CN102199706B - Method for comprehensively recovering valuable metal in diode core - Google Patents

Method for comprehensively recovering valuable metal in diode core Download PDF

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Publication number
CN102199706B
CN102199706B CN2011101321006A CN201110132100A CN102199706B CN 102199706 B CN102199706 B CN 102199706B CN 2011101321006 A CN2011101321006 A CN 2011101321006A CN 201110132100 A CN201110132100 A CN 201110132100A CN 102199706 B CN102199706 B CN 102199706B
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indium
nickel
germanium
solution
tin
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CN2011101321006A
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CN102199706A (en
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黄兴灯
汪洋
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CHINA GERMANIUM CO., LTD.
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NANJING GERMANIUM TECHNOLOGY Co Ltd
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    • YGENERAL 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
    • Y02TECHNOLOGIES OR APPLICATIONS FOR MITIGATION OR ADAPTATION AGAINST CLIMATE CHANGE
    • Y02PCLIMATE CHANGE MITIGATION TECHNOLOGIES IN THE PRODUCTION OR PROCESSING OF GOODS
    • Y02P10/00Technologies related to metal processing
    • Y02P10/20Recycling

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Abstract

The invention discloses a method for comprehensively recovering valuable metal in a diode core. The method comprises the steps of: adding 5mol/L hydrochloric acid into a material, wherein the weight ratio of the material to the hydrochloric acid is 1:3; leaching for 5 hours at 80-90 DEG C; reacting indium-tin alloy with the hydrochloric acid to enable the indium-tin alloy to be completely immersed in to a solution; washing with hot water and drying to obtain a metal mixture of germanium and nickel because germanium and nickel are insoluble to the hydrochloric acid; performing magnetic separation on the metal mixture of the germanium and nickel by using a magnet to obtain monocrystalline germanium slices and nickel rings; and adding caustic soda into a indium-tin-containing solution obtained through hydrochloric acid leaching to neutralize the PH value of the solution to 2, heating the solution to 90 DEG C, and adding hydrogen peroxide to oxidize and hydrolyze tin in the solution into a tin oxide precipitate so as to separate indium and tin. According to the invention, the recovery rates of germanium, nickel, indium and tin are respectively 99%, 96%, 97% and 95%.

Description

A kind of comprehensive method that reclaims of valuable metal in diode core
Technical field
The present invention relates to a kind of comprehensive method that reclaims of valuable metal in diode core.
Background technology
Diode core is rich in 4 kinds of valuable metals of germanium nickel indium tin as a kind of electronics regeneration feed.How valuable metal in this kind material being carried out comprehensively comprehensive alluvial must inquire into.
Summary of the invention
For problems of the prior art, this patent has been realized a kind of method of valuable metal in this kind material being carried out comprehensive comprehensive recovery.Wherein but germanium nickel indium direct production to elemental metals, is sold as the raw material of other smeltery's demands after tin is reclaimed with the enriched substance form.
Technical scheme of the present invention is: a kind of comprehensive method that reclaims of valuable metal in diode core,
Leaching in Hydrochloric Acid separates: 5mol/L hydrochloric acid is added in the diode core material, and material and hydrochloric acid weight ratio are 1:3, and extraction temperature is 80-90 degree centigrade, and extraction time is 5 hours, and indium stannum alloy and hydrochloric acid reaction enter solution fully; And germanium, nickel are hydrochloric acid insoluble substance due to strong to sour resistance to corrosion, obtain the metal mixture of germanium, nickel after the hot wash oven dry;
The recovery of germanium nickel: the metal mixture to germanium, nickel uses magnet to carry out magnetic separation, and nickel belongs to ferromagnetic material, can be picked up by magnet, and germanium can not be picked up by magnet; Obtain single germanium wafer and nickel ring after magnetic separation, single germanium wafer obtains the HpGe ingot through founding, district after melting; The nickel ring is as regenerated nickel;
The recovery of indium tin: the solution that Leaching in Hydrochloric Acid obtains is for containing the indium solution of tin, add in sheet alkali and regulator solution pH value to 2, heating makes solution temperature rise to 90 degrees centigrade, add hydrogen peroxide to make tin oxydrolysis generation stannic hydroxide precipitation in solution, and indium still exists in solution with ionic state, thereby indium is separated with tin; To contain at last solution of indium and use aluminium row displacement to obtain the sponge indium, the sponge indium obtains thick indium through founding; Stannic hydroxide precipitates after hot wash, oven dry as raw material.
Beneficial effect of the present invention: the rate of recovery of four kinds of metals of germanium nickel indium tin: the yield of germanium is 99%; The yield of nickel is 96%; The yield of indium is 97%; The yield of tin is 95%.
Description of drawings
Fig. 1 is the process flow sheet of the inventive method.
Embodiment
The present invention is further detailed explanation below in conjunction with the drawings and specific embodiments.The drawings and specific embodiments do not limit the scope of protection of present invention.
Principle and technique: material concrete form and consist of valuable metal and all exist with the simple substance form, the innermost layer is circular single germanium wafer, and skin is stained with the nickel ring, and the centre is indium alloy (stanniferous).
1, Leaching in Hydrochloric Acid separates: 5mol/L hydrochloric acid is added in material, and material and sour weight ratio are 1:3, and extraction temperature is 80-90 degree centigrade, and extraction time is 5 hours! Indium alloy and hydrochloric acid reaction enter solution fully; And germanium, nickel are hydrochloric acid insoluble substance due to strong to sour resistance to corrosion, obtain the metal mixture of germanium, nickel after the hot wash oven dry.
2, the recovery of germanium, nickel: the metal mixture to germanium, nickel uses magnet to carry out magnetic separation, and nickel belongs to ferromagnetic material, can be picked up by magnet, and germanium can not be picked up by magnet.Obtain single germanium wafer and nickel ring after magnetic separation, single germanium wafer obtains the HpGe ingot and sells after melt in founding, district; The nickel ring is sold as regenerated nickel.
3, the recovery of indium tin: the solution that Leaching in Hydrochloric Acid obtains is for containing the indium solution of tin, add in sheet alkali and regulator solution pH value to 2, heating makes solution temperature rise to 90 degrees centigrade, add hydrogen peroxide to make tin oxydrolysis generation stannic hydroxide precipitation in solution, and indium still exists in solution with ionic state, thereby indium is separated with tin.To contain at last solution of indium and use aluminium row displacement to obtain the sponge indium, the sponge indium obtains thick indium (indium content〉99%) through founding and sells; Stannic hydroxide precipitates after hot wash, oven dry as the raw material sale to the tin smeltery.
4, the rate of recovery of four kinds of metals: the yield of germanium is 99%; The yield of nickel is 96%; The yield of indium is 97%; The yield of tin is 95%.
Although the invention with preferred embodiment openly as above; but embodiment and accompanying drawing are not to limit the invention; anyly be familiar with this skill person; in the spirit and scope that do not break away from the invention; can make various changes or retouch from working as, but same within the protection domain of the invention.Therefore the protection domain of the invention should with the application claim was defined is as the criterion.

Claims (4)

1. the comprehensive method that reclaims of valuable metal in diode core, is characterized in that,
Leaching in Hydrochloric Acid separates: 5mol/L hydrochloric acid is added in the diode core material, and material and hydrochloric acid weight ratio are 1:3, and extraction temperature is 80-90 degree centigrade, and extraction time is 5 hours, gets the metal mixture of indium solution of tin and germanium nickel;
The recovery of germanium nickel: the metal mixture to germanium, nickel uses magnet to carry out magnetic separation, and nickel belongs to ferromagnetic material, can be picked up by magnet, and germanium can not be picked up by magnet;
The recovery of indium tin: the solution that Leaching in Hydrochloric Acid obtains is for containing the indium solution of tin, add in sheet alkali and regulator solution pH value to 2, heating makes solution temperature rise to 90 degrees centigrade, add hydrogen peroxide to make tin oxydrolysis generation stannic hydroxide precipitation in solution, and indium still exists in solution with ionic state, thereby indium is separated with tin; To contain solution of indium and use aluminium row displacement to obtain the sponge indium, the sponge indium obtains thick indium through founding.
2. the comprehensive method that reclaims of valuable metal in diode core according to claim 1, is characterized in that, in described Leaching in Hydrochloric Acid separating step, indium stannum alloy and hydrochloric acid reaction enter solution fully; And germanium, nickel are hydrochloric acid insoluble substance due to strong to sour resistance to corrosion, obtain the metal mixture of germanium, nickel after the hot wash oven dry.
3. the comprehensive method that reclaims of valuable metal in diode core according to claim 1, is characterized in that, in the recycling step of described germanium nickel, obtains single germanium wafer and nickel ring after magnetic separation, and single germanium wafer obtains the HpGe ingot through founding, district after melting; The nickel ring is as regenerated nickel.
4. the comprehensive method that reclaims of valuable metal in diode core according to claim 1, is characterized in that, in the recycling step of described indium tin, will contain solution of indium and use aluminium row displacement to obtain the sponge indium, and the sponge indium obtains thick indium through founding; Stannic hydroxide precipitates after hot wash, oven dry as raw material.
CN2011101321006A 2011-05-21 2011-05-21 Method for comprehensively recovering valuable metal in diode core Expired - Fee Related CN102199706B (en)

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Application Number Priority Date Filing Date Title
CN2011101321006A CN102199706B (en) 2011-05-21 2011-05-21 Method for comprehensively recovering valuable metal in diode core

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CN102199706A CN102199706A (en) 2011-09-28
CN102199706B true CN102199706B (en) 2013-05-15

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Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

Families Citing this family (4)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
CN102560133A (en) * 2012-02-29 2012-07-11 北京矿冶研究总院 Method for extracting gallium and germanium from zinc smelting slag
CN106399722A (en) * 2016-10-17 2017-02-15 扬州宁达贵金属有限公司 Method of recovering tin from liquid crystal containing indium concentrate
CN109468465B (en) * 2018-12-13 2020-09-11 怀化炯诚新材料科技有限公司 Process for recovering metal copper and nickel salt from waste ABS electroplated part
CN114480885B (en) * 2022-02-17 2023-08-22 株洲科能新材料股份有限公司 Method for recycling germanium from germanium-containing waste impurity

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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
CN1532297A (en) * 2003-03-20 2004-09-29 中南大学 Method for wet zinc refining without iron slag
CN101638725A (en) * 2009-08-14 2010-02-03 扬州宁达贵金属有限公司 Method for wet-process enrichment of germanium concentrate from low-germanium coal dust

Patent Citations (3)

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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
CN1532297A (en) * 2003-03-20 2004-09-29 中南大学 Method for wet zinc refining without iron slag
CN101638725A (en) * 2009-08-14 2010-02-03 扬州宁达贵金属有限公司 Method for wet-process enrichment of germanium concentrate from low-germanium coal dust

Non-Patent Citations (1)

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Title
曾林全 编著.第五节 从废铟合金及含铟肥料中回收铟.《电解锡生产》.冶金工业出版社,1981,第207-211页. *

Cited By (1)

* Cited by examiner, † Cited by third party
Publication number Priority date Publication date Assignee Title
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

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