recovery of indium is 95.35%.
Embodiment 3: 14.7 kilograms of the same powder among the embodiment 1 are joined in nitric acid, the mixed in hydrochloric acid acid the initial H of mixing acid
+Concentration is 3.144mol/l, solid-to-liquid ratio 1: 10, and the liquor capacity of reactor is 147 liters, dissolves 2 hours down at 90 ℃, obtains dissolving back liquid, dissolving back liquid adds 4 liters of hydrogen peroxide, 70 ℃ of following oxidations 2 hours, obtains oxidated solution; The Adlerika of oxidated solution, 5.8g/l concentration is added in first section reactor by under meter with the flow velocity of 25.3ml/min, 26.3ml/min respectively, the flow velocity of 15% sodium hydroxide solution is by the pH value control of reaction system, join in first section reactor by under meter, reaction system is the control automatically of the permanent pH value of two sections adverse currents, control pH is 2.0,80 ℃ of temperature of reaction; The time that reaction soln overflows from first section reactor to the second section reactor is 40 minutes, and what overflow contains throw out solution after solid-liquid separation, obtains indium-containing aqueous solution, the tin content＜0.1g/l in the solution; Making purity through displacement, founding anode, electrolysis is 99.997% indium metal (impurity component sees Table), and the rate of recovery of indium is 95.20%.
The impurity component analytical results of table 1 electrolytic metal indium
| The electrolysis indium | ? ????In(％) | Impurity chemical ingredients (ppm) | |||||||||
| ????Cu | ????Pb | ????Zn | ????Cd | ????Fe | ????Tl | ????Sn | ????As | ????Al | The impurity summation | ||
| Embodiment one | ????＞99.997 | ????1.5 | ????4.0 | ????2.4 | ????3.0 | ????3.0 | ????1.6 | ????1.8 | ????2.8 | ????8.0 | ????28.1 |
| Embodiment two | ????＞99.997 | ????1.4 | ????4.1 | ????3.8 | ????2.1 | ????3.0 | ????1.6 | ????3.9 | ????2.8 | ????5.7 | ????28.6 |
| Embodiment three | ????＞99.997 | ????1.7 | ????5.1 | ????1.1 | ????4.5 | ????4.9 | ????1.8 | ????1.8 | ????2.9 | ????4.6 | ????28.5 |
| National standard | ????99.993 | ????＜5 | ????＜10 | ????＜15 | ????＜15 | ????＜8 | ????＜10 | ????＜15 | ????＜5 | ????＜7 | ????＜70 |
Claims (5)
1. method of from the ITO waste material, extracting smart indium, this method is that ITO waste material etc. is levigate, be dissolved in the mineral acid, indium tin separates, solution makes smart indium through solid-liquid separation, displacement, founding anode, electrolysis subsequently, it is characterized in that: (1) will dissolve 70～90 ℃ of solvent temperatures in-200～-250 order waste material powder 1: 5～10 inorganic mixing acid that join solid-to-liquid ratio; (2) after dissolving, add hydrogen peroxide in the liquid, 50～80 ℃ of temperature, 0.5～3 hour reaction times; (3) to separate be to add an amount of alkali to neutralize in oxidated solution to indium tin, pH value is controlled in 1～4 scope, and adds inorganic coprecipitated dose simultaneously, makes impurity such as tin generate the throw out that a kind of densification, settling velocity are fast, be easy to solid-liquid separation.
2. a kind of method of extracting indium from the ITO waste material according to claim 1 is characterized in that: inorganic mixing acid can be the mixing acid of any two or two or more acid in the acid such as sulfuric acid, nitric acid, phosphoric acid, hydrofluoric acid, hydrochloric acid, Hydrogen bromide, the H of mixing acid
+Initial concentration is 2-5mol/l.
3. a kind of method of extracting indium from the ITO waste material according to claim 1, it is characterized in that: the add-on of hydrogen peroxide is Sn
2+Be oxidized to Sn
4+1～2 times of theoretical amount.
4. a kind of method of from the ITO waste material, extracting indium according to claim 1, it is characterized in that: inorganic coprecipitated dose can be villaumite, vitriol or the nitrate of basic metal or alkaline-earth metal; Inorganic coprecipitated dose concentration is 4～13g/l.
5. a kind of method of extracting indium from the ITO waste material according to claim 1 is characterized in that: indium tin separates the control automatically of the continuous permanent pH value of employing.
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB021397422A CN1191380C (en) | 2002-11-07 | 2002-11-07 | Method for extracting refined indium from indium tin oxide waste material |
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|---|---|---|---|
| CNB021397422A CN1191380C (en) | 2002-11-07 | 2002-11-07 | Method for extracting refined indium from indium tin oxide waste material |
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| CN1191380C CN1191380C (en) | 2005-03-02 |
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Cited By (21)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100340679C (en) * | 2005-11-01 | 2007-10-03 | 株洲冶炼集团有限责任公司 | Separation method of indium tin mixture |
| CN101113490B (en) * | 2007-09-12 | 2010-05-19 | 昆明理工大学 | Method for leaching indium from indium sulfide concentrate |
| CN101525693B (en) * | 2009-04-17 | 2011-02-09 | 深圳市中金岭南有色金属股份有限公司韶关冶炼厂 | Method for vulcanization, reducing oxidation and enrichment of low-grade material containing arsenic, indium and germanium |
| CN101748433B (en) * | 2008-12-18 | 2011-04-20 | 北京有色金属研究总院 | Purification method of electrolyte in indium electrolysis process |
| CN101701292B (en) * | 2009-10-20 | 2011-08-03 | 南京中锗科技股份有限公司 | Method for recovering indium and tin from ITO waste targets by utilizing oxidation method |
| CN101528986B (en) * | 2006-10-24 | 2011-08-17 | Jx日矿日石金属株式会社 | Method for collection of valuable metal from ITO scrap |
| CN102199706A (en) * | 2011-05-21 | 2011-09-28 | 南京中锗科技股份有限公司 | Method for comprehensively recovering valuable metal in diode core |
| CN101617067B (en) * | 2007-03-27 | 2011-10-26 | Jx日矿日石金属株式会社 | Method of recovering valuable metal from scrap containing conductive oxide |
| CN101981233B (en) * | 2008-03-06 | 2013-02-13 | Jx日矿日石金属株式会社 | Process for recovery of valuable metals from scrap IZO |
| CN103046108A (en) * | 2012-12-24 | 2013-04-17 | 上海申和热磁电子有限公司 | Electrolysis process used in ITO film cleaning |
| CN103103356A (en) * | 2012-11-09 | 2013-05-15 | 柳州百韧特先进材料有限公司 | Process for recovering crude indium and tin from ITO (indium tin oxide) waste target |
| CN104711638A (en) * | 2014-11-21 | 2015-06-17 | 株洲冶炼集团股份有限公司 | Method for extracting indium and tin from waste ITO targets through reduction and electrolysis |
| CN104862482A (en) * | 2014-02-18 | 2015-08-26 | 纳米及先进材料研发院有限公司 | Method of selective recovery of valuable metals from mixed metal oxides |
| CN104975186A (en) * | 2015-07-30 | 2015-10-14 | 赤峰海镧金属材料科技有限公司 | Comprehensive recycling method for ITO film sensor |
| CN105448822A (en) * | 2015-12-15 | 2016-03-30 | 江西沃格光电股份有限公司 | Method for removing ITO (tin indium oxide) on surface of base plate |
| CN107513619A (en) * | 2017-08-14 | 2017-12-26 | 中南大学 | A kind of method of recovery indium and tin in waste material from ito glass |
| CN107604167A (en) * | 2017-09-22 | 2018-01-19 | 京东方科技集团股份有限公司 | Method for treatment of waste material |
| CN108823405A (en) * | 2018-07-09 | 2018-11-16 | 刘罗平 | A kind of dilute immersion liquid method of wet process refining indium |
| CN110018155A (en) * | 2019-03-06 | 2019-07-16 | 江西瑞林稀贵金属科技有限公司 | A kind of method of tin amount in aes determination electronic waste smelting ash |
| CN110498443A (en) * | 2019-08-23 | 2019-11-26 | 云南锡业集团（控股）有限责任公司研发中心 | A method of with ITO give up target recasting ITO powder |
| CN115650281A (en) * | 2022-10-24 | 2023-01-31 | 广东欧莱高新材料股份有限公司 | Method for recovering indium and gallium from waste target material |
-
2002
- 2002-11-07 CN CNB021397422A patent/CN1191380C/en not_active Expired - Lifetime
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| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN100340679C (en) * | 2005-11-01 | 2007-10-03 | 株洲冶炼集团有限责任公司 | Separation method of indium tin mixture |
| CN101528986B (en) * | 2006-10-24 | 2011-08-17 | Jx日矿日石金属株式会社 | Method for collection of valuable metal from ITO scrap |
| CN101617067B (en) * | 2007-03-27 | 2011-10-26 | Jx日矿日石金属株式会社 | Method of recovering valuable metal from scrap containing conductive oxide |
| CN101113490B (en) * | 2007-09-12 | 2010-05-19 | 昆明理工大学 | Method for leaching indium from indium sulfide concentrate |
| CN101981233B (en) * | 2008-03-06 | 2013-02-13 | Jx日矿日石金属株式会社 | Process for recovery of valuable metals from scrap IZO |
| CN101748433B (en) * | 2008-12-18 | 2011-04-20 | 北京有色金属研究总院 | Purification method of electrolyte in indium electrolysis process |
| CN101525693B (en) * | 2009-04-17 | 2011-02-09 | 深圳市中金岭南有色金属股份有限公司韶关冶炼厂 | Method for vulcanization, reducing oxidation and enrichment of low-grade material containing arsenic, indium and germanium |
| CN101701292B (en) * | 2009-10-20 | 2011-08-03 | 南京中锗科技股份有限公司 | Method for recovering indium and tin from ITO waste targets by utilizing oxidation method |
| CN102199706A (en) * | 2011-05-21 | 2011-09-28 | 南京中锗科技股份有限公司 | Method for comprehensively recovering valuable metal in diode core |
| CN102199706B (en) * | 2011-05-21 | 2013-05-15 | 南京中锗科技股份有限公司 | Method for comprehensively recovering valuable metal in diode core |
| CN103103356A (en) * | 2012-11-09 | 2013-05-15 | 柳州百韧特先进材料有限公司 | Process for recovering crude indium and tin from ITO (indium tin oxide) waste target |
| CN103103356B (en) * | 2012-11-09 | 2014-12-10 | 柳州百韧特先进材料有限公司 | Process for recovering crude indium and tin from ITO (indium tin oxide) waste target |
| CN103046108A (en) * | 2012-12-24 | 2013-04-17 | 上海申和热磁电子有限公司 | Electrolysis process used in ITO film cleaning |
| CN103046108B (en) * | 2012-12-24 | 2017-03-29 | 上海申和热磁电子有限公司 | Application of the electrolysis process in ito film is cleaned |
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| CN104975186A (en) * | 2015-07-30 | 2015-10-14 | 赤峰海镧金属材料科技有限公司 | Comprehensive recycling method for ITO film sensor |
| CN105448822B (en) * | 2015-12-15 | 2018-05-25 | 江西沃格光电股份有限公司 | The method for removing substrate surface ITO |
| CN105448822A (en) * | 2015-12-15 | 2016-03-30 | 江西沃格光电股份有限公司 | Method for removing ITO (tin indium oxide) on surface of base plate |
| CN107513619A (en) * | 2017-08-14 | 2017-12-26 | 中南大学 | A kind of method of recovery indium and tin in waste material from ito glass |
| CN107513619B (en) * | 2017-08-14 | 2019-03-05 | 中南大学 | A method of recovery indium and tin from ito glass waste material |
| CN107604167A (en) * | 2017-09-22 | 2018-01-19 | 京东方科技集团股份有限公司 | Method for treatment of waste material |
| CN108823405A (en) * | 2018-07-09 | 2018-11-16 | 刘罗平 | A kind of dilute immersion liquid method of wet process refining indium |
| CN110018155A (en) * | 2019-03-06 | 2019-07-16 | 江西瑞林稀贵金属科技有限公司 | A kind of method of tin amount in aes determination electronic waste smelting ash |
| CN110498443A (en) * | 2019-08-23 | 2019-11-26 | 云南锡业集团（控股）有限责任公司研发中心 | A method of with ITO give up target recasting ITO powder |
| CN110498443B (en) * | 2019-08-23 | 2021-08-20 | 云南锡业集团（控股）有限责任公司研发中心 | Method for reproducing ITO powder by using ITO waste target |
| CN115650281A (en) * | 2022-10-24 | 2023-01-31 | 广东欧莱高新材料股份有限公司 | Method for recovering indium and gallium from waste target material |
| CN115650281B (en) * | 2022-10-24 | 2024-02-23 | 广东欧莱高新材料股份有限公司 | Method for recycling indium and gallium from waste target material |
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| CN1191380C (en) | 2005-03-02 |
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