JP4306167B2 - Method for decomposing organic resin for sealing - Google Patents
Method for decomposing organic resin for sealing Download PDFInfo
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- JP4306167B2 JP4306167B2 JP2001338108A JP2001338108A JP4306167B2 JP 4306167 B2 JP4306167 B2 JP 4306167B2 JP 2001338108 A JP2001338108 A JP 2001338108A JP 2001338108 A JP2001338108 A JP 2001338108A JP 4306167 B2 JP4306167 B2 JP 4306167B2
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- sealing
- organic resin
- humidity
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- decomposing
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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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/20—Waste processing or separation
-
- 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
- Y02W—CLIMATE CHANGE MITIGATION TECHNOLOGIES RELATED TO WASTEWATER TREATMENT OR WASTE MANAGEMENT
- Y02W30/00—Technologies for solid waste management
- Y02W30/50—Reuse, recycling or recovery technologies
- Y02W30/82—Recycling of waste of electrical or electronic equipment [WEEE]
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- Processing Of Solid Wastes (AREA)
- Surface Treatment Of Glass (AREA)
Description
【０００１】
【発明の属する技術分野】
本発明は封止用有機樹脂の分解方法に係り、特に、合わせガラス、強化ガラス、プラズマディスプレイパネル、電磁波シールドパネル、太陽電池、半導体などの電子素子封止製品の封止用有機樹脂を分解して、これらの廃棄物から、ガラス、フィルタ、セル、素子等の有価物を回収して再利用するための封止用有機樹脂の分解方法に関する。
【０００２】
【従来の技術】
近年、合わせガラス、強化ガラス、プラズマディスプレイパネル、電磁波シールドパネル、太陽電池、半導体などの電子素子封止製品の普及に伴い、これらの廃棄物の処理が問題視されるようになってきている。
【０００３】
これらの封止製品は、ガラス等の基板間に、用途に応じて、フィルタ、セル、素子、その他の機能性部品が封止用有機樹脂により封止された構成とされている。通常、これらの封止製品にあっては、主に封止用有機樹脂の劣化により廃品に到り、多くの場合、基板ガラスやフィルタ、セル、素子等は使用可能な状態である。
【０００４】
従って、廃棄物の減量、資源の有効利用を図るために、これらの封止製品の廃棄物を解体して、基板ガラス、フィルタ、セル、素子等の有価物を回収、再利用することが望まれるが、一般に封止用有機樹脂は難分解性であり、これらの封止製品を解体して、有価物をその性能を損ねることなく回収することは困難であった。このため、これらの封止製品の廃棄物は、不燃物として埋め立て処分とされているのが現状である。
【０００５】
しかし、埋め立て処分では、埋め立て地の不足、埋め立て範囲の限界の問題があり、また、例えば太陽電池セルの電極のように、鉛などの重金属を含むものが埋め立てられた場合には、環境への影響が懸念される。
【０００６】
そこで、これらの封止製品のリサイクル化の検討が盛んに行われ、例えば、太陽電池セルのリサイクル技術として、封止用有機樹脂の除去のために、硝酸処理法、熱分解法、流動床式燃焼法、有機溶媒法が提案された。
【０００７】
硝酸処理法は、８０℃に加熱した硝酸によって封止用有機樹脂を分解する方法である。熱分解法は、不活性ガス中において、約５００℃まで加熱して封止用有機樹脂を除去する方法である。流動床式燃焼法は、約４５０℃の流動床により封止用有機樹脂を除去する方法である。有機触媒法は、ｏ−ジクロルベンゼン、トリクロルエチレン等の有機溶媒によって封止用有機樹脂を除去する方法である。
【０００８】
【発明が解決しようとする課題】
上記従来の封止用有機樹脂の除去方法のうち、硝酸処理法は、硝酸廃液の処理、ＮＯｘ発生の可能性の欠点がある。熱分解法は、コストが安く、他の方法に比べてセルに近い状態で回収可能であるが、ＮＯｘ発生の可能性や太陽電池特性の劣化という欠点がある。流動床式燃焼法は、太陽電池表面を削り取るため、ウェハの状態で回収され、再セル化の作業を要するという欠点がある。
【０００９】
有機溶媒法では、太陽電池の性能を損ねることなく、ｏ−ジクロルベンゼンやトリクロルエチレン等の有機溶媒によって封止用有機樹脂のみを分解し、セルに近い状態で回収することが可能であるが、高温において有機溶媒で処理するため、有機溶媒の揮発による環境汚染及びコストの面で問題がある。
【００１０】
このようなことから、従来のリサイクル技術はいずれも実用化に到っていない。
【００１１】
本発明は、上記従来の問題点を解決し、環境に悪影響を及ぼすことなく、また、封止されている有価物の性能を損なうことなく、封止用有機樹脂を効果的に分解除去する方法を提供することを目的とする。
【００１２】
【課題を解決するための手段】
本発明の封止用有機樹脂の分解方法は、封止用有機樹脂を、温度１００℃以上、湿度１００％ＲＨ以上、かつ圧力１気圧以上の高温、高湿、高圧条件下に保持する封止用有機樹脂の分解方法であって、該封止用有機樹脂がエチレンビニルアセテート、ポリビニルアセタール、ポリビニルブチラール及びエポキシ系樹脂よりなる群から選ばれる１種又は２種以上であり、該封止用有機樹脂を高温、高湿、高圧条件に設定可能な装置内に投入した後加熱し、その後加湿した後加圧することにより、該封止用有機樹脂を、温度１００〜２００℃、相対湿度１００％（１００％ＲＨ）、圧力１〜３０気圧（０．１〜３．０ＭＰａ）の高温、高湿、高圧条件とすることを特徴とする。
【００１３】
封止用有機樹脂を高温、高湿、高圧条件下に保持することにより、有機溶媒を用いることなく、また、封止されているセル、素子等の有価物の性能を損ねることなく、封止用有機樹脂を分解することができる。
【００１４】
本発明においては、封止用有機樹脂により封止された物品を高温、高湿、高圧条件とすることが好ましい。
【００１５】
このような本発明が適用される封止物品としては、合わせガラス、強化ガラス、プラズマディスプレイパネル、電磁波シールドパネル、又は太陽電池、半導体などの電子素子封止物品が挙げられる。
【００１６】
【発明の実施の形態】
以下に本発明の封止用有機樹脂の分解方法の実施の形態を詳細に説明する。
【００１７】
本発明においては、具体的には、封止用有機樹脂により封止された物品を高温、高湿、高圧条件に設定可能な装置、例えば、オートクレーブ、プレッシャー・クッカー試験機等に投入し、高温、高湿、高圧条件下に所定時間保持する。
【００１８】
この処理条件とは、１００℃以上の高温、水蒸気量飽和状態、即ち、相対湿度１００％（１００％ＲＨ）の高湿、１気圧（０．１ＭＰａ）以上の高圧条件である。温度、圧力の上限については、分解する封止用有機樹脂の種類や封止製品の形態、処理時間、装置仕様、コスト等を考慮して適宜決定されるが、一般的には、温度１００〜２００℃、圧力１〜３０気圧（０．１〜３．０ＭＰａ）の範囲とする。処理時間は、これらの高温、高湿条件下において、封止用有機樹脂が分解除去される時間であり、処理条件、封止用有機樹脂の種類によっても異なるが、一般的には１〜５０時間程度である。
【００１９】
本発明を実施するには、例えば、前述の装置を用い、常温、常湿、常圧下で封止製品を投入して密閉し、その後加熱により１００℃以上の適切な温度に設定し、次いで加湿して１００％ＲＨに設定する。その後、徐々に加圧していき、１気圧以上に設定し、この条件で所定時間保持すれば良い。
【００２０】
本発明で分解対象となる封止用有機樹脂は、一般的には合わせガラス、強化ガラス、プラズマディスプレイパネル、電磁波シールドパネル、又は太陽電池、半導体などの電子素子封止物品の封止用有機樹脂として用いられるものであり、エチレンビニルアセテート（エチレン−酢酸ビニル共重合樹脂：ＥＶＡ）、ポリビニルアセテート、ポリビニルブチラール（ＰＶＢ）、エポキシ系樹脂が挙げられる。封止製品中には、これらの封止用有機樹脂が２種以上混合されて用いられていても良く、或いは２層以上の封止膜層が形成されていても良い。
【００２１】
このような本発明の封止用有機樹脂の分解方法によれば、合わせガラス、強化ガラス、プラズマディスプレイパネル、電磁波シールドパネル、太陽電池、半導体などの電子素子封止製品を前記条件下に処理して封止用有機樹脂を分解し、封止されているガラス、フィルタ、セル、素子等の有価物を良好な状態で回収して再利用することができる。なお、本発明で対象とする封止製品は、封止用有機樹脂により封止されたものであり、何ら上記のものに限定されるものではない。また、本発明は、このような封止製品の使用済廃棄物に限らず、工場で発生する不良品、ユーザーからの返品についても適用できることは言うまでもない。
【００２２】
【実施例】
以下に実施例を挙げて本発明をより具体的に説明する。
【００２３】
なお、以下において、封止製品を高温、高湿、高圧条件下で処理するための装置としては、タバイエスペック（株）製「プレッシャー・クッカー（ＴＰＣ−４１１Ｄ）」を用い、処理手順は前述の如く、(1)加熱、(2)加湿、(3)加圧の順とした。
【００２４】
実施例１
ガラス（厚み３ｍｍ）／封止用有機樹脂（ＥＶＡ）（厚み０．５ｍｍ）／ガラス（厚み３ｍｍ）からなる合わせガラスを試作し、この合わせガラスを上記装置により１２０℃、１００％ＲＨ、１．２気圧（０．１２ＭＰａ）の高温、高湿、高圧条件下に２４時間保持した。
【００２５】
処理後、合わせガラスの封止用有機樹脂は完全に分解しており、ガラスのみが回収された。回収されたガラスにはダメージは無く、リサイクル可能であった。
【００２６】
実施例２
フッ素樹脂フィルム（厚み５０μｍ）／封止用有機樹脂（ＥＶＡ）（厚み０．５ｍｍ）／太陽電池用セル／ガラス（厚み３ｍｍ）からなる太陽電池モジュールを試作し、この太陽電池モジュールを上記装置により１２０℃、１００％ＲＨ、１．２気圧（０．１２ＭＰａ）の高温、高湿、高圧条件下に２４時間保持した。
【００２７】
処理後、太陽電池モジュールの封止用有機樹脂は完全に分解しており、ガラスとセルのみが回収された。回収されたガラスにもセルにもダメージは無く、リサイクル可能であった。
【００２８】
実施例３
ガラス（厚み１ｍｍ）／メッシュ（厚み０．２ｍｍ）／封止用有機樹脂（ＥＶＡ）（厚み１ｍｍ）／ガラス（厚み１ｍｍ）からなるプラズマディスプレイ用電磁波シールドパネルを試作し、この電磁波シールドパネルを上記装置により１２０℃、１００％ＲＨ、１．２気圧（０．１２ＭＰａ）の高温、高湿、高圧条件下に２４時間保持した。
【００２９】
処理後、電磁波シールドパネルの封止用有機樹脂は完全に分解しており、ガラスとメッシュのみが回収された。回収されたガラスにもメッシュにもダメージは無く、リサイクル可能であった。
【００３０】
【発明の効果】
以上詳述した通り、本発明の封止用有機樹脂の分解方法によれば、環境に悪影響を及ぼすことなく、また、封止されている有価物の性能を損なうことなく、封止用有機樹脂を効果的に分解除去することができる。
本発明によれば、合わせガラス、強化ガラス、プラズマディスプレイパネル、電磁波シールドパネル、太陽電池、半導体などの電子素子封止製品の廃棄物から、ガラス、フィルタ、セル、素子等の有価物を回収して再利用することが可能となり、廃棄物の減量、資源の有効利用を図ることができる。[0001]
BACKGROUND OF THE INVENTION
The present invention relates to a method for decomposing an organic resin for sealing, and in particular, decomposes an organic resin for sealing an electronic device sealing product such as laminated glass, tempered glass, a plasma display panel, an electromagnetic shielding panel, a solar cell, and a semiconductor. In addition, the present invention relates to a method for decomposing a sealing organic resin for recovering and reusing valuable materials such as glass, filters, cells, and elements from these wastes.
[0002]
[Prior art]
In recent years, with the widespread use of electronic device sealing products such as laminated glass, tempered glass, plasma display panels, electromagnetic wave shield panels, solar cells, and semiconductors, the disposal of these wastes has become a problem.
[0003]
These sealed products have a configuration in which a filter, a cell, an element, and other functional parts are sealed with a sealing organic resin between substrates such as glass depending on applications. In general, these sealing products reach waste products mainly due to deterioration of the sealing organic resin, and in many cases, substrate glass, filters, cells, elements, and the like are usable.
[0004]
Therefore, in order to reduce the amount of waste and effectively use resources, it is desirable to dismantle the waste of these sealed products and collect and reuse valuable materials such as substrate glass, filters, cells, and devices. However, in general, the sealing organic resin is hardly decomposable, and it has been difficult to disassemble these sealing products and recover valuable materials without impairing their performance. For this reason, the present condition is that the wastes of these sealed products are disposed as landfills as incombustibles.
[0005]
However, in landfill disposal, there is a problem of shortage of landfill site and limit of landfill range.For example, when materials containing heavy metals such as lead, such as solar cell electrodes, are buried in the environment, There are concerns about the impact.
[0006]
Therefore, the recycling of these encapsulated products has been actively studied. For example, as a recycling technique for solar cells, a nitric acid treatment method, a thermal decomposition method, a fluidized bed type for removing an organic resin for sealing. Combustion methods and organic solvent methods were proposed.
[0007]
The nitric acid treatment method is a method of decomposing the sealing organic resin with nitric acid heated to 80 ° C. The thermal decomposition method is a method of removing the sealing organic resin by heating to about 500 ° C. in an inert gas. The fluidized bed combustion method is a method in which the organic resin for sealing is removed by a fluidized bed at about 450 ° C. The organic catalyst method is a method of removing the sealing organic resin with an organic solvent such as o-dichlorobenzene or trichloroethylene.
[0008]
[Problems to be solved by the invention]
Of the above method of removing the conventional sealing organic resin, nitric acid treatment process, the process of nitric acid waste liquid, there is a disadvantage of the possibility of the NO x generation. The thermal decomposition method is low in cost and can be recovered in a state closer to the cell than other methods, but has the disadvantage that NO x may be generated and the solar cell characteristics deteriorate. The fluidized bed combustion method has a drawback in that the surface of the solar cell is scraped off, so that it is collected in a wafer state and requires re-celling.
[0009]
In the organic solvent method, it is possible to decompose only the sealing organic resin with an organic solvent such as o-dichlorobenzene or trichloroethylene and recover it in a state close to the cell without impairing the performance of the solar cell. Since the treatment is performed with an organic solvent at a high temperature, there are problems in terms of environmental pollution and cost due to volatilization of the organic solvent.
[0010]
For these reasons, none of the conventional recycling technologies has been put into practical use.
[0011]
The present invention solves the above-mentioned conventional problems, and effectively decomposes and removes the sealing organic resin without adversely affecting the environment and without impairing the performance of the valuables being sealed. The purpose is to provide.
[0012]
[Means for Solving the Problems]
The method for decomposing an organic resin for sealing according to the present invention is a sealing in which an organic resin for sealing is maintained under conditions of high temperature, high humidity, and high pressure at a temperature of 100 ° C. or higher, a humidity of 100% RH or higher, and a pressure of 1 atmosphere or higher A method for decomposing an organic resin for sealing, wherein the sealing organic resin is one or more selected from the group consisting of ethylene vinyl acetate, polyvinyl acetal, polyvinyl butyral, and epoxy resin, and the sealing organic resin The resin is put in an apparatus that can be set to high temperature, high humidity, and high pressure conditions, heated, then humidified, and then pressurized to bring the sealing organic resin into a temperature of 100 to 200 ° C. and a relative humidity of 100% ( 100% RH), high temperature, high humidity, and high pressure conditions of 1-30 atm (0.1-3.0 MPa) pressure .
[0013]
By holding the sealing organic resin under high temperature, high humidity , and high pressure conditions, sealing without using an organic solvent and without impairing the performance of valuable materials such as sealed cells and elements. The organic resin can be decomposed.
[0014]
In the present invention, the high temperature of the sealed article by sealing organic resin, high humidity, it is preferable that the high pressure condition.
[0015]
The sealing article to which the present invention is applied, such as this, laminated glass, tempered glass, a plasma display panel, electromagnetic wave shielding panel, or a solar cell, an electronic device encapsulating articles such as semiconductor and the like.
[0016]
DETAILED DESCRIPTION OF THE INVENTION
Embodiments of the method for decomposing an organic resin for sealing of the present invention will be described in detail below.
[0017]
In the present invention, specifically, an article sealed with an organic resin for sealing is put into an apparatus that can be set to high temperature, high humidity, and high pressure conditions, such as an autoclave, a pressure cooker tester, etc. Hold for a predetermined time under high humidity and high pressure.
[0018]
This treatment condition is a high temperature of 100 ° C. or higher and a water vapor saturation state, that is, a high humidity of 100% relative humidity (100% RH) and a high pressure of 1 atm (0.1 MPa) or more. The upper limit of the temperature and pressure is appropriately determined in consideration of the type of the organic resin for sealing to be decomposed, the form of the sealing product, the processing time, the apparatus specifications, the cost, and the like. 200 ° C., shall be the range of pressure from 1 to 30 atmospheres (0.1~3.0MPa). The treatment time is the time during which the sealing organic resin is decomposed and removed under these high-temperature and high-humidity conditions, and varies depending on the treatment conditions and the type of the sealing organic resin. It is about time.
[0019]
In order to carry out the present invention, for example, using the above-mentioned apparatus, the sealed product is charged and sealed at room temperature, normal humidity, and normal pressure, and then set to an appropriate temperature of 100 ° C. or higher by heating, and then humidified. To 100% RH. Thereafter, the pressure is gradually increased, the pressure is set to 1 atm or higher, and this condition is maintained for a predetermined time.
[0020]
Sealing the organic resins to be decomposed in the present invention, laminated glass on one common, tempered glass, a plasma display panel, electromagnetic wave shielding panel, or a solar cell, for sealing electronic element sealing articles such as semiconductor is intended to be used as the organic resin, et Ji Ren vinyl acetate (ethylene - vinyl acetate copolymer resin: EVA), polyvinyl acetate, polyvinyl butyral (PVB), include epoxy resins it is. Two or more kinds of these sealing organic resins may be mixed and used in the sealing product, or two or more sealing film layers may be formed.
[0021]
According to such a method for decomposing an organic resin for sealing of the present invention, electronic device sealing products such as laminated glass, tempered glass, a plasma display panel, an electromagnetic wave shielding panel, a solar cell, and a semiconductor are processed under the above-described conditions. Thus, the sealing organic resin can be decomposed, and valuable materials such as sealed glass, filters, cells, and elements can be recovered and reused in a good state. In addition, the sealing product made into object by this invention is sealed with the organic resin for sealing, and is not limited to the above thing at all. Moreover, it goes without saying that the present invention is applicable not only to such waste products of sealed products, but also to defective products generated in factories and returns from users.
[0022]
【Example】
Hereinafter, the present invention will be described more specifically with reference to examples.
[0023]
In the following, as an apparatus for processing a sealed product under high temperature, high humidity and high pressure conditions, “Pressure Cooker (TPC-411D)” manufactured by Tabay Espec Co., Ltd. is used, and the processing procedure is as described above. Thus, (1) heating, (2) humidification, and (3) pressurization were performed in this order.
[0024]
Example 1
A laminated glass made of glass (thickness 3 mm) / sealing organic resin (EVA) (thickness 0.5 mm) / glass (thickness 3 mm) was made as a prototype, and this laminated glass was subjected to 120 ° C., 100% RH, and 1. It was kept under high temperature, high humidity and high pressure conditions of 2 atm (0.12 MPa) for 24 hours.
[0025]
After the treatment, the organic resin for sealing the laminated glass was completely decomposed, and only the glass was recovered. The recovered glass was not damaged and could be recycled.
[0026]
Example 2
A solar cell module made of a fluororesin film (thickness 50 μm) / organic resin for sealing (EVA) (thickness 0.5 mm) / cell for solar cell / glass (thickness 3 mm) was prototyped. It was kept under high temperature, high humidity and high pressure conditions of 120 ° C., 100% RH, 1.2 atm (0.12 MPa) for 24 hours.
[0027]
After the treatment, the organic resin for sealing the solar cell module was completely decomposed, and only glass and cells were recovered. The recovered glass and cells were not damaged and could be recycled.
[0028]
Example 3
An electromagnetic wave shielding panel for plasma display made of glass (thickness 1 mm) / mesh (thickness 0.2 mm) / organic resin for sealing (EVA) (thickness 1 mm) / glass (thickness 1 mm) was prototyped. The apparatus was maintained for 24 hours under conditions of 120 ° C., 100% RH, 1.2 atm (0.12 MPa), high temperature, high humidity, and high pressure.
[0029]
After the treatment, the organic resin for sealing the electromagnetic wave shield panel was completely decomposed, and only glass and mesh were recovered. The recovered glass and mesh were not damaged and could be recycled.
[0030]
【The invention's effect】
As described above in detail, according to the method for decomposing an organic resin for sealing of the present invention, the organic resin for sealing is obtained without adversely affecting the environment and without impairing the performance of the valuable material being sealed. Can be effectively decomposed and removed.
According to the present invention, valuable materials such as glass, filters, cells, and elements are recovered from wastes of electronic element sealing products such as laminated glass, tempered glass, plasma display panels, electromagnetic wave shield panels, solar cells, and semiconductors. Can be reused, reducing waste and effectively using resources.
Claims (3)
該封止用有機樹脂がエチレンビニルアセテート、ポリビニルアセタール、ポリビニルブチラール及びエポキシ系樹脂よりなる群から選ばれる１種又は２種以上であり、
該封止用有機樹脂を高温、高湿、高圧条件に設定可能な装置内に投入した後加熱し、その後加湿した後加圧することにより、該封止用有機樹脂を、温度１００〜２００℃、相対湿度１００％（１００％ＲＨ）、圧力１〜３０気圧（０．１〜３．０ＭＰａ）の高温、高湿、高圧条件とすることを特徴とする封止用有機樹脂の分解方法。A method for decomposing an organic resin for sealing, wherein the organic resin for sealing is maintained at a temperature of 100 ° C. or higher, a humidity of 100% RH or higher, and a pressure of 1 atm or higher, at a high temperature, high humidity, and high pressure.
The sealing organic resin is one or more selected from the group consisting of ethylene vinyl acetate, polyvinyl acetal, polyvinyl butyral, and epoxy resin,
The sealing organic resin is heated in an apparatus that can be set to high temperature, high humidity, and high pressure conditions, heated, then humidified, and then pressurized to bring the sealing organic resin to a temperature of 100 to 200 ° C., A method for decomposing an organic resin for sealing, characterized by high temperature, high humidity, and high pressure conditions of a relative humidity of 100% (100% RH) and a pressure of 1 to 30 atm (0.1 to 3.0 MPa) .
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| JP2001338108A JP4306167B2 (en) | 2001-11-02 | 2001-11-02 | Method for decomposing organic resin for sealing |
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| JP2001338108A JP4306167B2 (en) | 2001-11-02 | 2001-11-02 | Method for decomposing organic resin for sealing |
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| JP4306167B2 true JP4306167B2 (en) | 2009-07-29 |
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| EP2858125B1 (en) * | 2013-10-01 | 2021-07-21 | Korea Institute of Energy Research | Method for disassembling photovoltaic module |
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