CN106868323A - A kind of method that indium is extracted from discarded liquid crystal display panel - Google Patents
A kind of method that indium is extracted from discarded liquid crystal display panel Download PDFInfo
- Publication number
- CN106868323A CN106868323A CN201710098111.4A CN201710098111A CN106868323A CN 106868323 A CN106868323 A CN 106868323A CN 201710098111 A CN201710098111 A CN 201710098111A CN 106868323 A CN106868323 A CN 106868323A
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- China
- Prior art keywords
- indium
- liquid crystal
- crystal display
- display panel
- discarded liquid
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Classifications
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- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B58/00—Obtaining gallium or indium
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B3/00—Extraction of metal compounds from ores or concentrates by wet processes
- C22B3/20—Treatment or purification of solutions, e.g. obtained by leaching
- C22B3/26—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds
- C22B3/38—Treatment or purification of solutions, e.g. obtained by leaching by liquid-liquid extraction using organic compounds containing phosphorus
- C22B3/384—Pentavalent phosphorus oxyacids, esters thereof
- C22B3/3846—Phosphoric acid, e.g. (O)P(OH)3
-
- C—CHEMISTRY; METALLURGY
- C22—METALLURGY; FERROUS OR NON-FERROUS ALLOYS; TREATMENT OF ALLOYS OR NON-FERROUS METALS
- C22B—PRODUCTION AND REFINING OF METALS; PRETREATMENT OF RAW MATERIALS
- C22B7/00—Working up raw materials other than ores, e.g. scrap, to produce non-ferrous metals and compounds thereof; Methods of a general interest or applied to the winning of more than two metals
- C22B7/006—Wet processes
- C22B7/007—Wet processes by acid leaching
-
- 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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- Engineering & Computer Science (AREA)
- Chemical & Material Sciences (AREA)
- Mechanical Engineering (AREA)
- Manufacturing & Machinery (AREA)
- Materials Engineering (AREA)
- Metallurgy (AREA)
- Organic Chemistry (AREA)
- Geology (AREA)
- General Life Sciences & Earth Sciences (AREA)
- Environmental & Geological Engineering (AREA)
- Life Sciences & Earth Sciences (AREA)
- Geochemistry & Mineralogy (AREA)
- Processing Of Solid Wastes (AREA)
Abstract
The present invention relates to a kind of method that indium is extracted from discarded liquid crystal display panel, the novel process being combined using hydro-thermal method and acidleach.Compared with traditional direct incineration disposal, using the organic material more green high-efficient in the discarded liquid crystal panel of hydro-thermal method pretreatment, secondary pollution is not produced, and be conducive to the recycling of organic matter.This method realize organic material resource degrade while, it is suppressed that transfer from indium to liquid phase.Indium is subsequently transferred to by liquid phase from solid phase as leaching liquor using sulfuric acid, using two（2 ethylhexyls）Phosphoric acid（p204）+ sulfonated kerosene carries out enriching and recovering as back washing agent as extractant, hydrochloric acid to indium.On the premise of energy-conserving and environment-protective, the recovery to greatest extent of indium in the ito glass of discarded liquid crystal panel can be realized.
Description
Technical field
It is that one kind is combined using hydrothermal pretreatment technology with acidleach the invention belongs to electron wastes resource reclaim field
The method of recovery indium from waste liquid crystal display.
Background technology
Lcd technology has already taken up the leading position in display market as Display Technique of new generation.Liquid crystal display
Utensil has the advantages that definition is high, image color is good, environmentally friendly, power saving, frivolous and portable, has been widely used in all kinds of displays
In equipment.Due to the quick replacement of liquid crystal technology, a large amount of liquid crystal displays face to be scrapped.And contain in the liquid crystal display scrapped
Various poisonous and harmful substances such as heavy metal, if treatment is mishandling, by the potential threat huge to environment structure；If but can be rationally
This kind of material is reclaimed, will to a certain extent alleviate the problem of the current energy and material shortage.
, used as a kind of strategy metal, due to not finding independent indium ore deposit also, commercial run is for indium for indium in liquid crystal display
Recovery rate of mining it is relatively low.The content of indium just has recovery value more than 0.002% in usual raw material, and one piece of liquid crystal display glass
The content of indium is higher than 0.03% in glass substrate, therefore, it will be a kind of efficiently feasible side that indium is separated and recovered from liquid crystal display
Method.
In practical operation, pretreatment, but the method are typically directly burned or are pyrolyzed to liquid crystal panel organic material
Resources and energy consumption is big, is also easy to produce secondary pollution.Product is complicated and with environmental risk higher, is unfavorable for the resource of organic matter
Change and utilize.
And hydrothermal technique is considered as having green technology with broad prospects for development, in closed high temperature, water under high pressure phase, have
Machine thing can occur the oxidation reaction of the pyrolysis, hydrolysis and dissolving reaction and aerobic participation based on degraded, and then can be by high score
Sub- organic matter is transformed into micromolecular compound and monomer, even carbon dioxide and water.Can be by changing in processing procedure
Operating condition, controls reaction process and generates different products, and then can both realize the innoxious degraded of debirs, can also make it
Resource conversion is carried out to expected intermediate product, the integrated treatment disposal of discarded liquid crystal display panel can be realized.
In sum, a kind of more energy-conserving and environment-protective of invention and scientific and effective return from the waste liquid crystal display
Receive the process of indium.
The content of the invention
Problem to be solved by this invention is to provide that a kind of energy consumption is relatively low, and of reduced contamination returns from waste liquid crystal display
The method for receiving indium.
A kind of method that indium is extracted from discarded liquid crystal display panel proposed by the present invention, comprises the following steps that：
（1）First electronic equipment is disassembled and isolates discarded liquid crystal display panel, be broken into size for 1 ~ 3 cm2Fragment；
（2）Using hydro-thermal method pre-treatment step（1）The discarded liquid crystal display panel for obtaining, the discarded liquid crystal display panel of degraded removal
The polaroid organic matter on surface, obtains solid phase residue；Hydro-thermal method reaction condition is：Controlling reaction temperature is 280 ~ 350 DEG C, every gram
In discarded liquid crystal display panel, water consumption is 12 ~ 18 mL, and oxidant addition is 2 ~ 5 mL, react 12 in neutral conditions ~
18 min；
（3）Using sulfuric acid solution as leaching liquor, by step（2）Indium in the solid phase residue for obtaining is separated out and enters sulfuric acid solution
In, obtain containing solution of indium；
（4）Using two（2- ethyl hexyls）Phosphoric acid（p204）With sulfonated kerosene as extractant, to step（3）Obtain containing indium
Solution is extracted；
（5）Using hydrochloric acid as back washing agent to carrying out enriching and recovering containing the indium in solution of indium.
In the present invention, step（1）In, it is not necessary to the polaroid to discarding liquid crystal display panel surface carries out lift-off processing.
In the present invention, step（2）In, hydro-thermal method pretreatment realizes that the degraded of discarded liquid crystal display panel organic material is gone
Remove, while making the indium in the middle of discarded liquid crystal display panel retain in the middle of solid phase residue.
In the present invention, step（3）In, the indium in solid product, control are extracted using the sulfuric acid solution of 0.3 ~ 0.8mol/L
60-80 DEG C of reaction temperature, solid-to-liquid ratio is 1:10~1:1 g/mL, the reaction time is 30 ~ 60 min, is obtained containing solution of indium.
In the present invention, step（4）In, with 15% ~ 25% 2（2- ethyl hexyls）Phosphoric acid and sulfonated kerosene as extractant,
Compare 1 in extraction phase:10~1:2 ~ 5 min are extracted under conditions of 5 (O/A).
In the present invention, step（5）In, using 3 ~ 5mol/L HCl as back washing agent, back extraction compares 8:1~12:1 (O/A's)
Under the conditions of be stripped 8 ~ 12 min.
The method have the advantages that：
1) lift-off processing need not be carried out to discarded liquid crystal display panel, reduce energy resource consumption in processing procedure；
2) hydrothermal pretreatment technology reacts thorough and green high-efficient, does not produce secondary pollution；
3) the method realizes the harmlessness disposing of discarded liquid crystal panel while recovery indium, beneficial to its integrated treatment disposal；
4) reaction time consumption is short, and substance recovery is high, is adapted to industrial production；
5) structure of reaction system equipment is relatively easy to, and easy to operate, is easy to industrialization promotion.
Specific embodiment
With reference to specific embodiment, the present invention is further described.
Embodiment 1
（1）First electronic equipment is disassembled and isolates discarded liquid crystal display panel, be broken into cm × 1.5 cm's of size about 1
Fragment；
（2）Weigh（1）In the g of fragment 2.4, in putting it into hydro-thermal reaction device, controlling reaction temperature is 300 DEG C, water consumption
It is 36 mL, oxidant addition is 7.2 mL, and 15 min are reacted in neutral conditions.Now, liquid crystal panel organic material
90% is degraded, meanwhile, the indium in glass substrate is remained in solid phase residue；
（3）Right（2）In solid product carry out filter operation after, use 0.5 mol/L sulfuric acid solution extract solid product
In indium, 70 DEG C of controlling reaction temperature, solid-to-liquid ratio 1:2g/mL, reacts 40 min, obtains containing solution of indium；
（4）Using 20% p204+ sulfonated kerosenes as extractant, 1 is compared in extraction phase：8（O/A）Under conditions of, it is right（3）In containing indium
Solution extracts 3 min；
（5）Using 4 mol/L HCl as back washing agent, back extraction compares 10:1（O/A）Under conditions of be stripped 10 min, obtain chlorination
Solution of indium.
By the strict control to above operating process, the rate of recovery of indium can reach more than 95%.
Embodiment 2
（1）First electronic equipment is disassembled and isolates discarded liquid crystal display panel, be broken into the fragment of the cm2 of size about 1 ~ 3；
（2）Weigh（1）In the g of fragment 2.4, in putting it into hydro-thermal reaction device, controlling reaction temperature is 325 DEG C, uses water
It is 36 mL to measure, and oxidant addition is 7.2 mL, and 13 min are reacted in neutral conditions；
（3）Right（2）In solid product carry out filter operation after, use 0.5 mol/L sulfuric acid solution extract solid product
In indium, 60 DEG C of controlling reaction temperature, solid-to-liquid ratio 1:10 g/mL, react 60 min, obtain containing solution of indium.The now recovery of indium
Rate is up to 90%；
（4）Using 20% p204+ sulfonated kerosenes as extractant, 1 is compared in extraction phase：5（O/A）Under conditions of, it is right（3）In containing indium
Solution extracts 5 min.Now the extraction yield of indium can basically reach 100%；
（5）Using 4 mol/L HCl as back washing agent, back extraction compares 10:1（O/A）Under conditions of be stripped 8 min, obtain chlorination
Solution of indium.Now back extraction ratio is close to 85%.
Claims (6)
1. it is a kind of from discarded liquid crystal display panel extract indium method, it is characterised in that comprise the following steps that：
（1）First electronic equipment is disassembled and isolates discarded liquid crystal display panel, be broken into size for 1 ~ 3 cm2Fragment；
（2）Using hydro-thermal method pre-treatment step（1）The discarded liquid crystal display panel for obtaining, the discarded liquid crystal display panel of degraded removal
The polaroid organic matter on surface, obtains solid phase residue；Hydro-thermal method reaction condition is：Controlling reaction temperature is 280 ~ 350 DEG C, every gram
In discarded liquid crystal display panel, water consumption is 12 ~ 18 mL, and oxidant addition is 2 ~ 5 mL, react 12 in neutral conditions ~
18 min；
（3）Using sulfuric acid solution as leaching liquor, by step（2）Indium in the solid phase residue for obtaining is separated out and enters sulfuric acid solution
In, obtain containing solution of indium；
（4）Using two（2- ethyl hexyls）Phosphoric acid（p204）With sulfonated kerosene as extractant, to step（3）Obtain containing indium
Solution is extracted；
（5）Using hydrochloric acid as back washing agent to carrying out enriching and recovering containing the indium in solution of indium.
2. it is according to claim 1 from discarded liquid crystal display panel extract indium method, it is characterised in that：Step（1）
In, it is not necessary to the polaroid to discarding liquid crystal display panel surface carries out lift-off processing.
3. it is according to claim 3 from discarded liquid crystal display panel extract indium method, it is characterised in that：Step（2）
In, the degraded removal of discarded liquid crystal display panel organic material is realized in hydro-thermal method pretreatment, while making discarded liquid crystal display panel
Central indium is retained in the middle of solid phase residue.
4. it is according to claim 1 from discarded liquid crystal display panel extract indium method, it is characterised in that：Step（3）
In, the indium in solid product, 60-80 DEG C of controlling reaction temperature are extracted using the sulfuric acid solution of 0.3 ~ 0.8mol/L, solid-to-liquid ratio is
1:10~1:1g/mL, the reaction time is 30 ~ 60 min, is obtained containing solution of indium.
5. it is according to claim 1 from discarded liquid crystal display panel extract indium method, it is characterised in that：Step（4）
In, with 15% ~ 25% 2（2- ethyl hexyls）Phosphoric acid, as extractant, 1 is compared in extraction phase with sulfonated kerosene:10~1:5 (O/A's)
Under the conditions of extract 2 ~ 5 min.
6. it is according to claim 1 from discarded liquid crystal display panel extract indium method, it is characterised in that：Step（5）
In, using 3 ~ 5mol/L HCl as back washing agent, back extraction compares 8:1~12:8 ~ 12 min are stripped under conditions of 1 (O/A).
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710098111.4A CN106868323A (en) | 2017-02-23 | 2017-02-23 | A kind of method that indium is extracted from discarded liquid crystal display panel |
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| Application Number | Priority Date | Filing Date | Title |
|---|---|---|---|
| CN201710098111.4A CN106868323A (en) | 2017-02-23 | 2017-02-23 | A kind of method that indium is extracted from discarded liquid crystal display panel |
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| CN106868323A true CN106868323A (en) | 2017-06-20 |
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| CN201710098111.4A Pending CN106868323A (en) | 2017-02-23 | 2017-02-23 | A kind of method that indium is extracted from discarded liquid crystal display panel |
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Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112280986A (en) * | 2020-10-22 | 2021-01-29 | 上海交通大学 | Method for leaching gallium and arsenic from waste gallium arsenide-containing LED electronic devices and simultaneously recovering metallic silver and application |
| CN112410585A (en) * | 2020-10-22 | 2021-02-26 | 上海交通大学 | Method for recovering gallium arsenide and copper from waste and old IC components containing gallium arsenide and application |
| CN113005307A (en) * | 2021-02-25 | 2021-06-22 | 上海第二工业大学 | Method for recycling indium in waste liquid crystal panel by taking self-pyrolysis residue as reducing agent |
Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104498721A (en) * | 2015-01-08 | 2015-04-08 | 中国科学院城市环境研究所 | Innocent treatment method and system for liquid crystal panel |
| CN104630486A (en) * | 2015-01-28 | 2015-05-20 | 江苏理工学院 | Method for recovering indium oxide and stannum from ITO coating film of conducting glass |
| CN105420502A (en) * | 2015-11-27 | 2016-03-23 | 四川长虹格润再生资源有限责任公司 | Method for recovering indium from waste liquid crystal display screen panel |
-
2017
- 2017-02-23 CN CN201710098111.4A patent/CN106868323A/en active Pending
Patent Citations (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN104498721A (en) * | 2015-01-08 | 2015-04-08 | 中国科学院城市环境研究所 | Innocent treatment method and system for liquid crystal panel |
| CN104630486A (en) * | 2015-01-28 | 2015-05-20 | 江苏理工学院 | Method for recovering indium oxide and stannum from ITO coating film of conducting glass |
| CN105420502A (en) * | 2015-11-27 | 2016-03-23 | 四川长虹格润再生资源有限责任公司 | Method for recovering indium from waste liquid crystal display screen panel |
Cited By (3)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| CN112280986A (en) * | 2020-10-22 | 2021-01-29 | 上海交通大学 | Method for leaching gallium and arsenic from waste gallium arsenide-containing LED electronic devices and simultaneously recovering metallic silver and application |
| CN112410585A (en) * | 2020-10-22 | 2021-02-26 | 上海交通大学 | Method for recovering gallium arsenide and copper from waste and old IC components containing gallium arsenide and application |
| CN113005307A (en) * | 2021-02-25 | 2021-06-22 | 上海第二工业大学 | Method for recycling indium in waste liquid crystal panel by taking self-pyrolysis residue as reducing agent |
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Application publication date: 20170620 |