CN104975186B - Comprehensive recycling method for ITO film sensor - Google Patents
Comprehensive recycling method for ITO film sensor Download PDFInfo
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- CN104975186B CN104975186B CN201510455199.1A CN201510455199A CN104975186B CN 104975186 B CN104975186 B CN 104975186B CN 201510455199 A CN201510455199 A CN 201510455199A CN 104975186 B CN104975186 B CN 104975186B
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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
- Y02P10/20—Recycling
Abstract
The invention discloses a comprehensive recycling method for an ITO film sensor. The comprehensive recycling method comprises the following steps of A, mechanical pretreatment; B, degumming treatment; C, organic solvent removing and recovering from a film; D, non-ferrous metal removing; E, film regeneration; F, gum and solvent recovery; and G, metal recovery. By means of the comprehensive recycling method, valuable materials in the film are fully recovered, the film part is used for generating plastic particles, the metal part is used for obtaining respective high purity metals, and gum is used for generating regenerated gum and can be used for coating production; the regeneration recovery rate is high and reaches about 97%; environment friendliness is achieved, no new waste is generated in the regeneration process, and environment pollution is avoided; production cost is low, a certain profit margin exists in the recovery process, and an enterprise is high in operation maintaining capacity; production devices can be in matching, industrial production is facilitated, and the method is suitable for use and popularization.
Description
Technical field
The present invention relates to utilization of the recycling of renewable resources field, specifically the comprehensive reutilization side of ito film functional sheet
Method.
Background technology
Ito film functional sheet refers to play the film material of touch controllable function in the touch screens such as mobile phone, flat board, notebook,
It is made up of after etching ITO lines, printing conductive silver paste, laminating OCA ito film.Its common structure has following two
Kind：（1）Protecting film+ito film+OCA+ mould release membrances（PET film）；（2）Protecting film+ito film+OCA+ITO film+OCA+mould release membrance
（PET film）；The recoverable such as tin indium oxide wherein in OCA glue, ito film.
In ito film functional sheet production process, typically there are 3-5% bad products, it is impossible to use, have hundreds of according to statistics every year
As many as ton；Meanwhile, in there are the various intelligent artifacts such as superseded mobile phone, LCD TV, computer monitor every year, also there is ito film
Functional sheet, enormous amount.
There is the mode of two kinds of recovery at present, the first carries out heating separation using electrical heating wire to pressure sensitive adhesive, then uses stone
Oily ether is wiped to glue surface, is removed glue-line, then is reclaimed the tin indium oxide on film with pickling；The problem of presence, productivity ratio are low,
High cost, it is difficult to be after, while wipe glue material be difficult to reclaim, cause secondary pollution；Another kind is directly to burn to lose Organic substance,
Then the non-ferrous metals such as silver-colored indium are reclaimed, shortcoming in combustion, produces substantial amounts of toxic gas, and air pollution is serious.In order to
Pollution of these garbages to environment is reduced, the waste of useful materials is reduced, we have developed this new method.
The content of the invention
It is an object of the invention to overcome the deficiencies in the prior art, and provide a kind of synthetical recovery profit of ito film functional sheet
With method, glue that it can be in synthetical recovery ito film functional sheet and tin indium oxide etc..
The present invention is adopted the following technical scheme that：
The comprehensive reutilization method of ito film functional sheet, using following steps：
A, mechanical pretreatment：Diameter 0.5-6mm, the hole of spacing 1-35mm are got with puncher on ito film functional sheet；
B, degumming process：The ito film functional sheet of mechanical pretreatment is put in reactor, the organic of weight 2-5 times is added
Solvent, rotation, stirring, dissolves 5-12 hours, filters, and separates membrane, and glue is scattered in glued membrane in solvent, forms glued membrane and suspends
Body；The organic solvent is dichloromethane, chloroform, ethyl acetate, one or more in acetone；
C, film removing organic solvent are simultaneously reclaimed：By the film of degumming process, in closed vessel in heating to 100 DEG C, in 6-
2 hours under conditions of 20mmHg, to remove organic solvent, gas cooling reclaims organic solvent；
D, de- non-ferrous metal are processed：By de- organic solvent qualified film, the nitre of about 0.5-1mol/L is added in reactor
Acid, adds 1.5 kilograms of potassium permanganate, 3.5 kilograms of hydrogen peroxide by film per ton, reacts 6-10 hours, forms non-ferrous metal solution；
The regeneration of E, film：By de- non-ferrous metal qualified film, pelletize in comminutor is added, that is, obtains qualified plastic raw materialss
Granule；
F, glue, the recovery of solvent：Glued membrane suspended substance is filtered, filter cake is added in heating in vacuum reactor, at 85-100 °C,
Under conditions of 5-20mmHg, 3-5 hour is evaporated, that is, obtains reclaimed rubber；Organic solvent is reclaimed in the gas Jing coolings of evaporation；
The recovery of G, metal：Sodium chloride solution is added in non-ferrous metal solution, silver ion therein is kept completely separate, then
Adjust in the middle of pH=0.5-1.0, add the potassium permanganate and hydrogen peroxide with step D equivalent, stannum is divided from solution in tin ash
From, pH=0.5 being adjusted, is extracted with p204, with 6mol/L hydrochloric acid back extraction, evaporate recovery acid, it is brilliant that condensing crystallizing obtains indium chloride
Body, the dehydration under 333 °C of nitrogen protections obtain indium chloride；Detached silver, stannum are acidified respectively, are obtained each with zinc powder reduction
Metal.
It is an advantage of the current invention that：
1st, the valuable material in film has fully been reclaimed, wherein film part generates plastic grain, and metal part is obtained each
High pure metal, glue generate reclaimed rubber, can be used for coating production；
2nd, the response rate of regeneration is high, reaches 97% or so；
3rd, environmental friendliness, does not produce new garbage, does not result in environmental pollution in regenerative process；
4th, low production cost, has certain profit margin in removal process, and enterprise itself ability that keeps on the go is strong；Production
Equipment can be conducive to industrialized production with supporting, and these are that additive method is beyond one's reach.
Below specific embodiment, the invention will be further described.
Embodiment 1：The comprehensive reutilization method of ito film functional sheet, using following steps：
A, mechanical pretreatment：Diameter 0.5mm is got with puncher on ito film functional sheet, the hole of spacing 1mm is beneficial to
The diffusion of solvent, reduces the response time；
B, degumming process：The ito film functional sheet of mechanical pretreatment is put in reactor, the dichloromethane of 2 times of weight is added
Alkane, rotation, stirring, dissolves 5 hours, filters, and separates membrane, and glue is scattered in glued membrane in solvent, forms glued membrane suspended substance；
C, film removing organic solvent are simultaneously reclaimed：By the film of degumming process, in closed vessel in heating to 100 DEG C,
2 hours under conditions of 6mmHg, to remove organic solvent, gas cooling reclaims organic solvent；
D, de- non-ferrous metal are processed：By de- organic solvent qualified film, the nitric acid of about 0.5mol/L is added in reactor,
1.5 kilograms of potassium permanganate, 3.5 kilograms of hydrogen peroxide are added by film per ton, 6-10 hours are reacted, non-ferrous metal solution is formed；
The regeneration of E, film：By de- non-ferrous metal qualified film, pelletize in comminutor is added, that is, obtains qualified plastic raw materialss
Granule；
F, glue, the recovery of solvent：Glued membrane suspended substance is filtered, filter cake is added in heating in vacuum reactor, at 85 °C,
Under conditions of 5mmHg, 3 hours are evaporated, that is, obtains reclaimed rubber；Organic solvent is reclaimed in the gas Jing coolings of evaporation；
The recovery of G, metal：Sodium chloride solution is added in non-ferrous metal solution, silver ion therein is kept completely separate, then
Adjust in the middle of pH=0.5, add the potassium permanganate and hydrogen peroxide with step D equivalent, stannum is separated from solution in tin ash,
PH=0.5 is adjusted, is extracted with p204, with 6mol/L hydrochloric acid back extraction, evaporate recovery acid, condensing crystallizing obtains indium chloride crystal,
The dehydration under 333 °C of nitrogen protections obtains indium chloride；Detached silver, stannum are acidified respectively, obtain respective with zinc powder reduction
Metal.
As stated above, 200Kg ito film functional sheets, wherein argentiferous 1.62Kg, indium 300g stannum 35g are taken, glue is 28Kg, film
For 170Kg；Silver-colored 1.59Kg, indium chloride 547.4g stannum 33g is finally given, the qualified film 170.2Kg of non-ferrous metal, glue is taken off
27.4Kg.Wherein silver-colored extraction ratio is 98.1%, and the extraction ratio of indium is 94.35%, and the extraction ratio of stannum is 94.2%, the response rate of glue
For 97.8%, the response rate of film is 100.1%.
Embodiment 2:The comprehensive reutilization method of ito film functional sheet, using following steps：
A, mechanical pretreatment：Diameter 6mm, the hole of spacing 35mm are got with puncher on ito film functional sheet；
B, degumming process：The ito film functional sheet of mechanical pretreatment is put in reactor, three chloromethanes of 5 times of weight are added
Alkane, rotation, stirring, dissolves 12 hours, filters, and separates membrane, and glue is scattered in glued membrane in solvent, forms glued membrane suspended substance；
C, film removing organic solvent are simultaneously reclaimed：By the film of degumming process, in closed vessel in heating to 100 DEG C,
2 hours under conditions of 20mmHg, to remove organic solvent, gas cooling reclaims organic solvent；
D, de- non-ferrous metal are processed：By de- organic solvent qualified film, the nitric acid of about 1mol/L is added in reactor, is pressed
Film per ton adds 1.5 kilograms of potassium permanganate, 3.5 kilograms of hydrogen peroxide, reacts 6-10 hours, forms non-ferrous metal solution；
The regeneration of E, film：By de- non-ferrous metal qualified film, pelletize in comminutor is added, that is, obtains qualified plastic raw materialss
Granule；
F, glue, the recovery of solvent：Glued membrane suspended substance is filtered, filter cake is added in heating in vacuum reactor, at 100 °C,
Under conditions of 20mmHg, 5 hours are evaporated, that is, obtains reclaimed rubber；Organic solvent is reclaimed in the gas Jing coolings of evaporation；
The recovery of G, metal：Sodium chloride solution is added in non-ferrous metal solution, silver ion therein is kept completely separate, then
Adjust in the middle of pH=1.0, add the potassium permanganate and hydrogen peroxide with step D equivalent, stannum is separated from solution in tin ash,
PH=0.5 is adjusted, is extracted with p204, with 6mol/L hydrochloric acid back extraction, evaporate recovery acid, condensing crystallizing obtains indium chloride crystal,
The dehydration under 333 °C of nitrogen protections obtains indium chloride；Detached silver, stannum are acidified respectively, obtain respective with zinc powder reduction
Metal.
As stated above, 200Kg ito film functional sheets, wherein argentiferous 1.62Kg, indium 300g stannum 35g are taken, glue is 28Kg, film
For 170Kg；Silver-colored 1.57Kg, indium chloride 548.3g stannum 32g is finally given, the qualified film 170.7Kg of non-ferrous metal, glue is taken off
27.3Kg.Wherein silver-colored extraction ratio is 96.9%, and the extraction ratio of indium is 95%, and the extraction ratio of stannum is 91.4%, and the response rate of glue is
97.5%, the response rate of film is 100.4%.
Embodiment 3：The comprehensive reutilization method of ito film functional sheet, using following steps：
A, mechanical pretreatment：Diameter 2mm, the hole of spacing 15mm are got with puncher on ito film functional sheet；
B, degumming process：The ito film functional sheet of mechanical pretreatment is put in reactor, the acetic acid of weight 2-5 times is added
Ethyl ester, rotation, stirring, dissolves 7 hours, filters, and separates membrane, and glue is scattered in glued membrane in solvent, forms glued membrane suspended substance；
C, film removing organic solvent are simultaneously reclaimed：By the film of degumming process, in closed vessel in heating to 100 DEG C,
2 hours under conditions of 11mmHg, to remove organic solvent, gas cooling reclaims organic solvent；
D, de- non-ferrous metal are processed：By de- organic solvent qualified film, the nitric acid of about 0.7mol/L is added in reactor,
1.5 kilograms of potassium permanganate, 3.5 kilograms of hydrogen peroxide are added by film per ton, is reacted 8 hours, form non-ferrous metal solution；
The regeneration of E, film：By de- non-ferrous metal qualified film, pelletize in comminutor is added, that is, obtains qualified plastic raw materialss
Granule；
F, glue, the recovery of solvent：Glued membrane suspended substance is filtered, filter cake is added in heating in vacuum reactor, at 90 °C,
Under conditions of 10mmHg, 4 hours are evaporated, that is, obtains reclaimed rubber；Organic solvent is reclaimed in the gas Jing coolings of evaporation；
The recovery of G, metal：Sodium chloride solution is added in non-ferrous metal solution, silver ion therein is kept completely separate, then
Adjust in the middle of pH=0.8, add the potassium permanganate and hydrogen peroxide with step D equivalent, stannum is separated from solution in tin ash,
PH=0.5 is adjusted, is extracted with p204, with 6mol/L hydrochloric acid back extraction, evaporate recovery acid, condensing crystallizing obtains indium chloride crystal,
The dehydration under 333 °C of nitrogen protections obtains indium chloride；Detached silver, stannum are acidified respectively, obtain respective with zinc powder reduction
Metal.
As stated above, 200Kg ito film functional sheets, wherein argentiferous 1.62Kg, indium 300g stannum 35g are taken, glue is 28Kg, film
For 170Kg；Silver-colored 1.58Kg, indium chloride 547.6g stannum 32.5g is finally given, the qualified film 170.5Kg of non-ferrous metal, glue is taken off
27.4Kg.Wherein silver-colored extraction ratio is 97.5%, and the extraction ratio of indium is 94.1%, and the extraction ratio of stannum is 92.8%, and the response rate of glue is
97.9%, the response rate of film is 100.3%.
Embodiment 4：The comprehensive reutilization method of ito film functional sheet, using following steps：
A, mechanical pretreatment：Diameter 4mm, the hole of spacing 20mm are got with puncher on ito film functional sheet；
B, degumming process：The ito film functional sheet of mechanical pretreatment is put in reactor, the acetone of 4 times of weight, rotation is added
Turn, stir, dissolve 10 hours, filter, separate membrane, glue is scattered in glued membrane in solvent, form glued membrane suspended substance；
C, film removing organic solvent are simultaneously reclaimed：By the film of degumming process, in closed vessel in heating to 100 DEG C,
2 hours under conditions of 15mmHg, to remove organic solvent, gas cooling reclaims organic solvent；
D, de- non-ferrous metal are processed：By de- organic solvent qualified film, the nitric acid of about 0.9mol/L is added in reactor,
1.5 kilograms of potassium permanganate, 3.5 kilograms of hydrogen peroxide are added by film per ton, is reacted 9 hours, form non-ferrous metal solution；
The regeneration of E, film：By de- non-ferrous metal qualified film, pelletize in comminutor is added, that is, obtains qualified plastic raw materialss
Granule；
F, glue, the recovery of solvent：Glued membrane suspended substance is filtered, filter cake is added in heating in vacuum reactor, at 95 °C,
Under conditions of 15mmHg, 5 hours are evaporated, that is, obtains reclaimed rubber；Organic solvent is reclaimed in the gas Jing coolings of evaporation；
The recovery of G, metal：Sodium chloride solution is added in non-ferrous metal solution, silver ion therein is kept completely separate, then
Adjust in the middle of pH=0.8, add the potassium permanganate and hydrogen peroxide with step D equivalent, stannum is separated from solution in tin ash,
PH=0.5 is adjusted, is extracted with p204, with 6mol/L hydrochloric acid back extraction, evaporate recovery acid, condensing crystallizing obtains indium chloride crystal,
The dehydration under 333 °C of nitrogen protections obtains indium chloride；Detached silver, stannum are acidified respectively, obtain respective with zinc powder reduction
Metal.
As stated above, 200Kg ito film functional sheets, wherein argentiferous 1.62Kg, indium 300g stannum 35g are taken, glue is 28Kg, film
For 170Kg；Silver-colored 1.59Kg, indium chloride 546.9g stannum 32.8g is finally given, the qualified film 170.1Kg of non-ferrous metal, glue is taken off
27.5Kg.Wherein silver-colored extraction ratio is 98.1%, and the extraction ratio of indium is 94.0%, and the extraction ratio of stannum is 93.7%, and the response rate of glue is
98.2%, the response rate of film is 100.1%.
Embodiment 5：The comprehensive reutilization method of ito film functional sheet, using following steps：
A, mechanical pretreatment：Diameter 5mm, the hole of spacing 30mm are got with puncher on ito film functional sheet；
B, degumming process：The ito film functional sheet of mechanical pretreatment is put in reactor, the dichloro of 4.5 times of weight is added
Methane and chloroform, rotation, stirring, dissolve 11 hours, filter, and separate membrane, and glue is scattered in glued membrane in solvent, form glue
Film suspended substance；
C, film removing organic solvent are simultaneously reclaimed：By the film of degumming process, in closed vessel in heating to 100 DEG C,
2 hours under conditions of 18mmHg, to remove organic solvent, gas cooling reclaims organic solvent；
D, de- non-ferrous metal are processed：By de- organic solvent qualified film, the nitric acid of about 0.9mol/L is added in reactor,
1.5 kilograms of potassium permanganate, 3.5 kilograms of hydrogen peroxide are added by film per ton, is reacted 8 hours, form non-ferrous metal solution；
The regeneration of E, film：By de- non-ferrous metal qualified film, pelletize in comminutor is added, that is, obtains qualified plastic raw materialss
Granule；
F, glue, the recovery of solvent：Glued membrane suspended substance is filtered, filter cake is added in heating in vacuum reactor, at 97 °C,
Under conditions of 18mmHg, 3 hours are evaporated, that is, obtains reclaimed rubber；Organic solvent is reclaimed in the gas Jing coolings of evaporation；
The recovery of G, metal：Sodium chloride solution is added in non-ferrous metal solution, silver ion therein is kept completely separate, then
Adjust in the middle of pH=0.9, add the potassium permanganate and hydrogen peroxide with step D equivalent, stannum is separated from solution in tin ash,
PH=0.5 is adjusted, is extracted with p204, with 6mol/L hydrochloric acid back extraction, evaporate recovery acid, condensing crystallizing obtains indium chloride crystal,
The dehydration under 333 °C of nitrogen protections obtains indium chloride；Detached silver, stannum are acidified respectively, obtain respective with zinc powder reduction
Metal.
As stated above, 200Kg ito film functional sheets, wherein argentiferous 1.62Kg, indium 300g stannum 35g are taken, glue is 28Kg, film
For 170Kg；Silver-colored 1.58Kg, indium chloride 547.8g stannum 32.7g is finally given, the qualified film 170.5Kg of non-ferrous metal, glue is taken off
27.7Kg.Wherein silver-colored extraction ratio is 97.5%, and the extraction ratio of indium is 94.1%, and the extraction ratio of stannum is 93.4%, and the response rate of glue is
98.9%, the response rate of film is 100.3%.
When organic solvent is dichloromethane, chloroform, ethyl acetate, several in acetone, between them
Ratio is any.
According to above example result, the response rate of silver reaches more than 97%, the response rate of indium reaches more than 94%, and stannum is returned
Yield reaches more than 91%, the response rate more than 97% of glue, and film reaches more than 100%, this is because when leaching, having minimal amount of
Glue residua from terms of result, has reached fabulous effect on film.
Claims (1)
- The comprehensive reutilization method of 1.ITO film functional sheets, it is characterised in that adopt following steps：A, mechanical pretreatment：Diameter 0.5-6mm, the hole of spacing 1-35mm are got with puncher on ito film functional sheet；B, degumming process：The ito film functional sheet of mechanical pretreatment is put in reactor, the organic solvent of weight 2-5 times is added, Rotation, stirring, dissolve 5-12 hours, filter, and separate membrane, and glue is scattered in glued membrane in solvent, form glued membrane suspended substance；It is described Organic solvent is dichloromethane, chloroform, ethyl acetate, one or more in acetone；C, film removing organic solvent are simultaneously reclaimed：By the film of degumming process, in closed vessel in heating to 100 DEG C, in 6- 2 hours under conditions of 20mmHg, to remove organic solvent, gas cooling reclaims organic solvent；D, de- non-ferrous metal are processed：By de- organic solvent qualified film, the nitric acid of 0.5-1mol/L is added in reactor, by every Ton film adds 1.5 kilograms of potassium permanganate, 3.5 kilograms of hydrogen peroxide, reacts 6-10 hours, forms non-ferrous metal solution；The regeneration of E, film：By de- non-ferrous metal qualified film, pelletize in comminutor is added, that is, obtains qualified plastic raw materialss Grain；F, glue, the recovery of solvent：Glued membrane suspended substance is filtered, filter cake is added in heating in vacuum reactor, at 85-100 °C, 5- Under conditions of 20mmHg, 3-5 hour is evaporated, that is, obtains reclaimed rubber；Organic solvent is reclaimed in the gas Jing coolings of evaporation；The recovery of G, metal：Sodium chloride solution is added in non-ferrous metal solution, silver ion therein is kept completely separate, is then adjusted In the middle of pH=0.5-1.0, the potassium permanganate and hydrogen peroxide with step D equivalent is added, stannum is separated from solution in tin ash, PH=0.5 is adjusted, is extracted with p204, with 6mol/L hydrochloric acid back extraction, evaporate recovery acid, condensing crystallizing obtains indium chloride crystal, The dehydration under 333 °C of nitrogen protections obtains indium chloride；Detached silver, stannum are acidified respectively, obtain respective with zinc powder reduction Metal.
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| CN105489544B (en) * | 2016-01-12 | 2018-05-29 | 惠州Tcl移动通信有限公司 | The method and its required plant tin fixture that gluing integrated circuit recycles |
| CN110227679A (en) * | 2019-06-13 | 2019-09-13 | 慧迈材料科技(广东)有限公司 | A method of OCA glue on component is removed using solvent method |
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| JP3524568B2 (en) * | 1993-10-26 | 2004-05-10 | 日鉱金属株式会社 | Method for recovering indium from arsenic-containing indium solution |
| CN1191380C (en) * | 2002-11-07 | 2005-03-02 | 长沙矿冶研究院 | Method for extracting refined indium from indium tin oxide waste material |
| KR20040048662A (en) * | 2002-12-04 | 2004-06-10 | 주식회사 씨에스 이엔지 | Method for withdrawing indium from waste-ITO target by using nitric acid |
| CN101643853B (en) * | 2009-06-22 | 2012-02-22 | 云南锡业集团（控股）有限责任公司 | Method for extracting indium and recovering valuable metals from flue dust of tin |
| CN101660054B (en) * | 2009-07-15 | 2011-08-10 | 中国科学院青海盐湖研究所 | Method for extracting metal indium from waste residues generated from lead and zinc smelting |
| CN104630486B (en) * | 2015-01-28 | 2017-02-22 | 江苏理工学院 | Method for recovering indium oxide and stannum from ITO coating film of conducting glass |
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