CN104212983A - Method for recovering indium from waste LCDs - Google Patents
Method for recovering indium from waste LCDs Download PDFInfo
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- CN104212983A CN104212983A CN201410478633.3A CN201410478633A CN104212983A CN 104212983 A CN104212983 A CN 104212983A CN 201410478633 A CN201410478633 A CN 201410478633A CN 104212983 A CN104212983 A CN 104212983A
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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
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- 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 invention discloses a method for recovering indium from waste LCDs. The method comprises the following steps: waste LCD panels containing indium tin oxide are dismounted, crushed and then dissolved in an acid solution, and insoluble substances are removed by filtration; the filtrate obtained in the first step is adjusted to an appropriate pH value and then stands for precipitation, and precipitates are removed by filtration; trivalent indium ions in the filtrate obtained in the second step are selectively adsorbed by aminophosphonic acid chelate resin, and then desorbed by a hydrochloric acid solution to obtain a solution containing trivalent indium ions. The method is simple to operate and friendly to the environment, has a good indium separation effect and satisfies mass production.
Description
Technical field
The present invention relates to a kind of method of recovery indium from waste liquid crystal display, belong to the technical field of recycling of WEEE indium.
Background technology
Indium is a kind of rare metal, and hardness is lower than lead metal, and plasticity-is strong, have ductility, can be pressed into very thin tinsel; The alloy that the indium of 24% and the gallium of 76% are formed is at room temperature liquid; Indium is one of not retrievable key raw material of electronics, telecommunications, photovoltaic; The indium of 70% is for the manufacture of liquid crystal display product.Indium metal is mainly used in various Novel LCD and the aspects such as touch screen, glass for building purposes such as notebook computer, TV, mobile phone; ITO indium target (accounting for 70% of indium rate of utilization) consumption as transparent electrode coating strives the length that increases severely, and indium demand is just increased progressively with the rate of increase of average annual more than 30%.Indium is as a heavy metal species, comparatively large to the harm of human body, and has harm to environment, can cause dirty combustion to water body.Indium content in discarded liquid-crystal display is high, threatens to the health of environment and the mankind, simultaneously as the metal that a kind of high price is rare, and the focus making the recovery for waste liquid crystal display become investigators to pay close attention to.
The major technique that current indium metal reclaims has: 1, extraction process, uses hot acid or organic solvent to leach removing interfering ion, and then obtains comparatively pure indium ion system.This method operation is too complicated, wayward in the operating process of reality.2, reduction method, under the high temperature conditions, utilizes the reductibility of the material such as hydrogen or gac, is directly reduced by indium ion.What the reduction of this method obtained is alloy, instead of simple substance indium, after obtaining alloy, also will extract further, could realize the recovery of indium like this.Meanwhile, after forming alloy, it is separated comparatively difficulty, is unfavorable for obtaining the higher product of purity.3, membrane separation process, utilizes the feature of the selective penetrated property of artificial membrane to realize separation.The selective absorbing rate of this method to indium is lower, is difficult to realize industrialization.
Therefore, develop separating-purifying operation simple, high and method the has environmental friendliness feature indium recovery technology of products obtained therefrom purity is extremely necessary.
Summary of the invention
For the defect that existing indium metal recovery process exists, the object of the invention is to be to provide a kind of simple to operate, environmental friendliness, the method for high efficiente callback indium from waste liquid crystal display.
The invention provides a kind of method of recovery indium from waste liquid crystal display, the method is by after the waste liquid crystal display panel dismounting containing indium tin oxide, pulverizing, dissolves, filter I and isolate insolubles with acid solution; Filtering I gained filtrate regulates pH to be after 1.5 ~ 2.5, staticly settles, refilters II and isolate precipitation; Filter the filtrate of II gained by alpha-amino phosphonate base resin selective adsorption trivalent indium ion wherein, the alpha-amino phosphonate base resin concentration of having adsorbed trivalent indium ion is that 2 ~ 4mol/L hydrochloric acid soln carries out desorption, obtains the solution containing trivalent indium ion.
The method of recovery indium from waste liquid crystal display of the present invention also comprises following preferred version:
PH is regulated to be 1.8 ~ 2.0 filtration I gained filtrate in preferred scheme; Preferable ph is more conducive to other precipitation by metallic ion and is conducive to alpha-amino phosphonate base resin to the absorption of trivalent indium ion.
The temperature that in preferred scheme, acid solution dissolves is 30 ~ 80 DEG C, and the time is 40 ~ 60min; Most preferred temperature is 40 ~ 60 DEG C; Preferred dissolution conditions is more conducive to the stripping of trivalent indium ion.
In preferred scheme acid solution be mass percent concentration 10 ~ 30% hydrochloric acid, sulfuric acid or nitric acid.
In preferred scheme alpha-amino phosphonate base resin be with styrene-divinylbenzene copolymerization for matrix, be grafted with the porous resin of alpha-amino phosphonate base.Described alpha-amino phosphonate base resin can buy the D840 resin of the foundation Science and Technology Ltd. that to win honour in Beijing or the D405 resin of Anhui Province tree Chemical Co., Ltd..
Beneficial effect of the present invention: 1, high to the indium metal separation recovery efficiencies abandoned in liquid-crystal display, by selecting suitable pH value and selecting suitable resin, to the absorption rate of recovery of indium ion up to more than 90%; 2, simple to operate, be convenient to control, equipment requirements is low, meets industrialization continuous seepage; 3, do not need to adopt organic solvent completely, only need a small amount of acid to leach, acid is by alkali neutralizing treatment, environmentally friendly.
Embodiment
Following examples are intended to further illustrate content of the present invention, instead of limit the scope of the invention.Embodiment 1
After the waste liquid crystal display panel dismounting containing indium tin oxide, pulverizing, with mass percent concentration be 15% hydrochloric acid soln at 60 DEG C, carry out dissolving 40min after, filter to isolate insolubles, filtering gained filtrate regulates pH to be after 1.8, leave standstill without Precipitation, filtering separation, the filtrate obtained adopts D405 resin to carry out selective adsorption to the trivalent indium ion in filtrate, the D405 resin concentration of having adsorbed trivalent indium ion is that 2mol/L hydrochloric acid soln carries out desorption, obtains the solution containing trivalent indium ion.Indium solubility rate is not less than 99%, and by measuring the change of indium content in dissolution fluid and recovery solution, the indium ion rate of recovery is 92%.
Embodiment 2
After the waste liquid crystal display panel dismounting containing indium tin oxide, pulverizing, with mass percent concentration be 30% hydrochloric acid soln at 40 DEG C, carry out dissolving 60min after, filter to isolate insolubles, filtering gained filtrate regulates pH to be after 2.0, leave standstill until without Precipitation, filtering separation, the filtrate obtained adopts D840 resin to carry out selective adsorption to the trivalent indium ion in filtrate, the D840 resin concentration of having adsorbed trivalent indium ion is that 4mol/L hydrochloric acid soln carries out desorption, obtains the solution containing trivalent indium ion.Indium solubility rate is not less than 99%, and by measuring the change of indium content in dissolution fluid and recovery solution, the indium ion rate of recovery is 93%.
From embodiment 1 and 2, by controlling the adjustment of the pH value of dissolution fluid and adopting suitable resin, the indium in waste liquid crystal display panel can be reclaimed effective stripping and fractionation by adsorption.
Comparative example 1
After the waste liquid crystal display panel dismounting containing indium tin oxide, pulverizing, with mass percent concentration be 30% hydrochloric acid soln at 30 DEG C, carry out dissolving 60min after, filter to isolate insolubles, filtering gained filtrate regulates pH to be after 3.0, leave standstill until without Precipitation, filtering separation, the filtrate obtained adopts D840 resin to carry out selective adsorption to the trivalent indium ion in filtrate, the D840 resin concentration of having adsorbed trivalent indium ion is that 3mol/L hydrochloric acid soln carries out desorption, obtains the solution containing trivalent indium ion.Indium solubility rate is not higher than 84%, and by measuring the change of indium content in dissolution fluid and recovery solution, the indium ion rate of recovery is 78%.It is too high that this comparative example illustrates that dissolution fluid pH value regulates, and indium ion loses with other metal complex precipitation, and pH is too high is simultaneously not suitable for the adsorption selection of resin to trivalent indium ion.
Comparative example 2
After the waste liquid crystal display panel dismounting containing indium tin oxide, pulverizing, with mass percent concentration be 30% hydrochloric acid soln at 30 DEG C, carry out dissolving 60min after, filter to isolate insolubles, filtering gained filtrate regulates pH to be after 0.5, leave standstill, almost without Precipitation, filtrate adopts D840 resin to carry out selective adsorption to the trivalent indium ion in filtrate, the D840 resin concentration of having adsorbed trivalent indium ion is that 3mol/L hydrochloric acid soln carries out desorption, obtains the solution containing trivalent indium ion.Indium solubility rate is not less than 99%, and by measuring the change of indium content in dissolution fluid and recovery solution, the indium ion rate of recovery is 48%.This comparative example can find out, although pH is too low be conducive to negatively charged ion stripping, is unfavorable for the separation of other foreign metal ion of trivalent indium ion, and under this pH condition, D840 resin is weak to trivalent anion adsorptive power.
Claims (5)
1. the method for recovery indium from waste liquid crystal display, is characterized in that, after the waste liquid crystal display panel dismounting containing indium tin oxide, pulverizing, dissolves, filter I and isolate insolubles with acid solution; Filtering I gained filtrate regulates pH to be after 1.5 ~ 2.5, staticly settles, refilters II and isolate precipitation; Filter the filtrate of II gained by alpha-amino phosphonate base resin selective adsorption trivalent indium ion wherein, the alpha-amino phosphonate base resin concentration of having adsorbed trivalent indium ion is that 2 ~ 4mol/L hydrochloric acid soln carries out desorption, obtains the solution containing trivalent indium ion.
2. method according to claim 1, is characterized in that, filters I gained filtrate and regulates pH to be 1.8 ~ 2.0.
3. method according to claim 1, is characterized in that, the temperature that acid solution dissolves is 30 ~ 80 DEG C, and the time is 40 ~ 60min.
4. method according to claim 1, is characterized in that, described acid solution be mass percent concentration 10 ~ 30% hydrochloric acid, sulfuric acid or nitric acid.
5. method according to claim 1, is characterized in that, described alpha-amino phosphonate base resin be with styrene-divinylbenzene copolymerization for matrix, be grafted with the porous resin of alpha-amino phosphonate base.
Priority Applications (1)
| Application Number | Priority Date | Filing Date | Title |
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| CN201410478633.3A CN104212983A (en) | 2014-09-18 | 2014-09-18 | Method for recovering indium from waste LCDs |
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| CN201410478633.3A CN104212983A (en) | 2014-09-18 | 2014-09-18 | Method for recovering indium from waste LCDs |
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| CN201410478633.3A Pending CN104212983A (en) | 2014-09-18 | 2014-09-18 | Method for recovering indium from waste LCDs |
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Cited By (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104722563A (en) * | 2015-03-18 | 2015-06-24 | 合肥鑫晟光电科技有限公司 | Method for recycling indium on panel |
| CN107475523A (en) * | 2017-09-02 | 2017-12-15 | 河北工程大学 | A kind of method of the recovery indium from flyash |
| 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 |
| CN108893608A (en) * | 2018-05-30 | 2018-11-27 | 苏州精美科光电材料有限公司 | A kind of refinement method improving indium recovery |
| TWI803261B (en) * | 2022-03-28 | 2023-05-21 | 虹京金屬股份有限公司 | Method for recycling indium |
Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101014407A (en) * | 2004-07-09 | 2007-08-08 | 株式会社阿库泰克 | Indium adsorbing agent and method for separating indium |
-
2014
- 2014-09-18 CN CN201410478633.3A patent/CN104212983A/en active Pending
Patent Citations (1)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN101014407A (en) * | 2004-07-09 | 2007-08-08 | 株式会社阿库泰克 | Indium adsorbing agent and method for separating indium |
Non-Patent Citations (4)
| Title |
|---|
| XIONG CHUNHUA: "Sorption behavior and mechanism of inditnn(Ⅲ)onto aminomethylenephosphonic acid resin", 《JOURNAL OF WUHAN UNIVERSITY OF TECHNOLOGY:MATERIALS SCIENCE》, vol. 17, no. 2, 30 June 2002 (2002-06-30), pages 47 - 50 * |
| 何小林: "氨基膦酸螯合树脂应用现状", 《四川有色金属》, 30 September 2006 (2006-09-30) * |
| 刘军深: "螯合树脂法分离回收镓和铟的研究进展", 《稀有金属与硬质合金》, vol. 33, no. 4, 31 December 2005 (2005-12-31) * |
| 孙耀冉: "氨基膦酸型螯合离子交换剂的应用研究", 《安全与环境学报》, vol. 13, no. 5, 31 October 2013 (2013-10-31), pages 40 - 44 * |
Cited By (6)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104722563A (en) * | 2015-03-18 | 2015-06-24 | 合肥鑫晟光电科技有限公司 | Method for recycling indium on panel |
| 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 |
| CN107475523A (en) * | 2017-09-02 | 2017-12-15 | 河北工程大学 | A kind of method of the recovery indium from flyash |
| CN108893608A (en) * | 2018-05-30 | 2018-11-27 | 苏州精美科光电材料有限公司 | A kind of refinement method improving indium recovery |
| TWI803261B (en) * | 2022-03-28 | 2023-05-21 | 虹京金屬股份有限公司 | Method for recycling indium |
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Application publication date: 20141217 |