CN100340679C - Separation method of indium tin mixture - Google Patents
Separation method of indium tin mixture Download PDFInfo
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- CN100340679C CN100340679C CNB2005100323282A CN200510032328A CN100340679C CN 100340679 C CN100340679 C CN 100340679C CN B2005100323282 A CNB2005100323282 A CN B2005100323282A CN 200510032328 A CN200510032328 A CN 200510032328A CN 100340679 C CN100340679 C CN 100340679C
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- indium
- zinc
- tin
- indium tin
- separation method
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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
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Abstract
The present invention relates to a separation method for indium-tin mixtures, which comprises the steps of leaching waste material powder containing indium-tin mixtures in acid, carrying out metathesis by zinc, briquetting by sponge indium, carrying out casting and molding, etc., wherein the zinc metathesis steps comprise a zinc powder metathesis step and a zinc sheet metathesis step, namely that the zinc powder is added to hydrochloric acid solution or sulfuric acid solution containing the indium-tin mixtures, and tin ions are changed into solid tin at a temperature of 40 to 80 DEG C for 1 to 6 hours, so that solids and liquid are separated to obtain detinned solution and tin dross; then the detinned solution is permuted by zinc sheets to obtain sponge indium briquetted and cast into crude indium. The tin dross is soaked by concentrated nitric acid for edulcoration and is then reduced and smelted by coke powder into crude tin. Compared with the prior art, the present invention directly carries out permutation by the zinc without extract step so as to shorten the process flow and reduce the cost. The recovery rates of the indium and the tin in the present invention respectively reach 98%, and the separation method creates remarkable economic benefit after an inventor implements the separation method. The annual economic benefit exceeds one million yuan estimated according to the additional comprehensive recovery of one ton of indium per year.
Description
Technical field
The present invention relates to a kind of separation method of indium tin mixture.
Background technology
Smelt in production process and the derived product performance history at plumbous, zinc, all have a large amount of indium tin mixtures and produce, in the ito powder production process, have useless powder to produce; The user also has useless indium tinsolder and produces in the plated film sputter is produced, waste materials such as these useless targets, useless powder, useless indium tinsolder all are indium tin mixtures, have very high recovery economic worth.As containing In72～75% in the useless target that is produced in the ITO target production process, all the other are tin and oxygen, about the recyclable In0.7kg of 1kgITO target.In the past, this waste material generally reclaims technical process and is: waste material powder sulfuric acid leaches---extracts---back extraction---fresh sponge indium detin---zinc metal sheet displacement sponge indium---group of pressure---casting mold.This method process flow is long, and the indium direct yield is low, cost is high, and tin not effectively reclaim.How separating indium and tin effectively from contain indium tin material, reach the effect that reclaims indium and tin simultaneously, and improve the rate of recovery of indium, is the further problem of discussion that remains.
Summary of the invention
The object of the present invention is to provide a kind of method of separating indium and tin from contain the indium tin mixture material, realize reclaiming simultaneously the effect of indium and tin, the rate of recovery reaches more than 98%, and it is simple to have technology, the advantage that cost is low.
Technical scheme of the present invention is: a kind of separation method of indium tin mixture material, comprise the waste material powder that contains indium tin mixture with hydrochloric acid or sulfuric acid leach, zinc displacement, sponge indium press group, casting mold step, described zinc displacement step comprises zinc dust precipitation and zinc metal sheet is replaced two steps, promptly earlier in hydrochloric acid that contains indium tin mixture or sulphuric acid soln, be added into zinc powder, tin ion is replaced into solid tin, and temperature is 40～80 ℃, and the time is 1～6 hour, solid-liquid is separated, obtain liquid and scruff behind the detin; Liquid behind the detin is replaced with zinc metal sheet again, obtain the sponge indium after the group of pressure, founding becomes thick indium, and described scruff carries out retailoring again and gets thick tin after soaking removal of impurities with concentrated nitric acid.
As to further improvement of the present invention, described leaching step is with 3～8molL
-1Hydrochloric acid soln leaches.
As to further improvement of the present invention, in the described displacement step add-on of zinc powder (mol) be
1/
2* hydrochloric acid or sulfuric acid amount (mol)+2 * Sn
4+Or Sn
2+Amount (mol) } * 0.8～{ 1/2 * hydrochloric acid or sulfuric acid amount (mol)+2 * Sn
4+Or Sn
2+Amount (mol) } * 1.2.
The applied principles of chemistry of the present invention are:
Sn
2++Zn＝Sn↓+Zn
2+
Sn
4++2Zn＝Sn↓+2Zn
2+
2In
3++3Zn＝2In↓+3Zn
2+
3Sn
2++2In＝3Sn↓+2In
3+
3Sn
4++4In＝3Sn↓+4In
3+
Beneficial effect of the present invention is: this method is utilized the low metal of current potential can displace the high metal ion of current potential from solution and is made its principle that becomes metal, because
0In
3+/ In＞
0Sn
2+(Sn
4+)/Sn＞
0Zn
2+/ Zn, therefore, in hydrochloric acid that contains indium tin or sulphuric acid soln, be added into zinc powder after, but part zinc powder direct replacement Sn wherein
4+, Sn
2+And make it become metallic tin, the replaceable In of part zinc powder
3+Make it become indium metal, the indium that is displaced is replaced Sn again
4+, Sn
2+Make it become metallic tin, guaranteed Sn
4+, Sn
2+All be replaced into metallic tin, reached the effect of thorough detin, thereby realized the isolating purpose of indium tin by solid-liquid separation.By the mol ratio of the control add-on mole of zinc powder and tin, indium, when the add-on (mol) of zinc powder is { 1/2 * hydrochloric acid or sulfuric acid amount (mol)+2 * Sn
4+Or Sn
2+Amount (mol) } * 0.8～{ 1/2 * hydrochloric acid or sulfuric acid amount (mol)+2 * Sn
4+Or Sn
2+Amount (mol) } * 1.2 o'clock, best results.Mainly contain indium behind the detin in the liquid, only containing trace tin, can obtain the sponge indium with the zinc metal sheet displacement, is In (wt%) 〉=98% through the thick indium grade of the group's of pressure casting mold gained, scruff soaks thoroughly removal of impurities with concentrated nitric acid, use coke powder retailoring again, the thick tin grade of gained is Sn (wt%) 〉=95%, and the present invention compared with prior art, need not to adopt extraction step, directly with the zinc displacement, technical process is shortened, and cost reduces relatively.The indium tin rate of recovery of the present invention reaches 98% respectively.
Description of drawings
Fig. 1 is a technical process square frame of the present invention.
Embodiment
Embodiment 1
The useless target powder of ITO that adopts method processing of the present invention to contain indium tin, its composition (wt%) is In:75.2%, Sn:7.55% adopts hydrochloric acid to leach 80 ℃ of extraction temperatures, extraction time 3hr, concentration of hydrochloric acid: 5molL
-1, leach liquor composition (molL
-1): In
3+: 1.15molL
-1, Sn:0.086molL
-1, the temperature of zinc dust precipitation detin is 60 ℃, the time is 3hr, zinc powder consumption (molL
-1) be 0.9molL
-1, liquid (molL behind the gained detin
-1): in contain Sn:0.0085molL
-1, scruff composition (wt%): 72.8%, all the other are oxygen.
Liquid is replaced with zinc metal sheet behind the detin, obtains the sponge indium, becomes thick indium through pressing group's back founding, and scruff soaks to wash with concentrated nitric acid and carries out retailoring with coke powder after assorted and get thick tin.The thick indium composition of output (wt%): In:98.6%.
Embodiment 2
Adopt the present invention to handle the useless target powder of the ITO that contains indium tin by embodiment 1, its composition (wt%) is In:75.2%, Sn:7.55%, and difference is: adopt sulfuric acid to leach 40 ℃ of extraction temperatures, extraction time 6hr, sulfuric acid concentration: 2.5molL
-1, leach liquor composition (molL
-1): In
3+: 1.05molL
-1, Sn:0.075molL
-1, the temperature of zinc dust precipitation detin is 50 ℃, the time is 1hr, zinc powder consumption (molL
-1) be 0.9molL
-1, liquid (molL behind the gained detin
-1): in contain Sn:0.0060molL
-1, scruff composition (wt%): 70.1%, all the other are oxygen, the thick indium composition of output (wt%): In:98.6%.
Embodiment 3
Adopt the present invention to handle the useless powder of the ITO that contains indium tin by embodiment 1, its composition (wt%) is In:75.2%, Sn:7.55%, and difference is: adopt sulfuric acid to leach 80 ℃ of extraction temperatures, extraction time 3hr, sulfuric acid concentration: 2.5molL
-1, leach liquor composition (molL
-1): In
3+: 1.08molL
-1, Sn:0.065molL
-1, the temperature of zinc dust precipitation detin is 40 ℃, the time is 6hr, zinc powder consumption (molL
-1) be 0.9molL
-1, liquid (molL behind the gained detin
-1): in contain Sn:0.0060molL
-1, scruff composition (wt%): 70.1%, all the other are oxygen, the thick indium composition of output (wt%): In:98.6%.
Embodiment 4
Adopt the present invention to handle the useless powder of the ITO that contains indium tin by embodiment 1, its composition (wt%) is In:75.2%, Sn:7.55%, and difference is: adopt sulfuric acid to leach 80 ℃ of extraction temperatures, extraction time 3hr, sulfuric acid concentration: 2.5molL
-1, leach liquor composition (molL
-1): In
3+: 1.15molL
-1, Sn:0.077molL
-1, the temperature of zinc dust precipitation detin is 80 ℃, the time is 4hr, zinc powder consumption (molL
-1) be 0.95molL
-1, liquid (molL behind the gained detin
-1): in contain Sn:0.0065molL
-1, scruff composition (wt%): 70.31%, all the other are oxygen, the thick indium composition of output (wt%): In:98.8%.
Embodiment 5
Adopt the present invention to handle the useless indium tinsolder that contains indium tin by embodiment 1, its composition (wt%) is In:75.2%, Sn:7.55%, and difference is: adopt sulfuric acid to leach 80 ℃ of extraction temperatures, extraction time 4hr, sulfuric acid concentration: 2.6molL
-1, leach liquor composition (molL
-1): In
3+: 1.08molL
-1, Sn:0.078molL
-1, the temperature of zinc dust precipitation detin is 60 ℃, the time is 1hr, zinc powder consumption (molL
-1) be 1.1molL
-1, liquid (molL behind the gained detin
-1): in contain Sn:0.0058molL
-1, scruff composition (wt%): 76.1%, all the other are oxygen, the thick indium composition of output (wt%): In:98.7%.
Embodiment 6
Adopt the present invention to handle the useless indium tinsolder that contains indium tin by embodiment 1, its composition (wt%) is In:75.2%, Sn:7.55%, and difference is: adopt sulfuric acid to leach 60 ℃ of extraction temperatures, extraction time 5hr, sulfuric acid concentration: 2.8molL
-1, leach liquor composition (molL
-1): In
3+: 1.15molL
-1, Sn:0.055molL
-1, the temperature of zinc dust precipitation detin is 60 ℃, the time is 2hr, zinc powder consumption (molL
-1) be 1.2molL
-1, liquid (molL behind the gained detin
-1): in contain Sn:0.0062molL
-1, scruff composition (wt%): 75.1%, all the other are oxygen, the thick indium composition of output (wt%): In:98.2%.
The present invention is including but not limited to above-mentioned embodiment, as long as adopted the method for zinc dust precipitation detin and zinc metal sheet displacement detin, promptly in protection scope of the present invention.
Claims (5)
1, a kind of separation method of indium tin mixture, comprise the waste material powder that contains indium tin mixture with hydrochloric acid or sulfuric acid leach, zinc displacement, sponge indium press group, casting mold step, it is characterized in that: described zinc displacement step comprises zinc dust precipitation and zinc metal sheet is replaced two steps, promptly earlier in hydrochloric acid that contains indium tin mixture or sulphuric acid soln, be added into zinc powder, tin ion is replaced into solid tin, solid-liquid is separated, obtain liquid and scruff behind the detin; Again liquid behind the detin is replaced with zinc metal sheet, obtain the sponge indium.
2, the separation method of a kind of indium tin mixture according to claim 1 is characterized in that: the temperature of described zinc dust precipitation is 40～80 ℃, and the time is 1～6 hour.
3, the separation method of a kind of indium tin mixture according to claim 1 is characterized in that: described scruff soaks with concentrated nitric acid and carries out retailoring again with coke powder after the removal of impurities and get thick tin.
4, the separation method of a kind of indium tin mixture according to claim 1 is characterized in that: it is with 3～8molL that the described powder acidleach that contains indium tin mixture goes out
-1Hydrochloric acid soln leaches.
5, the separation method of a kind of indium tin mixture according to claim 1 is characterized in that: the add-on of zinc powder (mol) is { * hydrochloric acid or sulfuric acid amount (mol)+2 * Sn in the described displacement step
4+Or Sn
2+Amount (mol) } * 0.8～{ * hydrochloric acid or sulfuric acid amount (mol)+2 * Sn
4+Or Sn
2+Amount (mol) } * 1.2.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100323282A CN100340679C (en) | 2005-11-01 | 2005-11-01 | Separation method of indium tin mixture |
Applications Claiming Priority (1)
| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CNB2005100323282A CN100340679C (en) | 2005-11-01 | 2005-11-01 | Separation method of indium tin mixture |
Publications (2)
| Publication Number | Publication Date |
|---|---|
| CN1757768A CN1757768A (en) | 2006-04-12 |
| CN100340679C true CN100340679C (en) | 2007-10-03 |
Family
ID=36703334
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| Application Number | Title | Priority Date | Filing Date |
|---|---|---|---|
| CNB2005100323282A Active CN100340679C (en) | 2005-11-01 | 2005-11-01 | Separation method of indium tin mixture |
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Families Citing this family (11)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| JP4999058B2 (en) * | 2006-09-28 | 2012-08-15 | Ｄｏｗａメタルマイン株式会社 | Method for recovering 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 |
| 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 |
| CN105483385B (en) * | 2015-12-09 | 2018-06-05 | 中国矿业大学 | A kind of method that tin is recycled in the aqueous slkali from tin |
| 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 |
| CN112708763B (en) * | 2020-12-15 | 2022-09-06 | 先导薄膜材料（广东）有限公司 | Method for recovering valuable metal from ITO waste target |
Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1420184A (en) * | 2002-11-07 | 2003-05-28 | 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 |
-
2005
- 2005-11-01 CN CNB2005100323282A patent/CN100340679C/en active Active
Patent Citations (2)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN1420184A (en) * | 2002-11-07 | 2003-05-28 | 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 |
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| Publication number | Publication date |
|---|---|
| CN1757768A (en) | 2006-04-12 |
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