JP6444403B2 - ゴム系感圧接着剤発泡体 - Google Patents
ゴム系感圧接着剤発泡体 Download PDFInfo
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- JP6444403B2 JP6444403B2 JP2016531819A JP2016531819A JP6444403B2 JP 6444403 B2 JP6444403 B2 JP 6444403B2 JP 2016531819 A JP2016531819 A JP 2016531819A JP 2016531819 A JP2016531819 A JP 2016531819A JP 6444403 B2 JP6444403 B2 JP 6444403B2
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- Prior art keywords
- sensitive adhesive
- pressure sensitive
- foam
- acrylate
- less
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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Classifications
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Description
本願は、その全ての開示内容が参照によって本願に組み込まれる、2013年8月1日に出願された欧州特許出願第13178961.2号の利益を主張するものである。
本開示は、一般に感圧接着剤(PSA)発泡体の分野に関し、具体的にゴム系感圧接着剤発泡体及びゴム系感圧接着剤アセンブリの分野に関する。本開示はまた、かかる感圧接着剤発泡体及びアセンブリを製造する方法並びにその使用方法に関する。
接着剤は、様々なマーキング、保持、保護、封止、及び遮蔽目的のために使用されている。接着テープは、一般に、裏材又は基材、及び接着剤を含む。多くの用途で特に好ましい接着剤の一種は、感圧接着剤に代表される。感圧接着剤類(PSA)は、以下を含む特性を有することが、当業者に周知である。(1)強力かつ恒久的粘着、(2)指圧を超えない圧力での接着、(3)被着体への十分な保持力、及び(4)十分な粘着強度。
一態様によると、本開示は、ゴム系エラストマー材と、少なくとも1つの炭化水素粘着付与剤と、多官能(メタ)アクリレート化合物の群から選択される架橋添加剤と、を含む感圧接着剤発泡体に関する。
a)ゴム系エラストマー材;少なくとも1つの炭化水素粘着付与剤;多官能(メタ)アクリレート化合物の群から選択される架橋添加剤;場合により、好ましくは膨張性ミクロスフェア、グラスバブルズ、ガス空洞体、及びこれらの任意の組み合わせ若しくは混合物からなる群から選択される充填材料;場合により、少なくとも1つの可塑剤、特に、ポリイソブチレン可塑剤、を配合し、感圧接着剤発泡体配合物を形成する工程、及び、
b)好ましくは化学線、より好ましくは電子線照射により感圧接着剤発泡体配合物を架橋する、任意に採用される工程、を備える。
第一態様によると、本開示は、ゴム系エラストマー材と、少なくとも1つの炭化水素粘着付与剤と、多官能(メタ)アクリレート化合物の群から選択される架橋添加剤と、を含む感圧接着剤発泡体に関する。
H2C=C(R1)−(CO)−O−R2−[O−(CO)−(R1)C=CH2]n
[式中、R1は、水素又はメチルであり、nは、1、2、3、又は4であり、R2は、アルキレン、アリーレン、ヘテロアルキレン、又はこれらの任意の組み合わせである。]
a)前記感圧接着剤発泡体の重量に対して、20重量%〜80重量%、30重量%〜70重量%、又は40重量%〜60重量%の前記ゴム系エラストマー材、
b)前記感圧接着剤発泡体の重量に対して、5重量%〜60重量%、5重量%〜50重量%、10重量%〜45重量%、又は15重量%〜45重量%の前記炭化水素粘着付与剤、
c)多官能(メタ)アクリレート化合物からなる群から選択され、前記感圧接着剤発泡体の重量に対して、0.1重量%〜10重量%、0.5重量%〜8重量%、1重量%〜6重量%、又は2重量%〜5重量%の架橋添加剤、
d)前記感圧接着剤発泡体の重量に対して、1重量%〜40重量%、2重量%〜30重量%、5重量%〜30重量%、又は10重量%〜25重量%の、任意に用いられる前記ポリイソブチレン可塑剤、
e)好ましくは膨張性ミクロスフェア及びグラスバブルズからなる群から選択され、前記感圧接着剤発泡体の重量に対して、2重量%〜30重量%、2重量%〜20重量%、又は2重量%〜15重量%の、任意に用いられる充填材料、
f)熱安定剤、紫外線安定剤、プロセス安定剤からなる群から選択され、前記感圧接着剤発泡体の重量に対して、0.05重量%〜2重量%の、任意に用いられる安定剤、
g)好ましくは、カーボンブラック、アエロジル、及びケイ酸塩からなる群から選択され、前記感圧接着剤発泡体の重量に対して、0.1重量%〜5重量%の、任意に用いられる充填添加剤、を含む。
(a)イソ−オクチル(メタ)アクリレート、2−エチルへキシル(メタ)アクリレート、2−プロピルヘプチル(メタ)アクリレート、ブチルアクリレートからなる群から好ましくは選択される主要モノマーとしての直鎖又は分枝鎖アルキル(メタ)アクリレートエステル、及び場合により、
(b)エチレン性不飽和基、好ましくは、前記アクリレート主要モノマーと共重合性である強化モノエチレン性不飽和モノマーを有する第2のモノマー。
a)前記主要なモノマーが、イソ−オクチル(メタ)アクリレート、2−エチルへキシル(メタ)アクリレート、2−プロピルヘプチル(メタ)アクリレート、ブチルアクリレートからなる群から好ましくは選択される、50〜99.5重量パーセント又は60〜90重量パーセントの、第1の/主要なモノマーとしての直鎖又は分枝鎖アルキル(メタ)アクリレートエステル、場合により、
b)1.0〜50重量パーセント、3.0〜40重量パーセント、5.0〜35重量パーセント、又は更には10〜30重量パーセントの、エチレン性不飽和基を有する前記第2のモノマー、好ましくはエチレン性不飽和基を有する第2の非極性モノマー、場合により、
c)0.1〜15重量パーセント、0.5〜15重量パーセント、1.0〜10重量パーセント、2.0〜8.0重量パーセント、2.5〜6.0重量パーセント、又は更には3.0〜6.0重量パーセントの極性モノマー、好ましくは極性アクリレート、及び場合により、
d)粘着付与樹脂を含み、
重量パーセントは、重合性材料の総重量を基準とする。
a)主要なモノマーが、イソ−オクチル(メタ)アクリレート、2−エチルへキシル(メタ)アクリレート、2−プロピルヘプチル(メタ)アクリレート、ブチルアクリレートからなる群から好ましくは選択される、第1の/主要なモノマーとしての直鎖又は分枝鎖アルキル(メタ)アクリレートエステル、場合により、
b)1.0〜50重量パーセント、3.0〜40重量パーセント、5.0〜35重量パーセント、又は更には10〜30重量パーセントの、エチレン性不飽和基を有する第2のモノマー、好ましくはエチレン性不飽和基を有する第2の非極性モノマー、場合により、
c)0.1〜15重量パーセント、0.5〜15重量パーセント、1.0〜10重量パーセント、2.0〜8.0重量パーセント、2.5〜6.0重量パーセント、又は更には3.0〜6.0重量パーセントの第1の極性モノマー、好ましくは極性アクリレート、場合により、
d)第2の極性モノマー、好ましくは極性非アクリレートモノマー、及び場合により、
e)粘着付与樹脂を含み、
重量パーセントは、重合性材料の総重量を基準とする。
a)ゴム系エラストマー材;少なくとも1つの炭化水素粘着付与剤;多官能(メタ)アクリレート化合物の群から選択される架橋添加剤;場合により、好ましくは膨張性ミクロスフェア、グラスバブルズ、ガス空洞体、及びこれらの任意の組み合わせ若しくは混合物からなる群から選択される充填材料;場合により、少なくとも1つの可塑剤、特に、ポリイソブチレン可塑剤、を配合し、感圧接着剤発泡体配合物を形成する工程、
b)好ましくは化学線、より好ましくは電子線照射により感圧接着剤発泡体配合物を架橋する、任意に採用される工程、を備える。
H2C=C(R1)−(CO)−O−R2−[O−(CO)−(R1)C=CH2]n
[式中、R1は、水素又はメチルであり、nは、1、2、3、又は4であり、R2は、アルキレン、アリーレン、ヘテロアルキレン、又はこれらの任意の組み合わせである。]
a)前記感圧接着剤発泡体の重量に対して、20重量%〜80重量%、30重量%〜70重量%、又は40重量%〜60重量%の前記ゴム系エラストマー材、
b)前記感圧接着剤発泡体の重量に対して、5重量%〜60重量%、5重量%〜50重量%、10重量%〜45重量%、又は15重量%〜45重量%の前記炭化水素粘着付与剤、
c)多官能(メタ)アクリレート化合物からなる群から選択され、前記感圧接着剤発泡体の重量に対して、0.1重量%〜10重量%、0.5重量%〜8重量%、1重量%〜6重量%、又は2重量%〜5重量%の架橋添加剤、
d)前記感圧接着剤発泡体の重量に対して、1重量%〜40重量%、2重量%〜30重量%、5重量%〜30重量%、又は10重量%〜25重量%の、任意に用いられる前記ポリイソブチレン可塑剤、
e)好ましくは膨張性ミクロスフェア及びグラスバブルズからなる群から選択され、前記感圧接着剤発泡体の重量に対して、2重量%〜30重量%、2重量%〜20重量%、又は2重量%〜15重量%の、任意に用いられる充填材料、
f)熱安定剤、紫外線安定剤、プロセス安定剤からなる群から選択され、前記感圧接着剤発泡体の重量に対して、0.05重量%〜2重量%の、任意に用いられる安定剤、
g)好ましくは、カーボンブラック、アエロジル、及びケイ酸塩からなる群から選択され、前記感圧接着剤発泡体の重量に対して、0.1重量%〜5重量%の、任意に用いられる充填添加剤、を含む、感圧接着剤発泡体である。
a)ゴム系エラストマー材;少なくとも1つの炭化水素粘着付与剤;多官能(メタ)アクリレート化合物の群から選択される架橋添加剤;場合により、好ましくは膨張性ミクロスフェア、グラスバブルズ、ガス空洞体、及びこれらの任意の組み合わせ若しくは混合物からなる群から選択される充填材料;場合により、少なくとも1つの可塑剤、特に、ポリイソブチレン可塑剤、を配合し、感圧接着剤発泡体配合物を形成する工程、
b)好ましくは化学線、より好ましくは電子線照射により前記感圧接着剤発泡体配合物を架橋する、任意に採用される工程、を備える、製造方法である。
TGA試験方法
TGA(熱重量分析)測定は、Texas Instruments製Q5000IR装置を用いて行う。サンプルを白金皿に秤量し、オートサンプラーを用いて装置のオーブンに置く。オーブンの窒素の流量は、25mL/分で、残部の窒素の流量は、10mL/分である。温度は30℃で平衡化し、15分間保持される。その後、60℃/分の傾きで90℃まで昇温する。次に、90℃を30分間保持する。次の工程で、60℃/分の傾きで120℃まで昇温する。120℃を60分間保持する。90℃で30分間(VOC分析)及び120℃で60分間(FOG分析)の重量減少を記録する。
原材料サンプルのガス放出の測定は、選択した原料10gをアルミニウムカップに0.1mgの精度で秤量することによって、実施する。この工程の前に、0.1mgの同じ精度でアルミニウムカップを先に秤量する。秤量したサンプルを強制エアオーブンに160℃で2時間置く。サンプルをオーブンから一旦取り出し、周囲温度(23℃+/−2℃)で放冷し、詰めたアルミニウムカップを再度秤量する。オーブン乾燥前後のサンプルの重量減少を計算し、%単位で記録する。
VDA試験方法278は、自動車の内装の製造に使用される非金属トリム部分からの有機物放散の決定のために使用される試験方法である(VDAは、「Verband der Automobilindustrie」の略である。the German Association of Automobilists)。試験方法により、放散された有機化合物を以下の2つのグループに分類する。
VOC値−最大n−C20揮発性及び半揮発性化合物の合計、
FOG値−n−C16〜n−C32半揮発性及び重い化合物の合計。
−VOC分析。これは、サンプルを90℃で30分間、脱着し、最大n−C20のVOCを抽出することに関連する。この後、サンプル1g当たりトルエン当量μgとして各化合物の半定量分析を行う。
−FOG分析。これは、サンプルを120℃で60分間、脱着し、最大n−C16〜n−C32に及ぶ半揮発性化合物を抽出することに関連する。この後、サンプル1g当たりヘキサデカン当量μgとして各化合物の半定量分析を行う。
本開示に従う、10mmの幅及び120mm超の長さを有する多層感圧接着剤アセンブリストリップを、サンプル材料から縦方向に切り取る。
周囲室温(23℃+/−2℃及び50%+/−5%相対湿度)で試験を実行する。試験片を12.7mm×25.4mmの寸法を有するように切断する。次に、試験片の片面からライナ−を除去し、接着剤を25.4mm×50mm×厚さ1mmの寸法を有し、重り用の穴を有するアルミニウムプレートに接着させる。その後、第2のライナーを試験片から除去し、この試験片を有する小さなパネルを50mm×50mm×2mmの寸法を有する試験パネル(ステンレス鋼)の短辺に貼付する。
試験は70℃で行う。試験片を12.7mm×25.4mmの寸法を有するように切断する。次に、試験片の片面からライナ−を除去し、接着剤を25.4mm×50mm×厚さ1mmの寸法を有し、重り用の穴を有するアルミニウムプレートに接着させる。その後、第2のライナーを試験片から除去し、この試験片を有する小さなパネルを50mm×50mm×2mmの寸法を有する試験パネル(ステンレス鋼)の短辺に貼付する。
FS(「発泡体分裂」は、発泡体コアの凝集破壊を示す)
2B(「2−接着」は、外皮及び発泡体コアの剥離、即ち外皮/プライマー又はプライマー/外皮のそれぞれの破損を示す)
使用した原材料及び市販の接着テープを以下の表1にまとめる。
接着発泡体テープ調製
混練容積が370cm3のBrabender Plastograph混練機(Brabender GmbH製、デュースブルグ、ドイツ)を用いて、ホットメルト工程で、ゴム系エラストマー材としてオレフィン系ブロックコポリマーを含む感圧接着剤発泡体を調製する。ブロモ−ブチルゴムをベースにした感圧接着剤発泡体は、混練容積が250cm3のHaake Polylab OS混練機内でホットメルト配合される。
次に、Electron Crosslinking AB(ネーレン、ドイツ)製の80〜300kVの電子線装置を用いて、発泡体シートに電子線を放射する。電子線放射前に、トップライナーを除去する。次に、発泡体シートに両面から電子線を照射する。発泡体をベースにするオレフィン系ブロックコポリマーの場合、265kVの加速電圧を使用し、860〜900g/m2発泡体シートに最良のイオン化特性を提供する。このような発泡体シートに各面から照射量100kGyを使用して照射する。窒素間隙は30mmに調整する。
本発明による感圧接着剤アセンブリを提供するために、電子線照射した発泡体シートをPrimer94(3M Deutschland GmbH製、ドイツ)の薄層又は電子線硬化性プライマーを用いて下塗りする。溶剤系プライマーP94を使用する場合、溶剤を蒸発した後、アクリル系転写接着剤468MPの層を室温(23℃+/−2℃)で発泡体シート上に積層する。外皮/コア/外皮構造が所望される場合、発泡体コアの第2の側面に対して、この工程を繰り返す。
第1工程で、発泡体コアを上述したように製造する。合計14個の異なる発泡体コア(E1〜E14)及び1つの比較用発泡体コア(C1)を製造する。次に、これらのコア発泡体にアクリル系転写テープを積層し、静的剪断及び剥離試験に有用な外皮/コア/外皮感圧接着剤アセンブリを提供する。
TGA試験結果
いくつかの発泡体原料及び市販の発泡体に関して、熱重量分析(TGA)を行う。結果を表6に記載する。
選択された発泡体原料が低VOC感圧接着剤発泡体を得ることに貢献する場合、実験室規模の迅速な評価に関するオーブンガス放出試験が可能である。この試験の結果を表7に示し、重量減少%として記録する。
VOC値及びFOG値を決定するために、いくつかの発泡体コアシートに対して、VDA 278による測定を行う。結果を表8に記載する。
実施例の室温及び70℃での90°剥離試験結果及び静的剪断試験結果を表9に示す。
Claims (5)
- 感圧接着剤発泡体を含むコア層と、第2の感圧接着剤を含む発泡体ではない外皮層と、を含む感圧接着剤アセンブリであって、
前記感圧接着剤発泡体が、
a)前記感圧接着剤発泡体の重量に対して、30重量%〜70重量%のゴム系エラストマー材、
b)前記感圧接着剤発泡体の重量に対して、10重量%〜45重量%の炭化水素粘着付与剤、
c)多官能(メタ)アクリレート化合物の群から選択され、前記感圧接着剤発泡体の重量に対して、0.1重量%〜10重量%の架橋添加剤、
d)前記感圧接着剤発泡体の重量に対して、1重量%〜40重量%のポリイソブチレン可塑剤、
e)前記感圧接着剤発泡体の重量に対して、2重量%〜30重量%の、ミクロスフェア、膨張性ミクロスフェア、ガラスビーズ、ガラスミクロスフェア、グラスバブルズ、及びこれらの任意の組み合わせ若しくは混合物からなる群から選択される充填材料、
f)熱安定剤、紫外線安定剤及びプロセス安定剤からなる群から選択され、前記感圧接着剤発泡体の重量に対して、0.05重量%〜2重量%の、任意に用いられる安定剤、及び、
g)カーボンブラック、アエロジル、及びケイ酸塩からなる群から選択され、前記感圧接着剤発泡体の重量に対して、0.1重量%〜5重量%の、任意の用いられる充填添加剤、
を含む、感圧接着剤アセンブリ。 - 前記第2の感圧接着剤がポリアクリレートを含む、請求項1に記載の感圧接着剤アセンブリ。
- 第3の感圧接着剤を含む第2の外皮層を更に含み、前記第3の感圧接着剤がポリアクリレートを含む、請求項2に記載の感圧接着剤アセンブリ。
- 前記感圧接着剤発泡体が電子線照射により架橋される、請求項1に記載の感圧接着剤アセンブリ。
- 前記充填材料がグラスバブルズを含む、請求項1に記載の感圧接着剤アセンブリ。
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EP13178961.2 | 2013-08-01 | ||
EP13178961.2A EP2832780B1 (en) | 2013-08-01 | 2013-08-01 | Rubber-Based Pressure Sensitive Adhesive Foam |
PCT/US2014/048621 WO2015017414A1 (en) | 2013-08-01 | 2014-07-29 | Rubber-based pressure sensitive adhesive foam |
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EP (1) | EP2832780B1 (ja) |
JP (1) | JP6444403B2 (ja) |
KR (1) | KR20160037214A (ja) |
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-
2013
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2014
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- 2014-07-29 WO PCT/US2014/048621 patent/WO2015017414A1/en active Application Filing
- 2014-07-29 US US14/905,524 patent/US10106708B2/en active Active
- 2014-07-29 KR KR1020167005123A patent/KR20160037214A/ko not_active Application Discontinuation
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EP2832780B1 (en) | 2019-09-25 |
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EP2832780A1 (en) | 2015-02-04 |
WO2015017414A1 (en) | 2015-02-05 |
JP2016527367A (ja) | 2016-09-08 |
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US20160152871A1 (en) | 2016-06-02 |
US10106708B2 (en) | 2018-10-23 |
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