JP2014019837A - Hot-melt sealing composition - Google Patents
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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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Abstract
Description
本発明は，フレームレス太陽電池モジュールのシール組成物に関し，特に２枚のガラス板を一定の隙間を持たせて重ね合わせた際に形成される４方向の端部をシールするホットメルトシール組成物に関する。 The present invention relates to a seal composition for a frameless solar cell module, and in particular, a hot melt seal composition that seals the ends in four directions formed when two glass plates are stacked with a certain gap therebetween. About.
従来，太陽電池用反応型ホットメルトシーリング材組成物として，ブチルゴムと，シリル化したアモルファスポリ−α−オレフィン重合体とを含有する太陽電池用反応型ホットメルトシーリング材組成物が提案されている（特許文献１）。 Conventionally, a reactive hot-melt sealing material composition for solar cells containing butyl rubber and a silylated amorphous poly-α-olefin polymer has been proposed as a reactive hot-melt sealing material composition for solar cells ( Patent Document 1).
また，複層ガラスおよび太陽電池パネルの端部を，簡易かつ効率的に封止でき，しかも，絶縁性，防水性，水蒸気バリア性，耐久性に優れるシーリング組成物として，ゴム成分とポリオレフィンとを含有し，前記ゴム成分は，ブチルゴムと，粘度平均分子量が５０万〜３００万のポリイソブチレンとを含有し，前記ゴム成分の配合割合が，前記ゴム成分および前記ポリオレフィンの総量１００重量部に対して，４０〜９０重量部であり，吸湿性化合物を，前記ゴム成分および前記ポリオレフィンの総量１００重量部に対して，０〜３０重量部含有することを特徴とする，シーリング組成物が提案されている（特許文献２）。 In addition, rubber components and polyolefins are used as sealing compositions that can easily and efficiently seal the edges of multi-layer glass and solar cell panels, and are excellent in insulation, waterproofness, water vapor barrier properties, and durability. And the rubber component contains butyl rubber and polyisobutylene having a viscosity average molecular weight of 500,000 to 3,000,000, and the blending ratio of the rubber component is 100 parts by weight based on the total amount of the rubber component and the polyolefin. 40 to 90 parts by weight, and a hygroscopic compound is contained in an amount of 0 to 30 parts by weight with respect to 100 parts by weight of the total amount of the rubber component and the polyolefin. (Patent Document 2).
しかし，特許文献１に示される太陽電池用反応型ホットメルトシーリング材組成物は，その用途が主としてフレームを有する太陽電池モジュール用に使用され，また評価されたものであり，本願発明が目的としているフレームレス太陽電池モジュールのガラス板端部をシールする用途にそのまま適用することが出来ないという課題がある。また該太陽電池用反応型ホットメルトシーリング材組成物は，ブチルゴムが主たるゴム成分であるため，高温における流れ性が不十分な場合があるという課題がある。 However, the reactive hot-melt sealing material composition for solar cells shown in Patent Document 1 is used and evaluated mainly for solar cell modules having a frame, and is the object of the present invention. There exists a subject that it cannot apply as it is to the use which seals the glass plate edge part of a frameless solar cell module. Moreover, since the reaction type hot-melt sealing material composition for solar cells is a main rubber component of butyl rubber, there is a problem that the flowability at high temperature may be insufficient.
また，特許文献２に示されるシーリング組成物は，ブチルゴムのほかにポリイソブチレンを含有するものであるが，ポリイソブチレンの粘度平均分子量は５０万〜３００万であって，どちらかというと該分子量は高めである。このため，特許文献２において開示された実施例（明細書段落０１３３の表１）には炭酸カルシウム等の充填剤を配合したものが具体的には示されてはおらず，該充填剤を配合すると該シーリング組成物は高粘度になる可能性があり，使用時に高温で溶融させることを考慮してもその流れ性が十分でない場合があるという課題がある。 Moreover, the sealing composition shown in Patent Document 2 contains polyisobutylene in addition to butyl rubber, and the viscosity average molecular weight of polyisobutylene is 500,000 to 3,000,000. It is high. For this reason, the example disclosed in Patent Document 2 (Table 1 of the specification paragraph 0133) does not specifically show that a filler such as calcium carbonate is blended, and when the filler is blended, The sealing composition may have a high viscosity, and there is a problem that the flowability may not be sufficient even when considering melting at a high temperature during use.
本発明が解決しようとする課題は，フレームレスの太陽電池モジュールのシール材に使用可能で，シール材の溶融温度において適度な流れ性を有し，絶縁性，防水性，水蒸気バリア性，耐久性に優れるホットメルトシール組成物を提供することにある。 The problem to be solved by the present invention is that it can be used as a sealing material for a frameless solar cell module, has an appropriate flowability at the melting temperature of the sealing material, and has insulating properties, waterproof properties, water vapor barrier properties, durability. An object of the present invention is to provide a hot melt seal composition having excellent resistance.
請求項１記載の発明は，重量平均分子量が１５〜２５万のポリイソブチレンと，重量平均分子量が３５〜４５万のポリイソブチレンと，重量平均分子量が８〜１０万のポリイソブチレンと，少なくとも生石灰またはゼオライトから成る吸湿剤と，シラン変性ポリオレフィンと，充填剤と，から成り，各ポリイソブチレンの重量平均分子量から求める数平均の分子量が１９万〜３０万であることを特徴とするホットメルトシール組成物である。 The invention according to claim 1 includes a polyisobutylene having a weight average molecular weight of 150,000 to 250,000, a polyisobutylene having a weight average molecular weight of 35 to 450,000, a polyisobutylene having a weight average molecular weight of 80 to 100,000, and at least quick lime or A hot melt seal composition comprising a hygroscopic agent comprising zeolite, a silane-modified polyolefin, and a filler, wherein the number average molecular weight determined from the weight average molecular weight of each polyisobutylene is 190,000 to 300,000. It is.
請求項２記載の発明は，吸湿剤はポリイソブチレン１００重量部に対して２０〜６０重量部含むことを特徴とする請求項１に記載のホットメルトシール組成物である。 The invention according to claim 2 is the hot melt seal composition according to claim 1, characterized in that the hygroscopic agent is contained in an amount of 20 to 60 parts by weight with respect to 100 parts by weight of polyisobutylene.
請求項３記載の発明は，シラン変性ポリオレフィンはポリイソブチレン１００重量部に対して１５〜４５重量部含むことを特徴とする請求項１または請求項２のいずれかに記載のホットメルトシール組成物である。 The invention according to claim 3 is the hot melt seal composition according to claim 1 or 2, wherein the silane-modified polyolefin contains 15 to 45 parts by weight with respect to 100 parts by weight of polyisobutylene. is there.
請求項４記載の発明は，充填剤は，ポリイソブチレン１００重量部に対して５０〜２００重量部含むことを特徴とする請求項１乃至請求項３のいずれかに記載のホットメルトシール組成物である。 The invention according to claim 4 is the hot melt seal composition according to any one of claims 1 to 3, characterized in that the filler contains 50 to 200 parts by weight with respect to 100 parts by weight of polyisobutylene. is there.
請求項５記載の発明は，充填剤は，タルク，カオリンクレー，およびカーボンブラックのいずれかより選択される少なくとも１から成ることを特徴とする請求項１乃至請求項４のいずれかに記載のホットメルトシール組成物である。 The invention according to claim 5 is characterized in that the filler is at least one selected from any of talc, kaolin clay, and carbon black. It is a melt seal composition.
本発明に係るホットメルトシール組成物は，重量平均分子量が異なるポリイソブチレンの混合物から成り，特に重量平均分子量が１５〜２５万のポリイソブチレンと，重量平均分子量が３５〜４５万のポリイソブチレンと，重量平均分子量が８〜１０万のポリイソブチレンとの混合物から成っていて，混合割合は各重量平均分子量から求める数平均の分子量が１９〜３０万と成るように配合すればよい。このため，原料となるポリイソブチレンの選択性が広く，手元にあるこれらのポリイソブチレンを各重量平均分子量から求めた数平均の分子量が１９〜３０万と成るように適宜調整することで，原料を効率良く使用することが可能になり，生産効率が高くなるという効果がある。また配合されたポリイソブチレンの分子量は従来のシーリング組成物と比較して低分子量であるため、高温での使用時に適度の流れ性を有していて施工作業性が良好であるという効果がある。また本発明は特に充填剤を含むものであるが，充填剤が配合された状態で，良好な絶縁性と防水性と水蒸気バリア性及び耐久性を有するという効果がある。 The hot melt seal composition according to the present invention comprises a mixture of polyisobutylenes having different weight average molecular weights, in particular, polyisobutylene having a weight average molecular weight of 150,000 to 250,000, polyisobutylene having a weight average molecular weight of 35 to 450,000, It is composed of a mixture with polyisobutylene having a weight average molecular weight of 80 to 100,000, and the mixing ratio may be blended so that the number average molecular weight obtained from each weight average molecular weight is 190 to 300,000. For this reason, the selectivity of the polyisobutylene used as a raw material is wide, and by appropriately adjusting these polyisobutylenes at hand so that the number average molecular weight obtained from each weight average molecular weight is 190 to 300,000, the raw material is adjusted. It can be used efficiently and has the effect of increasing production efficiency. Moreover, since the molecular weight of the blended polyisobutylene is lower than that of a conventional sealing composition, it has an effect that it has an appropriate flowability when used at a high temperature and has good workability. In addition, the present invention particularly includes a filler, but in the state where the filler is blended, there is an effect of having good insulating properties, waterproof properties, water vapor barrier properties, and durability.
以下本発明について詳細に説明する。 The present invention will be described in detail below.
本発明のホットメルトシール組成物は，重量平均分子量が１５〜２５万のポリイソブチレンと，重量平均分子量が３５〜４５万のポリイソブチレンと，重量平均分子量が８〜１０万のポリイソブチレンと，少なくとも生石灰またはゼオライトから成る吸湿剤と，シラン変性ポリオレフィンと，充填剤と，から成り，各ポリイソブチレンの重量平均分子量から求める数平均の分子量が１９万〜３０万であることを特徴とするホットメルトシール組成物であり，必要により，チクソ付与剤，希釈剤，粘着付与剤，耐熱補助剤、難燃剤，酸化防止剤等が配合される。ここでいう各ポリイソブチレンの重量平均分子量から求める数平均の分子量とは，配合された各ポリイソブチレンの分子量（重量平均分子量）の総合計値を，各ポリイソブチレンの分子数の総合計値で除した数値である。 The hot melt seal composition of the present invention comprises a polyisobutylene having a weight average molecular weight of 15 to 250,000, a polyisobutylene having a weight average molecular weight of 35 to 450,000, a polyisobutylene having a weight average molecular weight of 80 to 100,000, A hot melt seal comprising a moisture absorbent composed of quicklime or zeolite, a silane-modified polyolefin, and a filler, and having a number average molecular weight determined from the weight average molecular weight of each polyisobutylene of 190,000 to 300,000. It is a composition, and if necessary, a thixotropic agent, a diluent, a tackifier, a heat-resistant auxiliary agent, a flame retardant, an antioxidant and the like are blended. The number average molecular weight obtained from the weight average molecular weight of each polyisobutylene here is the total sum of the molecular weight (weight average molecular weight) of each blended polyisobutylene divided by the total sum of the number of molecules of each polyisobutylene. It is a numerical value.
ポリイソブチレン
本発明に使用されるポリイソブチレンは，重量平均分子量が１５〜２５万のイソブチレンの重合体と，重量平均分子量が３５〜４５万のイソブチレンの重合体と，重量平均分子量が８〜１０万のイソブチレンの重合体である。これらのポリイソブチレンは各ポリイソブチレンの重量平均分子量から求める数平均の分子量が１９万〜３０万となるように混合されるが，混合されたポリイソブチレンは優れた水蒸気バリア効果を有し，比較的低分子量であるため，高温で溶融させて使用する際に良好な流れ性がある。各ポリイソブチレンの重量平均分子量から求める数平均の分子量が１９万未満では，高温溶融時の流れ性が過剰となり，３０万超では高温溶融時の流れ性が不足する。市販の重量平均分子量が２０万のポリイソブチレンにはｏｐｐａｎｏｌＢ３０ＳＦ（商品名，ＢＡＳＦ社製）が，同重量平均分子量が４０万のポリイソブチレンにはｏｐｐａｎｏｌＢ５０ＳＦ（商品名，ＢＡＳＦ社製），同重量平均分子量が９万のポリイソブチレンにはｏｐｐａｎｏｌＢ１５ＳＦＮ（商品名，ＢＡＳＦ社製）がある。
Polyisobutylene The polyisobutylene used in the present invention comprises a polymer of isobutylene having a weight average molecular weight of 150,000 to 250,000, a polymer of isobutylene having a weight average molecular weight of 35 to 450,000, and a weight average molecular weight of 80 to 100,000. This is a polymer of isobutylene. These polyisobutylenes are mixed so that the number average molecular weight obtained from the weight average molecular weight of each polyisobutylene is 190,000 to 300,000, but the mixed polyisobutylene has an excellent water vapor barrier effect, Because of its low molecular weight, it has good flowability when melted at high temperatures. If the number average molecular weight obtained from the weight average molecular weight of each polyisobutylene is less than 190,000, the flowability at high temperature melting becomes excessive, and if it exceeds 300,000, the flowability at high temperature melting is insufficient. For commercial polyisobutylene having a weight average molecular weight of 200,000, opanol B30SF (trade name, manufactured by BASF), for polyisobutylene having the same weight average molecular weight of 400,000, oppanol B50SF (trade name, manufactured by BASF), the same weight average molecular weight There is oppanol B15SFN (trade name, manufactured by BASF).
吸湿剤
本発明に使用される吸湿剤は，少なくとも生石灰またはゼオライトから成り，複層ガラスの周囲を本発明であるホットメルトシール組成物でシールした際に，該周囲から複層ガラス内に進入する水分を吸着保持するために配合され，水分を吸着した際の重量増加率は，１０〜３０％のものが適していて，より好ましくは２０〜２５％である。１０％未満では十分な吸着性能を保持できず,３０％超では、吸湿性能が高いため保存安定性が不足する。特に配合される生石灰に関しては，ポリイソブチレンに対する分散性が良好な，粒子の表面を脂肪酸等で処理したものが適している。市販の生石灰としては，ＣＭＬ＃３１（商品名，表面脂肪酸処理生石灰，水分吸着時の重量増加率：２０％，近江化学工業製）が、市販のゼオライトとしては、ミズカシーブス５ＡＰ(商品名，水分吸着時の重量増加率：２４％，水澤化学製）がある。
Hygroscopic agent The hygroscopic agent used in the present invention is composed of at least quick lime or zeolite, and enters the multilayer glass from the periphery when the periphery of the multilayer glass is sealed with the hot melt seal composition of the present invention. It is blended for adsorbing and retaining moisture, and the weight increase rate when adsorbing moisture is suitably 10 to 30%, more preferably 20 to 25%. If it is less than 10%, sufficient adsorption performance cannot be maintained, and if it exceeds 30%, the moisture absorption performance is high and storage stability is insufficient. In particular, with respect to quicklime to be blended, those having good dispersibility with respect to polyisobutylene and having the surface of the particles treated with fatty acid or the like are suitable. Commercially available quicklime is CML # 31 (trade name, surface fatty acid-treated quicklime, weight increase rate upon moisture adsorption: 20%, manufactured by Omi Chemical Co., Ltd.), and commercially available zeolite is Mizuka Sieves 5AP (tradename, moisture adsorption). The weight increase rate at the time: 24%, manufactured by Mizusawa Chemical).
吸湿剤の配合量は，前記ポリイソブチレン１００重量部に対して２０〜６０重量部であり，より好ましくは３０〜５０重量部である。２０重量部以下では吸湿効果が不十分であり，６０重量部超では絶縁性が低下する。３０重量部以下では吸湿効果が不十分となる傾向があり，５０重量部超では絶縁性が低下する傾向にある。 The blending amount of the hygroscopic agent is 20 to 60 parts by weight, more preferably 30 to 50 parts by weight with respect to 100 parts by weight of the polyisobutylene. If it is 20 parts by weight or less, the hygroscopic effect is insufficient, and if it exceeds 60 parts by weight, the insulating property is lowered. If it is 30 parts by weight or less, the moisture absorption effect tends to be insufficient, and if it exceeds 50 parts by weight, the insulating property tends to decrease.
シラン変性ポリオレフィン
シラン変性ポリオレフィンは，シリル化したアモルファスポリ−α-オレフィン重合体である。シリル化前のアモルファス−α−オレフィン重合体としては，アタクチックポリプレピレン，アタクチックポリブテンー１などのホモポリマー，コポリマー；エチレン，プロピレン，ブチレンなどのコポリマーまたはターポリマーを挙げることができる。該シラン変性ポリオレフィンの市販品としてはｖｅｓｔｏｐｌａｓｔ２０６（粘度；５±１Ｐａ・ｓ／１９０℃，エポニックデグサ社製）、または、ｖｅｓｔｏｐｌａｓｔＥＰ２４０３（粘度；３±１Ｐａ・ｓ／１９０℃，エポニックデグサ社製）、がある。
Silane-modified polyolefin Silane-modified polyolefin is a silylated amorphous poly-α-olefin polymer. Examples of the amorphous α-olefin polymer before silylation include homopolymers and copolymers such as atactic polypropylene and atactic polybutene 1, and copolymers or terpolymers such as ethylene, propylene and butylene. Commercially available products of the silane-modified polyolefin include vestoplast 206 (viscosity: 5 ± 1 Pa · s / 190 ° C., manufactured by Eponic Degussa) or vestoplast EP2403 (viscosity: 3 ± 1 Pa · s / 190 ° C., manufactured by Eponic Degussa) There is.
シラン変性ポリオレフィンの配合量は，前記ポリイソブチレン１００重量部に対して１５〜４５重量部であり，より好ましくは２０〜４０重量部である。１５重量部以下では密着性が不良と成り，４５重量部超では高温溶融時の流れ性及び絶縁性が不十分となる。２０重量部以下では密着性が不良と成る傾向があり，４０重量部超では高温溶融時の流れ性及び絶縁性が不十分となる傾向がある。 The compounding quantity of silane modified polyolefin is 15-45 weight part with respect to 100 weight part of said polyisobutylene, More preferably, it is 20-40 weight part. If it is 15 parts by weight or less, the adhesion is poor, and if it exceeds 45 parts by weight, the flowability and insulation at high temperature melting are insufficient. If it is 20 parts by weight or less, the adhesion tends to be poor, and if it exceeds 40 parts by weight, the flowability and insulation at the time of high-temperature melting tend to be insufficient.
充填剤
本発明に使用する充填剤は，タルク，カオリンクレー，およびカーボンブラックのいずれかより選択される少なくとも１から成る。これらの充填剤は補強性を向上させる効果、および透湿性を向上させる効果があり，粒子表面がカップリング剤（ビニルシランまたは、アミノシラン）で処理されているもののほか未処理のものも使用できる。充填剤の平均粒子径は１ｎｍ〜１０００μｍであり，より好ましくは１０ｎｍ〜１００μｍである。
Filler The filler used in the present invention comprises at least one selected from any of talc, kaolin clay, and carbon black. These fillers have an effect of improving the reinforcing property and an effect of improving the moisture permeability, and those whose particle surfaces are treated with a coupling agent (vinylsilane or aminosilane) can also be used. The average particle size of the filler is 1 nm to 1000 μm, more preferably 10 nm to 100 μm.
充填剤の配合量は，前記ポリイソブチレン１００重量部に対して５０〜２００重量部であり，より好ましくは８０重量部〜１５０重量部である。５０重量部以下では補強効果が不十分であり，２００重量部超では密着性が不十分となる。８０重量部以下では補強効果と透湿性が不十分となる傾向に有り，１５０重量部超では密着性が不十分となる傾向がある。 The blending amount of the filler is 50 to 200 parts by weight, more preferably 80 to 150 parts by weight with respect to 100 parts by weight of the polyisobutylene. If it is 50 parts by weight or less, the reinforcing effect is insufficient, and if it exceeds 200 parts by weight, the adhesion is insufficient. If it is 80 parts by weight or less, the reinforcing effect and moisture permeability tend to be insufficient, and if it exceeds 150 parts by weight, the adhesion tends to be insufficient.
市販の炭酸カルシウムとしては，ＢＦ２００(商品名，平均粒子径５．５μｍ，備北粉化製)があり，タルクとしては，タルクＭＳ（商品名，平均粒子径２０μｍ，日本タルク社製），カオリンクレーとしては，ＳＴ−ＫＥ（商品名，ビニルシラン処理焼成カオリンクレー，平均粒子径２．２μｍ，白石カルシウム社製），カーボンブラックとして，旭サーマルカーボン（商品名，旭サーマル社製）やＭＡ１００（商品名，三菱化学製）がある。 Commercially available calcium carbonate includes BF200 (trade name, average particle size 5.5 μm, manufactured by Bihoku Powders), and talc includes talc MS (trade name, average particle size 20 μm, manufactured by Nippon Talc Co., Ltd.), Kaolin clay. As ST-KE (trade name, vinylsilane-treated calcined kaolin clay, average particle size 2.2 μm, manufactured by Shiraishi Calcium Co., Ltd.), carbon black, Asahi Thermal Carbon (trade name, manufactured by Asahi Thermal Co., Ltd.) and MA100 (trade name) , Manufactured by Mitsubishi Chemical).
以下，実施例及び比較例にて本出願に係るホットメルトシール組成物について具体的に説明する。 Hereinafter, the hot melt seal composition according to the present application will be specifically described with reference to Examples and Comparative Examples.
実施例１乃至実施例７
表１に示す配合にて，重量平均分子量２０万のポリイソブチレンとしてｏｐｐａｎｏｌＢ３０ＳＦを，同重量平均分子量が４０万のポリイソブチレンにはｏｐｐａｎｏｌＢ５０ＳＦを，同重量平均分子量が９万のポリイソブチレンにはｏｐｐａｎｏｌＢ１５ＳＦＮを，吸湿剤としてＣＭＬ＃３１またはミズカシーブス５ＡＰを，充填剤としてタルクＭＳ，旭サーマルカーボン，またはカオリンクレーとしてＳＴ−ＫＥを，炭酸カルシウムとしてＢＦ２００を，シラン変性ポリオレフィンとしてｖｅｓｔｏｐｌａｓｔ２０６またはｖｅｓｔｏｐｌａｓｔＥＰ２４０３を使用し，試験用ニーダー（１Ｌ）で１６０℃に加熱しながら混練し，実施例１乃至実施例５を得た。
Example 1 to Example 7
In the formulation shown in Table 1, opanol B30SF is used as polyisobutylene having a weight average molecular weight of 200,000, opanol B50SF is used for polyisobutylene having the same weight average molecular weight of 400,000, and oppanol B15SFN is used for polyisobutylene having the same weight average molecular weight of 90,000, A test kneader using CML # 31 or Mizuka Sieves 5AP as a hygroscopic agent, talc MS, Asahi thermal carbon as filler, ST-KE as kaolin clay, BF200 as calcium carbonate, bestplast 206 or bestplast EP2403 as silane-modified polyolefin. Kneading while heating to 160 ° C. at (1 L), Examples 1 to 5 were obtained.
比較例１乃至比較例７
表１に示す配合にて，実施例１乃至実施例７と同様の方法で混練し，比較例１乃至比較例７を得た。
Comparative Examples 1 to 7
The compositions shown in Table 1 were kneaded in the same manner as in Examples 1 to 7, and Comparative Examples 1 to 7 were obtained.
評価項目および評価方法Evaluation items and evaluation methods
透湿度及び透湿飽和時間
実施例１乃至実施例７及び比較例１乃至比較例７のホットメルトシール組成物を０．７ｍｍ厚みに調整した試験片について，ＪＩＳＫ７１２９：２００８プラスチックフィルム及びシート−水蒸気透過度の求め方（機器測定法）の赤外線センサ法（付属書Ｂ）に準拠し，透過セルの温度８５℃湿度１００％の条件で，透湿度を測定した。９ｇ／ｍｍ２・ｄａｙ以下を○と評価し，これを越えるものを×とした。また一定の透湿度に到るまでの時間を透湿飽和時間（時間）として求めた。４０時間以上を○と評価し，４０時間未満を×とした。
Moisture permeability and moisture permeability saturation time JISK7129: 2008 plastic film and test pieces prepared by adjusting the hot melt seal compositions of Examples 1 to 7 and Comparative Examples 1 to 7 to 0.7 mm thickness In accordance with the infrared sensor method (Appendix B) of the sheet-water vapor permeability calculation method (apparatus measurement method), the moisture permeability was measured under the conditions of a temperature of the transmission cell of 85 ° C. and a humidity of 100%. A value of 9 g / mm 2 · day or less was evaluated as ◯, and a value exceeding this value was rated as x. Further, the time until reaching a certain moisture permeability was determined as moisture permeability saturation time (hour). 40 hours or more were evaluated as “good”, and less than 40 hours were evaluated as “x”.
吸湿性
実施例１乃至実施例７及び比較例１乃至比較例７のホットメルトシール組成物を１０ｍｍ×１００ｍｍ×０．７ｍｍ厚みに調整した試験片を，４０℃９０％ＲＨに１４日間放置した際の重量変化率を測定した。重量変化率が２％以上を○と評価し，２％未満を×とした。
When the specimens prepared by adjusting the hot melt seal compositions of Examples 1 to 7 and Comparative Examples 1 to 7 to a thickness of 10 mm × 100 mm × 0.7 mm were left at 40 ° C. and 90% RH for 14 days. The weight change rate of was measured. A weight change rate of 2% or more was evaluated as ○, and less than 2% was evaluated as ×.
せん断密着強度及びせん断密着破壊状態
２０ｍｍ×５０ｍｍ×３ｍ厚のガラス板に実施例１乃至実施例７及び比較例１乃至比較例７のホットメルトシール組成物を１４０〜１６０℃に加熱して厚さ０．７ｍｍ厚で塗付し，直ちに同形状のガラス板を巾１０ｍｍでオーバーラップさせるように載置する。１５０℃５分間真空脱気後，５５ｋＰａ圧力で１５分間プレスする。その後さらに２３℃２日間養生後，引張速度２０ｍｍ／分で２枚のガラス板を引張り，破壊強度を測定し，単位面積あたりの破壊強度をせん断密着強度（Ｎ／ｍｍ２）とした。０．４Ｎ／ｍｍ２以上を○と評価し０．４Ｎ／ｍｍ２未満を×とした。 また，破壊時の破壊面を目視で評価し，ホットメルトシール組成物の１００％凝集破壊を○と評価し，これ以外を×とした。
Shear adhesion strength and shear adhesion failure state 20 mm x 50 mm x 3 m thick glass plates of Examples 1 to 7 and Comparative Examples 1 to 7 were heated to 140-160 ° C to obtain a thickness. Apply with a thickness of 0.7 mm, and immediately place a glass plate of the same shape to overlap with a width of 10 mm. After degassing at 150 ° C for 5 minutes, press at 55 kPa pressure for 15 minutes. Thereafter, after further curing at 23 ° C. for 2 days, two glass plates were pulled at a tensile rate of 20 mm / min, the fracture strength was measured, and the fracture strength per unit area was defined as shear adhesion strength (N / mm 2 ). 0.4 N / mm 2 or more was evaluated as “good”, and less than 0.4 N / mm 2 was evaluated as “x”. Moreover, the fracture surface at the time of fracture was evaluated visually, 100% cohesive fracture of the hot melt seal composition was evaluated as “good”, and the others were marked as “x”.
１８０度はく離密着強度及び１８０度はく離破壊状態
１８０ｍｍ×３０ｍｍ×３ｍｍ厚のガラス板に実施例１乃至実施例７及び比較例１乃至比較例７のホットメルトシール組成物を１４０〜１６０℃に加熱して厚さ０．７ｍｍで塗付し，直ちに２５ｍｍ×４００ｍｍ×１ｍｍの綿布を張り付ける。１５０℃５分間真空脱気後，５５ｋＰａ圧力で１５分間プレスする。その後さらに２３℃２日間養生した後，引張速度１００ｍｍ／分で綿布をガラス板に対して１８０度方向に引っ張り，綿布がはく離する際の強度を測定し，単位長あたりの強度を１８０度はく離密着強度（Ｎ／ｍｍ）とした。１．５Ｎ／ｍｍ以上を○と評価し，１．５Ｎ／ｍｍ未満を×とした。また，はく離時のはく離面を目視で評価し，ホットメルトシール組成物の５０％以上の凝集破壊を○と評価し，これ以外を×とした。
The hot melt seal compositions of Examples 1 to 7 and Comparative Examples 1 to 7 were heated to 140 to 160 ° C. on a glass plate having a 180 ° peel adhesion strength and a 180 ° peel failure state of 180 mm × 30 mm × 3 mm thickness. Apply at a thickness of 0.7 mm, and immediately apply a 25 mm x 400 mm x 1 mm cotton cloth. After degassing at 150 ° C for 5 minutes, press at 55 kPa pressure for 15 minutes. After further curing at 23 ° C. for 2 days, the cotton cloth was pulled 180 ° with respect to the glass plate at a pulling speed of 100 mm / min. The strength when the cotton cloth was peeled off was measured, and the strength per unit length was peeled off by 180 degrees. Strength (N / mm) was used. 1.5 N / mm or more was evaluated as ◯, and less than 1.5 N / mm was evaluated as x. Moreover, the peeling surface at the time of peeling was evaluated visually, 50% or more of the cohesive failure of the hot melt seal composition was evaluated as “good”, and the others were marked as “x”.
ラミネート性
ガラス板上に実施例１乃至実施例７及び比較例１乃至比較例７のホットメルトシール組成物を１４０〜１６０℃に加熱して厚さ０．７ｍｍで塗付し，１４５℃で５分間脱気後，５５ｋＰａ圧力で１５分間プレスし，その状態を目視で観察した。ホットメルトシール組成物に気泡の混入がないものを○と評価し，気泡があるものを×とした。
The hot melt seal compositions of Examples 1 to 7 and Comparative Examples 1 to 7 were heated to 140 to 160 ° C. and applied to a thickness of 0.7 mm on a laminate glass plate, and 5 ° C. at 145 ° C. After deaeration for 5 minutes, pressing was performed at 55 kPa pressure for 15 minutes, and the state was visually observed. The hot melt seal composition was evaluated as “Good” when no bubbles were mixed, and “X” when the bubbles were present.
耐熱フロー性
ガラス板上に１．４ｍｍ×１．４ｍｍ×１．４ｍｍに成形した実施例１乃至実施例７及び比較例１乃至比較例７のホットメルトシール組成物を載置し，１５０℃１時間後のフローを測定した。１０ｍｍ以上２０ｍｍ以下を○と評価し，１０ｍｍ未満を△，２０ｍｍ超を×とした。
The hot-melt seal compositions of Examples 1 to 7 and Comparative Examples 1 to 7 molded to 1.4 mm × 1.4 mm × 1.4 mm were placed on a heat-resistant flowable glass plate, and 150 ° C. 1 The flow after time was measured. 10 mm or more and 20 mm or less were evaluated as ◯, less than 10 mm as Δ, and more than 20 mm as X.
絶縁性
ＪＩＳＫ６９１１の５．１３抵抗率に準拠し，実施例１乃至実施例７及び比較例１乃至比較例７の体積抵抗率（Ω・ｃｍ）を測定した。１０１１Ω・ｃｍ以上を○とし，１０１１Ω・ｃｍ未満を×とした。
The volume resistivity (Ω · cm) of Examples 1 to 7 and Comparative Examples 1 to 7 was measured in accordance with 5.13 resistivity of insulating JISK6911. 10 11 Ω · cm or more was rated as ◯, and less than 10 11 Ω · cm was rated as x.
評価結果
評価結果を表２に示す。実施例１乃至実施例７はすべての評価項目が○であった。
Evaluation results The evaluation results are shown in Table 2. In Examples 1 to 7, all evaluation items were “good”.
Claims (5)
The hot-melt seal composition according to any one of claims 1 to 4, wherein the filler comprises at least one selected from talc, kaolin clay, and carbon black.
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| JP2016089098A (en) * | 2014-11-07 | 2016-05-23 | アイカ工業株式会社 | Yellowing-resistant hot melt sealing composition |
| JP2016196537A (en) * | 2015-04-02 | 2016-11-24 | アイカ工業株式会社 | Hot melt sealing composition |
| JP2017179353A (en) * | 2016-03-29 | 2017-10-05 | アイカ工業株式会社 | Hot melt seal composition |
| JP2018080213A (en) * | 2016-11-14 | 2018-05-24 | アイカ工業株式会社 | Adhesive composition and adhesive sheet |
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| WO2011047185A1 (en) * | 2009-10-14 | 2011-04-21 | Adco Products, Inc. | Edge sealant composition with reactive or unsaturated polyolefins |
| WO2011068597A1 (en) * | 2009-10-14 | 2011-06-09 | Adco Products, Inc. | Use of calcium oxide as a water scavenger in solar module applications |
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| WO2011047185A1 (en) * | 2009-10-14 | 2011-04-21 | Adco Products, Inc. | Edge sealant composition with reactive or unsaturated polyolefins |
| WO2011068597A1 (en) * | 2009-10-14 | 2011-06-09 | Adco Products, Inc. | Use of calcium oxide as a water scavenger in solar module applications |
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| Publication number | Priority date | Publication date | Assignee | Title |
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| JP2016089098A (en) * | 2014-11-07 | 2016-05-23 | アイカ工業株式会社 | Yellowing-resistant hot melt sealing composition |
| JP2016196537A (en) * | 2015-04-02 | 2016-11-24 | アイカ工業株式会社 | Hot melt sealing composition |
| JP2017179353A (en) * | 2016-03-29 | 2017-10-05 | アイカ工業株式会社 | Hot melt seal composition |
| JP2018080213A (en) * | 2016-11-14 | 2018-05-24 | アイカ工業株式会社 | Adhesive composition and adhesive sheet |
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