CN106702167A - Method for efficiently removing impurities from pickle liquor of abandoned liquid crystal display - Google Patents
Method for efficiently removing impurities from pickle liquor of abandoned liquid crystal display Download PDFInfo
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- CN106702167A CN106702167A CN201710132240.0A CN201710132240A CN106702167A CN 106702167 A CN106702167 A CN 106702167A CN 201710132240 A CN201710132240 A CN 201710132240A CN 106702167 A CN106702167 A CN 106702167A
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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
- 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
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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
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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 efficiently removing impurities from pickle liquor of an abandoned liquid crystal display, and belongs to the technical field of recycling of the pickle liquor of the abandoned liquid crystal display. The hydrochloric acid concentration of the pickle liquor of the abandoned liquid crystal display is adjusted, mixed liquid 1 is obtained, a combined extraction agent is added into the mixed liquid 1 for extraction, and an oil and liquid mixed phase 1 is obtained, and is subject to liquid separation, tail liquid 1 containing impurities of Al3+, Ca2+, Na+ and Mg2+ and an extraction oil phase 1 containing In3+, Fe3+ and Sn2+ are obtained, a sodium nitrate and hydrochloric acid mixed solution is added into the extraction oil phase 1 for washing and impurity removal, and In rich liquid and an extraction oil phase 2 containing Fe3+ and Sn2+ are obtained; hydrochloric acid is added into the extraction oil phase 2 for washing, and the extraction agent is purified, so that the combined extraction agent and tail liquid 2 containing Fe3+ and Sn2+ can be recycled are obtained. Efficient impurity removal can be achieved, leached-out tail liquid can be recycled, and the beneficial effects of being high in separation efficiency, simple and short in flow process and friendly to environment are achieved.
Description
Technical field
The invention belongs to the utilization technology field of waste liquid crystal display leachate, liquid crystal is more particularly to discarded
Show the efficient impurity removal method of device pickle liquor.
Background technology
Used as the display system of a new generation, liquid crystal display is more frivolous, and color is also more bright-coloured, and image quality is also much
Exceed traditional CRT monitor, be widely used in various electronic products such as LCD TV, computer display screen, mobile phone.However, with
Continuing to develop for Display Technique to need to be recycled with update, a large amount of discarded electronic products.By taking LCD TV as an example,
Only 2009 sales volumes nearly 70,000,000, and its service life is generally 6-8, this means that just there is more than 7,000 ten thousand only single year
The learies of platform, quantity is very huge.Used as the one kind in dangerous electron wastes, it largely scraps right waste liquid crystal display
The huge potential threat of environment structure.And LCD plate surface, with soda-lime glass as substrate, surface deposition has 140~
ITO (the In of 150nm2O3:SnO2=9:1) film, average indium content up to 0.03%, significantly larger than raw ore indium production standard
0.002%.And indium is used as a kind of dissipated metal, global reserves are only the 1/6 of gold, by the U.S., Japan, multiple states such as China
Family is classified as strategy metal.The secondary resource that a large amount of discarded liquid crystal displays are smelted as indium metal, carries out recycling pole
Tool environment strategy meaning.
At present, in waste liquid crystal display the recovery research of indium it is main in a wet process based on (Chinese invention patent CN
200610088278.4th, CN201010295590.7, ZL200910024354.9), obtain what indium was reclaimed by disassembling for initial stage
Direct material --- useless ito glass, pickle liquor containing indium, then purified-displacement-thick indium refining are obtained by it by acidleach mode
Removal of impurities purification is carried out etc. process.However, waste liquid crystal display is during acidleach, due to useless ito glass complicated component, cause
Determination of Multi-Impurities (aluminium, calcium, sodium, magnesium, iron, tin) is leached jointly during acidleach with indium.Therefore, waste liquid crystal display
Efficient impurity removal is the key for influenceing indium to reclaim in pickle liquor.But research is directed to the pickling liquid of the plurality of impurities metal ion at present
The impurity-removing method of system does not trigger a large amount of concerns yet.
The method that Chinese invention patent (ZL20131054468.6) discloses recovery indium in a kind of liquid crystal display.Its profit
Abstraction impurity removal is carried out with P204, but because Leaching Systems acidity of sulfuric acid is 2mol/L-6mol/L, a large amount of acid-base accommodation pH need to be consumed
To 1.0-2.0, to reach the acidity that extraction is required；And the extractant and sulfonated kerosene volatility of use are stronger, inflammable, there is potential
Environmental pollution threaten, do not fully take into account the recycle and reuse of extractant yet.Indium and common extraction elemental iron, tin separative efficiency
It is relatively low, it is difficult to realize efficient impurity removal.Ionic liquid is widely used in efficient abstraction impurity removal as novel green solvent.But at present
Research focuses primarily upon abstraction impurity removal (Chinese invention patent ZL200710179062.3, CN of rare earth element
201410109393.X).Not yet there is research to be related to the recycling of indium in liquid crystal display.
The content of the invention
Indium recycles problem during the object of the invention is mainly solution waste liquid crystal display, particularly solves discarded liquid crystal
The efficient impurity removal problem of display pickle liquor.Extractant instant invention overcomes existing research is applicable that Acidity Range is narrow, extractant
Volatile, inflammable, potential pollution is serious, the low shortcoming of dust removal rate, discloses a kind of high in liquid crystal display pickle liquor from abandoning
The method for imitating removal of impurities, realizes efficiently separating for impurity element aluminium, calcium, sodium, magnesium, iron, tin and indium.The present invention has impurity element
Separative efficiency is high, short flow, tail washings reusable edible, it is environment-friendly the characteristics of.
The method of efficient impurity removal is as follows in the pickle liquor from waste liquid crystal display of the present invention：
1) waste liquid crystal display pickle liquor concentration of hydrochloric acid is adjusted, concentration of hydrochloric acid is preferably adjusted to 0.6mol/L-8mol/L,
Obtain mixed liquor 1；
2) 1- methyl-trioctylphosphine-ammonium nitrate (A336NO3) and 1- methyl-trioctylmethylammonium chloride are added in mixed liquor 1
(A336Cl) a kind of mixture with trialkyl phosphoric-oxygenic compound (Cyanex923) in, the volume of trialkyl phosphoric-oxygenic compound
Fraction is preferably 40%-70%, is uniformly mixed into row combined extraction, and fluid ratio is 1:1-1:20, extraction time is 5min-
40min, extractive reaction temperature is 25 DEG C -60 DEG C, obtains fluid mixed phase 1；
3) 1 point of liquid of fluid mixed phase, obtains containing impurity A l3+、Ca2+、Na+、Mg2+Tail washings 1, and contain In3+、Fe3+、
Sn2+Extraction oil phase 1；
4) extraction oil phase 1 adds the mixed solution wash-out removal of impurities of sodium nitrate and hydrochloric acid, and the sodium nitrate of preferably mixed solution is dense
Degree 1mol/L-4mol/L, H+It is 2mol/L-6mol/L, fluid is in a ratio of 1:0.5-1:10, the reaction time is 3min-20min,
Reaction temperature is 35 DEG C -70 DEG C.Obtain In pregnant solutions and contain Fe3+、Sn2+Extraction oil phase 2；
5) extraction oil phase 2 adds salt acid elution, purifies extractant, and preferably concentration of hydrochloric acid is 0.1mol/L-1mol/L, fluid
It is in a ratio of 1:2-1:20, the washing reaction time is 10min-30min, and reaction temperature is 30 DEG C -50 DEG C, obtains recycling
Combined extraction phase and contain Fe3+、Sn2+Tail washings 2, tail washings 2 can extract wherein remaining indium with circulating and recovering.
Further by step 4) the In pregnant solutions that obtain carry out step 1 again) -4) circulation；Can repeatedly be circulated.
Outstanding role of the invention has：
Quaternary ammonium salt ionic liquid A336NO is utilized in the present invention3/ A336Cl and acid phosphine type extractant Cyanex923 conducts
Combined extraction agent carrys out extraction of indium, and it is wider that the system is applicable Acidity Range.And the present invention is by sodium nitrate and salt acid elution, remove
With the iron tin impurity of indium common extraction, the single separation rate of wherein tin/indium and iron/indium reaches 104More than.The joint extraction that the present invention is used
Agent is taken, circulating and recovering has also been obtained.
Brief description of the drawings
Fig. 1 represent a kind of pickle liquor from waste liquid crystal display in efficient impurity removal process chart；
Specific embodiment
With reference to embodiment, the degree present invention is described further, but the present invention is not limited to following examples.
All features disclosed in this specification, in method and process, except mutually exclusive feature is, can be with any side
Formula self assemble.
Embodiment 1
Adjustment waste liquid crystal display pickle liquor concentration of hydrochloric acid obtains mixed liquor 1 to 2mol/L, is added in mixed liquor 1
, used as extractant, corresponding fluid ratio is 1 for A336Cl (30%) and Cyanex923 (70%):5, after reacting 20min in 25 DEG C
To fluid mixed phase 1, carry out point liquid and obtain containing impurity A l3+、Ca2+、Na+、Mg2+Tail washings 1, and contain In3+、Fe3+、Sn2+
Extraction oil phase 1；Extraction oil phase 1 adds 2mol/L hydrochloric acid to elute impurity with 3mol/L sodium nitrate mixed liquor, and fluid ratio is 1:10,
3min is eluted in 40 DEG C, In pregnant solutions is obtained and is contained Fe3+、Sn2+Extraction oil phase 2；Extraction is washed using the watery hydrochloric acid of 1mol/L
Oil phase 2 is taken, extractant is purified, preferred fluid ratio is 1：2,10min is washed in 30 DEG C, the indium recovery after one cycle is
94.38%, solution kind indium purity is up to 98.84%.
Embodiment 2
Adjustment waste liquid crystal display pickle liquor concentration of hydrochloric acid obtains mixed liquor 1 to 3mol/L, is added in mixed liquor 1
, used as extractant, corresponding fluid ratio is 1 for A336Cl (40%) and Cyanex923 (60%):10, after reacting 5min in 25 DEG C
To fluid mixed phase 1, fluid mixed phase 1 carries out point liquid and obtains containing impurity A l3+、Ca2+、Na+、Mg2+Tail washings 1, and contain In3 +、Fe3+、Sn2+Extraction oil phase 1；Extraction oil phase 1 adds 4mol/L hydrochloric acid to elute impurity, fluid with 3mol/L sodium nitrate mixed liquor
Than being 1:0.5,20min is eluted in 50 DEG C, obtain In pregnant solutions and contain Fe3+、Sn2+Extraction oil phase 2；Using 0.1mol/L
Watery hydrochloric acid washing extraction oil phase 2, purify extractant, preferred fluid ratio be 1：5,15min is washed in 50 DEG C, after one cycle
Indium recovery be 96.46%, solution kind indium purity is up to 99.58%.
Embodiment 3
Adjustment waste liquid crystal display pickle liquor concentration of hydrochloric acid obtains mixed liquor 1 to 0.8mol/L, is added in mixed liquor 1
, used as extractant, corresponding fluid ratio is 1 for A336Cl (60%) and Cyanex923 (40%):1, after reacting 30min in 45 DEG C
To fluid mixed phase 1, fluid mixed phase 1 carries out point liquid and obtains containing impurity A l3+、Ca2+、Na+、Mg2+Tail washings 1, and contain In3 +、Fe3+、Sn2+Extraction oil phase 1；Extraction oil phase 1 adds 2mol/L hydrochloric acid to elute impurity, fluid with 3mol/L sodium nitrate mixed liquor
Than being 1:10,30min is eluted in 30 DEG C, obtain In pregnant solutions and contain Fe3+、Sn2+Extraction oil phase 2；Using 0.5mol/L's
Watery hydrochloric acid washing extraction oil phase 2, purifies extractant, and preferred fluid ratio is 1：20,30min is washed in 30 DEG C, after one cycle
Indium recovery be 96.68%, solution kind indium purity is up to 99.88%.
Embodiment 4
Adjustment waste liquid crystal display pickle liquor concentration of hydrochloric acid obtains mixed liquor 1 to 4.8mol/L, is added in mixed liquor 1
, used as extractant, corresponding fluid ratio is 1 for A336Cl (50%) and Cyanex923 (50%):1, after reacting 30min in 45 DEG C
To fluid mixed phase 1, fluid mixed phase 1 carries out point liquid and obtains containing impurity A l3+、Ca2+、Na+、Mg2+Tail washings 1, and contain In3 +、Fe3+、Sn2+Extraction oil phase 1；Extraction oil phase 1 adds 6mol/L hydrochloric acid to elute impurity, fluid with 1mol/L sodium nitrate mixed liquor
Than being 1:1,20min is eluted in 70 DEG C, obtain In pregnant solutions and contain Fe3+、Sn2+Extraction oil phase 2；Using 0.8mol/L's
Watery hydrochloric acid washing extraction oil phase 2, purifies extractant, and preferred fluid ratio is 1：10,30min is washed in 45 DEG C, after one cycle
Indium recovery be 95.82%, solution kind indium purity is up to 98.36%.
Embodiment 5
Adjustment waste liquid crystal display pickle liquor concentration of hydrochloric acid obtains mixed liquor 1 to 0.6mol/L, is added in mixed liquor 1
, used as extractant, corresponding fluid ratio is 1 for A336Cl (55%) and Cyanex923 (45%):20, after reacting 10min in 60 DEG C
Fluid mixed phase 1 is obtained, fluid mixed phase 1 carries out point liquid and obtains containing impurity A l3+、Ca2+、Na+、Mg2+Tail washings 1, and contain
In3+、Fe3+、Sn2+Extraction oil phase 1；Extraction oil phase 1 adds 6mol/L hydrochloric acid to elute impurity with 1mol/L sodium nitrate mixed liquor,
Fluid ratio is 1:1,20min is eluted in 60 DEG C, obtain In pregnant solutions and contain Fe3+、Sn2+Extraction oil phase 2；Using 0.1mol/
The watery hydrochloric acid washing extraction oil phase 2 of L, purifies extractant, and preferred fluid ratio is 1：20, wash 30min, one cycle in 35 DEG C
Indium recovery afterwards is 96.24%, and solution kind indium purity is up to 97.58%.
Embodiment 6
Adjustment waste liquid crystal display pickle liquor concentration of hydrochloric acid obtains mixed liquor 1 to 6.6mol/L, is added in mixed liquor 1
A336NO3(35%) and Cyanex923 (65%) is used as extractant, corresponding fluid ratio is 1:20, after reacting 40min in 60 DEG C
Fluid mixed phase 1 is obtained, fluid mixed phase 1 carries out point liquid and obtains containing impurity A l3+、Ca2+、Na+、Mg2+Tail washings 1, and contain
In3+、Fe3+、Sn2+Extraction oil phase 1；Extraction oil phase 1 adds 6mol/L hydrochloric acid to elute impurity with 4mol/L sodium nitrate mixed liquor,
Fluid ratio is 1:1,40min is eluted in 60 DEG C, obtain In pregnant solutions and contain Fe3+、Sn2+Extraction oil phase 2；Using 0.1mol/
The watery hydrochloric acid washing extraction oil phase 2 of L, purifies extractant, and preferred fluid ratio is 1：5, wash 30min, one cycle in 45 DEG C
Indium recovery afterwards is 92.36%, and solution kind indium purity is up to 99.92%.
Embodiment 7
Adjustment waste liquid crystal display pickle liquor concentration of hydrochloric acid obtains mixed liquor 1 to 8mol/L, is added in mixed liquor 1
A336NO3(45%) and Cyanex923 (55%) is used as extractant, corresponding fluid ratio is 1:8, after reacting 10min in 48 DEG C
The fluid mixed phase 1 for obtaining, fluid mixed phase 1 carries out point liquid and obtains containing impurity A l3+、Ca2+、Na+、Mg2+Tail washings 1, and contain
There is In3+、Fe3+、Sn2+Extraction oil phase 1；It is miscellaneous that extraction oil phase 1 adds 3mol/L hydrochloric acid to be eluted with 1mol/L sodium nitrate mixed liquor
Matter, fluid ratio is 1:4,15min is eluted in 50 DEG C, obtain In pregnant solutions and contain Fe3+、Sn2+Extraction oil phase 2；Utilize
The watery hydrochloric acid washing extraction oil phase 2 of 0.1mol/L, purifies extractant, and preferred fluid ratio is 1：20,20min is washed in 35 DEG C,
Indium recovery after one cycle is 97.44%, and solution kind indium purity is up to 95.58%.
Embodiment 8
Adjustment waste liquid crystal display pickle liquor concentration of hydrochloric acid obtains mixed liquor 1 to 4.2mol/L, is added in mixed liquor 1
A336NO3(60%) and Cyanex923 (40%) is used as extractant, corresponding fluid ratio is 1:12, after reacting 25min in 45 DEG C
Fluid mixed phase 1 is obtained, fluid mixed phase 1 carries out point liquid and obtains containing impurity A l3+、Ca2+、Na+、Mg2+Tail washings 1, and contain
In3+、Fe3+、Sn2+Extraction oil phase 1；It is miscellaneous that extraction oil phase 1 adds 3.5mol/L hydrochloric acid to be eluted with 3.5mol/L sodium nitrate mixed liquor
Matter, fluid ratio is 1:15,15min is eluted in 55 DEG C, obtain In pregnant solutions and contain Fe3+、Sn2+Extraction oil phase 2；Utilize
The watery hydrochloric acid washing extraction oil phase 2 of 0.8mol/L, purifies extractant, and preferred fluid ratio is 1：14,20min is washed in 30 DEG C,
Indium recovery after one cycle is 95.93%, and solution kind indium purity is up to 99.92%.
Claims (9)
1. in a kind of pickle liquor from waste liquid crystal display efficient impurity removal method, it is characterised in that comprise the following steps:
1) waste liquid crystal display pickle liquor concentration of hydrochloric acid is adjusted, mixed liquor 1 is obtained；
2) 1- methyl-trioctylphosphine-ammonium nitrate (A336NO3) and 1- methyl-trioctylmethylammonium chloride (A336Cl) are added in mixed liquor 1
In a kind of mixture with trialkyl phosphoric-oxygenic compound (Cyanex923), be uniformly mixed into row combined extraction, obtain fluid mixing
Phase 1；
3) 1 point of liquid of fluid mixed phase, obtains containing impurity A l3+、Ca2+、Na+、Mg2+Tail washings 1, and contain In3+、Fe3+、Sn2+'s
Extraction oil phase 1；
4) extraction oil phase 1 adds the mixed solution wash-out removal of impurities of sodium nitrate and hydrochloric acid, obtains In pregnant solutions and contains Fe3+、Sn2+'s
Extraction oil phase 2；
5) extraction oil phase 2 adds salt acid elution, purifies extractant, obtains recycled combined extraction phase and contains Fe3+、
Sn2+Tail washings 2, tail washings 2 can extract wherein remaining indium with circulating and recovering.
2., according to the method for efficient impurity removal in a kind of pickle liquor from waste liquid crystal display described in claim 1, its feature exists
In step 1) adjust concentration of hydrochloric acid to 0.6mol/L-8mol/L.
3., according to the method for efficient impurity removal in a kind of pickle liquor from waste liquid crystal display described in claim 1, its feature exists
In step 2) in 1- methyl-trioctylphosphine-ammonium nitrate (A336NO3) and 1- methyl-trioctylmethylammonium chloride (A336Cl) it is a kind of with
The volume fraction of trialkyl phosphoric-oxygenic compound is preferably 40%- in the mixture of trialkyl phosphoric-oxygenic compound (Cyanex923)
70%.
4., according to the method for efficient impurity removal in a kind of pickle liquor from waste liquid crystal display described in claim 1, its feature exists
In step 2) fluid ratio be 1:1-1:20, extraction time is 5min-40min, and extractive reaction temperature is 25 DEG C -60 DEG C.
5., according to the method for efficient impurity removal in a kind of pickle liquor from waste liquid crystal display described in claim 1, its feature exists
In step 4) the sodium nitrate concentration 1mol/L-4mol/L, H of mixed solution+It is 2mol/L-6mol/L.
6., according to the method for efficient impurity removal in a kind of pickle liquor from waste liquid crystal display described in claim 1, its feature exists
In step 4) fluid is in a ratio of 1:0.5-1:10, the reaction time is 3min-20min, and reaction temperature is 35 DEG C -70 DEG C.
7., according to the method for efficient impurity removal in a kind of pickle liquor from waste liquid crystal display described in claim 1, its feature exists
In step 5) concentration of hydrochloric acid be 0.1mol/L-1mol/L.
8., according to the method for efficient impurity removal in a kind of pickle liquor from waste liquid crystal display described in claim 1, its feature exists
In step 5) fluid is in a ratio of 1:2-1:20, the washing reaction time is 10min-30min, and reaction temperature is 30 DEG C -50 DEG C.
9., according to the method for efficient impurity removal in a kind of pickle liquor from waste liquid crystal display described in claim 1, its feature exists
In by step 4) the In pregnant solutions that obtain carry out step 1 again) -4) circulation；Repeatedly circulated.
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Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100224030A1 (en) * | 2009-03-04 | 2010-09-09 | Chung Yuan Christian University | Indium recovery by supported liquid membrane with strip dispersion |
| CN101660047B (en) * | 2009-07-15 | 2011-05-25 | 中国科学院青海盐湖研究所 | Composite extractant, preparation thereof and application thereof in metal indium extraction |
| CN104087750A (en) * | 2014-07-14 | 2014-10-08 | 厦门稀土材料研究所 | Rare earth extraction and separation method |
| US20140299543A1 (en) * | 2010-12-17 | 2014-10-09 | University Of South Australia | Extraction of metals |
| CN105483389A (en) * | 2016-01-13 | 2016-04-13 | 云南大学 | Leaching method for indium in waste liquid crystal panel and leaching agent |
-
2017
- 2017-03-07 CN CN201710132240.0A patent/CN106702167B/en active Active
Patent Citations (5)
| Publication number | Priority date | Publication date | Assignee | Title |
|---|---|---|---|---|
| US20100224030A1 (en) * | 2009-03-04 | 2010-09-09 | Chung Yuan Christian University | Indium recovery by supported liquid membrane with strip dispersion |
| CN101660047B (en) * | 2009-07-15 | 2011-05-25 | 中国科学院青海盐湖研究所 | Composite extractant, preparation thereof and application thereof in metal indium extraction |
| US20140299543A1 (en) * | 2010-12-17 | 2014-10-09 | University Of South Australia | Extraction of metals |
| CN104087750A (en) * | 2014-07-14 | 2014-10-08 | 厦门稀土材料研究所 | Rare earth extraction and separation method |
| CN105483389A (en) * | 2016-01-13 | 2016-04-13 | 云南大学 | Leaching method for indium in waste liquid crystal panel and leaching agent |
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