CN1757768A - Separation method of indium tin mixture - Google Patents

Separation method of indium tin mixture Download PDF

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Publication number
CN1757768A
CN1757768A CNA2005100323282A CN200510032328A CN1757768A CN 1757768 A CN1757768 A CN 1757768A CN A2005100323282 A CNA2005100323282 A CN A2005100323282A CN 200510032328 A CN200510032328 A CN 200510032328A CN 1757768 A CN1757768 A CN 1757768A
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tin
indium
mol
powder
zinc
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CN100340679C (en
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陈顺
王全
刘一宁
陈雪云
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Zhuzhou Smelter Group Co Ltd
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Zhuzhou Smelter Group Co Ltd
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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

A process for separating the In-Sn mixture from the rejected material powder includes such steps as immersing the rejected material powder in hydrochloric acid or sulfuric acid, Adding Zn powder to displace the Sn ions to obtain solid tin, solid-liquid separation to obtain tin dregs and solution, adding Sn flakes to the solution to displace In and obtain sponge indium, die press to become blocks, smelting, casting to obtain coarse indium, immersing said tin dregs in concentrated nitric acid for removing impurities, adding code powder for reducing and smelting to obtain coarse tin.

Description

Separation method of indium-tin mixture
Technical Field
The invention relates to a method for separating an indium-tin mixture.
Background
In the lead and zinc smelting production process and the downstream product development process, a large amount of indium-tin mixture is generated, and waste powder is generated in the ITO powder production process; the waste indium tin solders are also generated in the coating sputtering production of users, and the waste materials such as the waste targets, the waste powders, the waste indium tin solders and the like are indium tin mixtures, so that the method has high recycling economic value. For example, the waste target generated In the production process of the ITO target contains 72-75% of In and the balance of tin and oxygen, and about 0.7kg of In0.7kg can be recovered from 1kg of the ITO target. In the past, this waste material was generally recycled by the following process: the method comprises the steps of waste powder sulfuric acid leaching, extraction, back extraction, fresh sponge indium tin removal, sponge indium replacement by zinc sheets, briquetting and casting. The method has long process flow, low direct indium yield and high cost, and the tin is not effectively recovered. How to effectively separate indium and tin from indium-tin-containing materials, achieve the effect of simultaneously recovering indium and tin, and improve the recovery rate of indium is a problem to be further discussed.
Disclosure of Invention
The invention aims to provide a method for separating indium and tin from an indium-tin-containing mixed material, which realizes the effect of simultaneously recovering indium and tin, has the recovery rate of more than 98 percent, and has the advantages of simple process and low cost.
The technical scheme of the invention is as follows: a method for separating indium and tin mixed materials comprises the steps of waste powder acid leaching of indium and tin containing mixtures, zinc replacement, sponge indium briquetting, casting and the like, wherein the zinc replacement step comprises two steps of zinc powder replacement and zinc sheet replacement, namely zinc powder is added into hydrochloric acid or sulfuric acid solution of the indium and tin containing mixtures, tin ions are replaced by solid tin at the temperature of 40-80 ℃ for 1-6 hours, and solid and liquid are separated to obtain tin-removed liquid and tin slag; and replacing the tin-removed liquid by using a zinc sheet, briquetting to obtain sponge indium, casting to obtain crude indium, soaking tin slag in concentrated nitric acid to remove impurities, and then carrying out reduction smelting to obtain crude tin.
As a further improvement of the invention, the leaching step is carried out by using 3-8 mol.L-1Leaching with hydrochloric acid solution.
As to the inventionIn the replacement step, the addition amount (mol) of the zinc powder is1/2X amount of hydrochloric acid or sulfuric acid (mol) +2 XSn4+Or Sn2+Quantity (mol) } × 0.8-facial contour1/2X amount of hydrochloric acid or sulfuric acid (mol) +2 XSn4+Or Sn2+Amount (mol) } × 1.2.
The chemical principle applied by the invention is as follows:
the invention has the beneficial effects that: the method utilizes the principle that metal with low potential can displace metal ions with high potential from solution to make the metal ions become metal, because of phi0In3+/In＞Φ0Sn2+(Sn4+)/Sn＞Φ0Zn2+Zn, so that, after adding zinc powder to a hydrochloric acid or sulfuric acid solution containing indium and tin, part of the zinc powder can directly replace Sn4+、Sn2+So that the zinc powder becomes metallic tin, and part of the zinc powder can replace In3+To make it into metal indium, and the replaced indium replaces Sn4+、Sn2+Making it become metallic tin, ensuring Sn4+、Sn2+Is completely replaced by metallic tin, and the effect of complete tin removal is achieved through solid-liquid separation, thereby realizing the purpose of indium-tin separation. Controlling the mole ratio of the added zinc powder to the mole ratio of tin and indium when the added zinc powder is (mol)1/2X amount of hydrochloric acid or sulfuric acid (mol) +2 XSn4+Or Sn2+Quantity (mol) } × 0.8-facial contour1/2X amount of hydrochloric acid or sulfuric acid (mol) +2 XSn4+Or Sn2+The best effect is obtained when the amount (mol) } × 1.2 is used. The solution after tin removal mainly contains indium and only contains trace tinThe sponge indium can be obtained by replacing with zinc sheets, the grade of crude indium obtained by briquetting and casting is more than or equal to 98 percent of In (wt%), the tin slag can be thoroughly decontaminated by soaking In concentrated nitric acid, and then is reduced and smelted by coke powder, and the grade of crude tin obtained is more than or equal to 95 percent of Sn (wt%). The indium tin recovery rate of the invention respectively reaches 98 percent. The economic benefit of the inventor is remarkable after the implementation, and the annual economic benefit exceeds 100 ten thousand yuan estimated by comprehensively recycling 1 ton of indium.
Drawings
FIG. 1 is a block diagram of the process of the present invention.
Detailed Description
Example 1
The method for treating the ITO waste target powder containing indium and tin comprises the following components In percentage by weight: 75.2%, Sn: 7.55 percent, leaching by adopting hydrochloric acid, wherein the leaching temperature is 80 ℃, the leaching time is 3 hours, and the hydrochloric acid concentration: 5 mol. L-1The components (mol. L) of the leaching solution-1)：In3+：1.15mol·L-1，Sn：0.086mol·L-1The temperature of zinc powder displacement detinning is 60 deg.C, the time is 3hr, and the amount of zinc powder is mol.L-1) Is 0.9 mol. L-1The obtained solution after tin removal (mol. L)-1): the Sn content: 0.0085 mol. L-1The tin slag comprises the following components in percentage by weight: 72.8%, the balance being oxygen
And (3) replacing the solution after tin removal by using a zinc sheet to obtain sponge indium, briquetting, casting into crude indium, soaking and washing impurities in tin slag by using concentrated nitric acid, and reducing and smelting by using coke powder to obtain crude tin. Crude indium content (wt%) was produced: in: 98.6 percent.
Example 2
The invention is adopted to treat ITO waste target powder containing indium and tin according to the embodiment 1, and the components (wt%) of the ITO waste target powder are In: 75.2%, Sn: 7.55%, except that: leaching by adopting sulfuric acid, wherein the leaching temperature is 40 ℃, the leaching time is 6hr, and the sulfuric acid concentration is as follows: 2.5 mol. L-1The components (mol. L) of the leaching solution-1)：In3+：1.05mol·L-1，Sn：0.075mol·L-1The temperature for removing tin by zinc powder replacement is 50 ℃, the time is 1hr, and the amount of zinc powder is (mol. L)-1) Is 0.9 mol. L-1The obtained tin-removed liquid(mol·L-1): the Sn content: 0.0060 mol. L-1The tin slag comprises the following components in percentage by weight: 70.1 percent and the balance of oxygen, and crude indium components (wt percent) are produced: in: 98.6 percent
Example 3
The invention is adopted to treat ITO waste powder containing indium and tin according to the embodiment 1, and the components (wt%) of the ITO waste powder are In: 75.2%, Sn: 7.55%, except that: leaching by adopting sulfuric acid, wherein the leaching temperature is 80 ℃, the leaching time is 3hr, and the sulfuric acid concentration is as follows: 2.5 mol. L-1The components (mol. L) of the leaching solution-1)：In3+：1.08mol·L-1，Sn：0.065mol·L-1The temperature of zinc powder replacement detinning is 40 ℃, the time is 6hr, and the amount of zinc powder is (mol. L)-1) Is 0.9 mol. L-1The obtained solution after tin removal (mol. L)-1): the Sn content: 0.0060 mol. L-1The tin slag comprises the following components in percentage by weight: 70.1 percent and the balance of oxygen, and crude indium components (wt percent) are produced: in: 98.6 percent
Example 4
The invention is adopted to treat ITO waste powder containing indium and tin according to the embodiment 1, and the components (wt%) of the ITO waste powder are In: 75.2%, Sn: 7.55%, except that: leaching by adopting sulfuric acid, wherein the leaching temperature is 80 ℃, the leaching time is 3hr, and the sulfuric acid concentration is as follows: 2.5 mol. L-1The components (mol. L) of the leaching solution-1)：In3+：1.15mol·L-1，Sn：0.077mol·L-1The temperature for removing tin by zinc powder replacement is 80 ℃, the time is 4hr, and the amount of zinc powder is (mol. L)-1) Is 0.95 mol. L-1The obtained solution after tin removal (mol. L)-1): the Sn content: 0.0065 mol. L-1The tin slag comprises the following components in percentage by weight: 70.31 percent, and the balance of oxygen, yielding a crude indium composition (wt%): in: 98.8 percent
Example 5
The waste indium tin solder containing indium tin is treated by adopting the method of the invention according to the embodiment 1, and the components (wt%) of the waste indium tin solder are In: 75.2%, Sn: 7.55%, except that: leaching by adopting sulfuric acid at the leaching temperature of 80 ℃,leaching time 4hr, sulfuric acid concentration: 2.6 mol. L-1The components (mol. L) of the leaching solution-1)：In3+：1.08mol·L-1，Sn：0.078mol·L-1The temperature of zinc powder displacement detinning is 60 deg.C, the time is 1hr, and the amount of zinc powder is mol.L-1) Is 1.1 mol. L-1The obtained solution after tin removal (mol. L)-1): the Sn content: 0.0058 mol. L-1The tin slag comprises the following components in percentage by weight: 76.1% and the remainder oxygen, yielding a crude indium composition (wt%): in: 98.7 percent.
Example 6
The waste indium tin solder containing indium tin is treated by adopting the method of the invention according to the embodiment 1, and the components (wt%) of the waste indium tin solder are In: 75.2%, Sn: 7.55%, except that: leaching by adopting sulfuric acid, wherein the leaching temperature is 60 ℃, the leaching time is 5hr, and the sulfuric acid concentration is as follows: 2.8 mol. L-1The components (mol. L) of the leaching solution-1)：In3+：1.15mol·L-1，Sn：0.055mol·L-1The temperature of zinc powder displacement detinning is 60 deg.C, the time is 2hr, and the amount of zinc powder is mol.L-1) Is 1.2 mol. L-1The obtained solution after tin removal (mol. L)-1): the Sn content: 0.0062 mol. L-1The tin slag comprises the following components in percentage by weight: 75.1% and the remainder oxygen, yielding a crude indium composition (wt%): in: 98.2 percent.
The present invention includes, but is not limited to, the above embodiments, and is within the scope of the present invention as long as the zinc powder displacement tin removal and the zinc sheet displacement tin removal methods are used.

Claims (5)

1. A method for separating indium-tin mixture comprises the steps of waste powder acid leaching of indium-tin-containing mixture, zinc replacement, sponge indium briquetting, casting and the like, and is characterized in that: the zinc replacement step comprises two steps of zinc powder replacement and zinc sheet replacement, namely, zinc powder is added into hydrochloric acid or sulfuric acid solution containing an indium-tin mixture, tin ions are replaced by solid tin, and solid and liquid are separated to obtain tin-removed liquid and tin slag; and replacing the tin-removed solution with a zinc sheet to obtain sponge indium.
2. The method of claim 1, further comprising the steps of: the temperature of zinc powder replacement is 40-80 ℃, and the time is 1-6 hours.
3. The method of claim 1, further comprising the steps of: and soaking the tin slag in concentrated nitric acid to remove impurities, and then reducing and smelting the tin slag by using coke powder to obtain crude tin.
4. The method of claim 1, further comprising the steps of: the powder acid leaching of the indium-tin-containing mixture is carried out by using 3-8 mol.L-1Leaching with hydrochloric acid solution.
5. The method of claim 1, further comprising the steps of: the adding amount (mol) of the zinc powder in the replacement step is { (la) hydrochloric acid or sulfuric acid amount (mol) +2 xSn4+Or Sn2+Amount (mol) } × 0.8- { (la × hydrochloric acid or sulfuric acid amount (mol) +2 × Sn4+Or Sn2+Amount (mol) } × 1.2.
CNB2005100323282A 2005-11-01 2005-11-01 Separation method of indium tin mixture Active CN100340679C (en)

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Cited By (11)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN100443604C (en) * 2006-11-20 2008-12-17 深圳市中金岭南有色金属股份有限公司韶关冶炼厂 Extraction and separation technology for reclaiming main impurity in indium in hydrochloric acid system
CN101186976B (en) * 2006-09-28 2010-11-24 同和金属矿业有限公司 Method for withdrawing indium from indium-containing material
CN102912155A (en) * 2012-09-20 2013-02-06 福建省固体废物处置有限公司 Recovery processing process of stanniferous electrofacing sludge
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
CN104313327A (en) * 2014-10-17 2015-01-28 金川集团股份有限公司 Method for eliminating cadmium in nickel sulfate solution
CN104674012A (en) * 2015-02-16 2015-06-03 广西德邦科技有限公司 Method of separating indium from tin slag
CN105483385A (en) * 2015-12-09 2016-04-13 中国矿业大学 Method for recycling tin from tin alkali solution
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
CN108330297A (en) * 2018-03-26 2018-07-27 赣州市赤鼎再生资源有限公司 A kind of method that abandoned mine material recycles
CN112095010A (en) * 2020-08-28 2020-12-18 昆明理工大学 Method for separating and recovering tin and zinc from tin-zinc-containing gold spraying powder
CN112708763A (en) * 2020-12-15 2021-04-27 先导薄膜材料（广东）有限公司 Method for recovering valuable metal from ITO waste target

Family Cites Families (2)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN1191380C (en) * 2002-11-07 2005-03-02 长沙矿冶研究院 Method for extracting refined indium from indium tin oxide waste material
JP2005200735A (en) * 2004-01-19 2005-07-28 National Institute Of Advanced Industrial & Technology Method of producing indium-containing aqueous solution

Cited By (12)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN101186976B (en) * 2006-09-28 2010-11-24 同和金属矿业有限公司 Method for withdrawing indium from indium-containing material
CN100443604C (en) * 2006-11-20 2008-12-17 深圳市中金岭南有色金属股份有限公司韶关冶炼厂 Extraction and separation technology for reclaiming main impurity in indium in hydrochloric acid system
CN102912155A (en) * 2012-09-20 2013-02-06 福建省固体废物处置有限公司 Recovery processing process of stanniferous electrofacing sludge
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
CN104313327A (en) * 2014-10-17 2015-01-28 金川集团股份有限公司 Method for eliminating cadmium in nickel sulfate solution
CN104674012A (en) * 2015-02-16 2015-06-03 广西德邦科技有限公司 Method of separating indium from tin slag
CN105483385A (en) * 2015-12-09 2016-04-13 中国矿业大学 Method for recycling tin from tin alkali solution
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
CN108330297A (en) * 2018-03-26 2018-07-27 赣州市赤鼎再生资源有限公司 A kind of method that abandoned mine material recycles
CN112095010A (en) * 2020-08-28 2020-12-18 昆明理工大学 Method for separating and recovering tin and zinc from tin-zinc-containing gold spraying powder
CN112708763A (en) * 2020-12-15 2021-04-27 先导薄膜材料（广东）有限公司 Method for recovering valuable metal from ITO waste target

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