JP2018522094A - 赤外放射で硬化可能な潜在性2液型ポリウレタン接着剤 - Google Patents
赤外放射で硬化可能な潜在性2液型ポリウレタン接着剤 Download PDFInfo
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Abstract
【選択図】なし
Description
以下の実施例は、開示された組成物を説明するために提供されるが、その範囲を限定することを意図するものではない。全ての部及び割合は、別段の指示がない限り、重量によるものである。
ポリオールAは、1000g/molの分子量の平均分子量及び約55mg KOH/gのOH数を有する、ポリプロピレンホモポリマーである。
ポリオールBは、1800g/molの分子量の平均分子量及び約35mg KOH/gのOH数を有する、公称的に三官能性のグリセリン開始エチレンオキシド系プロポキシ化トリオールである。
ポリオールCは、280のヒドロキシル価、7の官能価、1400の分子量、及び200の当量を有する、スクロース開始オキシプロピレンオキシエチオレン(oxyethyolene)ポリオールである、多官能性ポリオールである。
1,4−ブタンジオール。
アミノ化ポリエーテルは、Huntsman CorporationによってJeffamine(商標)D−400として販売される、第1級アミン基において末端化される、400g/molの二官能性ポリ(プロピレンオキシド)である。
脂肪族ポリイソシアネートは、193のイソシアネート当量を有する、ヘキサメチレンジイソシアネートに基づく市販の生成物である(Bayer Material SciencesからのDesmodur(商標)N3400)。
液体MDIは、約2.2のイソシアネート官能価及び約143の当量を有する市販の変性MDI生成物である。
プレポリマーを、ポリオールA(17.74部)、約2000の分子量及び約1000のヒドロキシル当量を有する公称的に二官能性のポリ(プロピレンオキシド)(12.09部)、「液体MDI」生成物(27.5部)、ならびに可塑剤((18.07部)を組み合わせ、得られる混合物を一定のイソシアネート含有量になるまで加熱して、可塑化プレポリマーを形成することによって作製する。可塑化プレポリマーを、次いで、主に4,4’−異性体を含有し、約125のイソシアネート当量(5.08部)及びカーボンブラック(19部)を有する、純MDI生成物とブレンドする。
触媒Aは、市販のジオクチルスズチオグリコレート触媒である。それは、本質的に100%の活性材料を含有する。
触媒Bは、約50重量%の活性材料を含有する、フェノールでブロックされた1,8−ジアザビシクロウンデカ−7−エン触媒である。
触媒Cは、カルボン酸でブロックされた1,8−ジアザビシクロウンデカ−7−エンである。
約2μm(90%>10μm)の平均粒径、8.5m2/gのBET表面積、及び6.0〜6.5のpHを有する、焼成白土(55% SiO2、45% Al2O3)。
疎水変性ポリジメチルシロキサン被覆ヒュームドシリカ。
4A型の分子ふるい。
カーボンブラック。
ジ−イソノニル−フタレート
以下の原料を組み合わせ、ブレンドし、2液手動分注ガンにおいて有用な、空気中の湿度を通さない容器中で保管する。原料の量は、表3に示される。
以下の原料を組み合わせ、ブレンドし、2液手動分注ガンにおいて有用な、空気中の湿度を通さない容器中で保管する。
ポリオール側及びイソシアネート側を1対1の比率で利用する。反応性をレオロジーによって測定した。1時間及び2時間の重ね剪断強度を、15×25×1.5mmの接着寸法を有するeコーティング鋼基材を用いて測定する。重ね剪断熱硬化実験を、180秒の加熱サイクル、及び45×15×1.5mmの接着寸法を有するDow CFK基材を用いて実行する。結果は、表3に集計される。表3中、Cは、比較例を意味する。
Claims (22)
- ポリオール成分と、イソシアネート成分と、を含む組成物であって、
a)前記ポリオール成分は、
i)400〜2000のヒドロキシル当量及び2〜3の公称ヒドロキシル官能価を有する1つ以上のポリオールと、
ii)1つ以上の脂肪族ジオール鎖延長剤と、
iii)1つ以上の潜在性室温有機金属触媒と、
iv)3を超える官能価を有する1つ以上の多官能性ポリオールと、を含み、
b)前記ポリイソシアネート成分は、
iv)1つ以上のポリイソシアネート化合物を含み、
前記ポリイソシアネート成分及び前記ポリオール成分は、約1.0〜約1.8のイソシアネートインデックスにおいて接触し、v)1つ以上のカルボン酸でブロックされた環状アミジン化合物、vi)1つ以上のフェノールでブロックされた環状アミジン化合物、またはv)1つ以上のカルボン酸でブロックされた環状アミジン化合物及びvi)1つ以上のフェノールでブロックされた環状アミジン化合物の両方は、前記ポリオール成分または前記イソシアネート成分中に位置し、前記組成物は、2成分ポリウレタン接着剤組成物として有用である、組成物。 - 前記3を超える官能価を有する1つ以上の多官能性ポリオールは、前記ポリオール成分の約1〜約10重量%の量で存在する、請求項1に記載の組成物。
- v)1つ以上のカルボン酸でブロックされた環状アミジン化合物及びvi)1つ以上のフェノールでブロックされた環状アミジン化合物の両方は、前記ポリオール成分または前記イソシアネート成分中に位置する、請求項1または2に記載の組成物。
- 前記1つ以上の多官能性ポリオールは、約4以上の官能価を有する、請求項1〜3のいずれか1項に記載の組成物。
- 前記1つ以上の多官能性ポリオールは、約5〜約8の官能価を有する、請求項1〜4のいずれか1項に記載の組成物。
- 前記1つ以上の潜在性室温有機金属触媒は、スズ、亜鉛、またはビスマスを含有する、請求項1〜5のいずれか1項に記載の組成物。
- 前記1つ以上の潜在性室温有機金属触媒は、亜鉛アルカノエート、ビスマスアルカノエート、ジアルキルスズアルカノエート、ジアルキルスズメルカプチド、ジアルキルスズビス(アルキルメルカプトアセテート)、ジアルキルスズチオグリコレート、またはこれらの混合物である、請求項1〜6のいずれか1項に記載の組成物。
- 前記1つ以上の潜在性室温有機金属触媒は、ジアルキルスズメルカプチド、ジアルキルスズビス(アルキルメルカプトアセテート)、ジアルキルスズチオグリコレート、またはこれらの混合物である、請求項1〜7のいずれか1項に記載の組成物。
- 前記1つ以上の環状アミジン化合物は、1,8−ジアザビシクロ[5.4.0]ウンデカ−7−エン)または1,5−ジアザビシクロ[4.3.0]ノン−5−エンのうちの1つ以上を含む、請求項1〜8のいずれか1項に記載の組成物。
- 前記1つ以上の潜在性室温有機金属触媒は、前記ポリオール成分の重量に基づき約0.005〜約1.0重量%の量で存在し、前記フェノールでブロックされた環状アミジンは、前記ポリオールまたはポリイソシアネート成分の重量に基づき約0.01〜約2.0重量%の量で存在し、前記カルボン酸でブロックされた環状アミジンは、前記ポリオールまたはポリイソシアネート成分の重量に基づき約0.01〜約2.0重量%の量で存在する、請求項1〜9のいずれか1項に記載の組成物。
- 前記ポリオール成分は、1つ以上の粒子状充填剤を含有し、前記ポリイソシアネート成分は、1つ以上の粒子状充填剤を含有する、請求項1〜10のいずれか1項に記載の組成物。
- 400〜2000のヒドロキシル当量及び2〜3の公称ヒドロキシル官能価を有する前記1つ以上のポリオールは、前記ポリオール成分の約35〜約80重量%の量で存在し、
前記1つ以上の鎖延長剤は、前記ポリオール成分の約1〜約10重量%の量で存在し、
前記ポリイソシアネート化合物は、前記ポリイソシアネート成分の約20〜約65重量%の量で存在する、請求項6に記載の組成物。 - 前記1つ以上の潜在性室温有機金属触媒は、前記ポリオール成分の重量に基づき約0.020〜約0.070重量%の量で存在し、前記フェノールでブロックされた環状アミジンは、前記ポリオールまたはポリイソシアネート成分の重量に基づき約0.01〜約1.0重量%の量で存在し、前記カルボン酸でブロックされた環状アミジンは、前記ポリオールまたはポリイソシアネート成分の重量に基づき約0.01〜約1.0重量%の量で存在する、請求項1〜9のいずれか1項に記載の組成物。
- 前記ポリオール成分及び前記イソシアネート成分を接触させた後の前記組成物のオープンタイムは、8分以上である、請求項1〜13のいずれか1項に記載の組成物。
- 前記酸でブロックされたアミジン化合物は、1〜24個の炭素原子を有する脂肪族カルボン酸またはこれらの2つ以上の混合物でブロックされる、請求項1〜14のいずれか1項に記載の組成物。
- 前記フェノールでブロックされたアミジン化合物は、フェノール、置換フェノール、またはこれらの2つ以上の混合物でブロックされる、請求項1〜15のいずれか1項に記載の組成物。
- 前記粒子状充填剤は、前記ポリイソシアネート成分の重量の約10〜約50%、及び前記ポリオール成分の重量の約25〜約60%を構成する、請求項1〜16のいずれか1項に記載の組成物。
- a)請求項1〜17のいずれか1項に記載のポリオール成分及びイソシアネート成分を接触させ、混合して、均一混合物を形成するステップと、
b)前記混合物を第1の基材に適用するステップと、
c)第2の基材を前記第1の基材と接触させるステップであって、パートaの前記混合物は、前記第1の基材と前記第2の基材との間に配置されるステップと、
d)前記基材が動かされ得るように前記第1及び第2の基材が結合されるように、前記混合物が部分的に十分に硬化するような条件下で、前記混合物の一部分を熱に曝露するステップと、を含む、方法。 - e)前記2つの基材をある時間ある温度で加熱して、前記混合物を完全に硬化させて、前記2つの基材を一緒に結合するステップをさらに含む、請求項18に記載の方法。
- 前記熱は、赤外線加熱によってステップdで加えられる、請求項18または19に記載の方法。
- ステップdとeとの間の前記時間枠は、約1時間以上である、請求項18〜20のいずれか1項に記載の方法。
- 前記基材のうちの少なくとも1つは、繊維強化プラスチックである、請求項18〜21のいずれか1項に記載の方法。
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