JP2019150994A - ガスバリア性積層体の製造方法 - Google Patents
ガスバリア性積層体の製造方法 Download PDFInfo
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- JP2019150994A JP2019150994A JP2018036716A JP2018036716A JP2019150994A JP 2019150994 A JP2019150994 A JP 2019150994A JP 2018036716 A JP2018036716 A JP 2018036716A JP 2018036716 A JP2018036716 A JP 2018036716A JP 2019150994 A JP2019150994 A JP 2019150994A
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Abstract
Description
コーティング組成物の塗布方法としては、特に制限されず、例えば、グラビアコート法、リバースコート法、ロールコート法、バーコート法、スプレーコート法、エアナイフコート法、ディッピング法などの公知のコーティング方法が挙げられる。
(ポリウレタンディスパージョン)
0.1gのポリウレタンディスパージョンを10mLのジメチルアセトアミド(DMAc)の溶離液に溶解した後、得られた溶液を一晩静置した。この溶液を0.45μmメンブレンフィルターでろ過し、ろ液についてGPC測定(ポリスチレン換算)して、数平均分子量(Mn)を求めた。
0.3gのコーティング組成物を10mLのジメチルアセトアミド(DMAc)の溶離液に溶解した後、得られた溶液を一晩静置した。この溶液を0.45μmメンブレンフィルターでろ過し、ろ液についてGPC測定(ポリスチレン換算)して、数平均分子量(Mn)を求めた。
分析装置:TOSOH HLC−8320GPC+UV−8320
解析装置:TOSOH GPC Work station EcoSEC−WS
カラム:TOSOH TSK−GEL TSK gel α−M Column No.G0032+G0033
溶離液:0.01mol−LiBr/1000ml−DMAc(N,N−Dimethylacetamide)
検出器:RI 40℃
カラム温度:40℃
流速:0.6mL/min
注入量:100μL
合成例1(ポリウレタンディスパージョン1(PUD1)の合成)
タケネート500(1,3−キシリレンジイソシアネート、m−XDI、三井化学社製)170.7g、VestanatH12MDI(4,4’−メチレンビス(シクロヘキシルイソシアネート)、H12MDI、エボニック社製)29.8g、エチレングリコール34.3g、トリメチロールプロパン2.6g、ジメチロールプロピオン酸19.6gおよび溶剤としてメチルエチルケトン146.2gを混合し、窒素雰囲気下65〜70℃で、NCO%が9.53%以下になるまで反応させ、透明なイソシアネート基末端プレポリマー反応液を得た。
タケネート600(1,3−ビス(イソシアナトメチル)シクロヘキサン、m−H6XDI、三井化学社製)200.2g、エチレングリコール27.8g、ジメチロールプロピオン酸16.7gおよび溶剤としてアセトニトリル72.2gを混合し、窒素雰囲気下65〜70℃で、NCO%が15.73%以下になるまで反応させ、透明なイソシアネート基末端プレポリマー反応液を得た。
m−XDI:タケネート500、1,3−キシリレンジイソシアネート、m−XDI、三井化学社製
H6XDI:タケネート600、1,3−ビス(イソシアナトメチル)シクロヘキサン、1,3−H6XDI、三井化学社製
H12MDI:VestanatH12MDI、4,4’−メチレンビス(シクロヘキシルイソシアネート、エボニック社製
MEK:メチルエチルケトン
TEA:トリエチルアミン
実施例1〜12および比較例1〜4
・コーティング組成物の調製
表2〜表4に記載の割合で、イオン交換水を撹拌しながら2−プロパノールを添加し、さらに、主剤としてのポリウレタンディスパージョン(上記の合成例で得られたPUD)を添加し、混合した。次いで、得られた混合液に、表2〜表4に記載の割合で、硬化剤としてのKBM−403(エポキシシラン、商品名KBM−403、3−グリシドキシプロピルトリメトキシシラン、信越化学社製)を添加し、5分間混合した。
基材としてのポリエステルフィルム(商品名E5102、厚み12μm、東洋紡社製)の一方面に、連続式真空蒸着機(アルバック社製)を用いて、表2〜表4に記載の酸化アルミニウム(Al2O3)または酸化ケイ素(SiO2)を蒸着(1×10−5Pa真空条件下、IB方式)させ、厚み10nmの無機質層(金属蒸着層)を得た。
各実施例および各比較例において得られたガスバリア性積層体を、以下の手順にて評価した。その結果を、表2〜表4に併せて示す。
(1)ラミネートフィルムの製造
ガスバリア性積層体のポリウレタン層に、接着剤としてタケラックA−310(三井化学社製)とタケネートA−3(三井化学社製)と酢酸エチルの混合物(タケラックA−310/タケネートA−3/酢酸エチル=10/1/17.8(質量比))を、乾燥厚み3.7g/m2となるようにバーコーターにて塗布し、ドライヤーで乾燥させた。
(2)密着性および耐熱水性(ラミネート強度)
上記で得られたラミネートフィルムのラミネート強度を、JIS K 6854(1999年)に準拠したT字剥離試験(15mm幅)にて測定した。
(3)酸素透過度
ラミネートフィルムの酸素透過度を、酸素透過度測定装置(MOCON社、OX−TRAN 2/20)にて、20℃、相対湿度80%(80%RH)の条件下で測定した。
また、表中の「材料破壊」とは、ポリエステルフィルムおよび/または金属蒸着層の材料破壊であり、少なくとも、ガスバリア性積層体におけるポリウレタン層と金属蒸着層との密着性に優れることを示す。なお、ラミネート強度の数値は、ガスバリア性積層体におけるポリウレタン層と金属蒸着層との界面剥離における強度を示す。
表5に記載の処方に従って、PUD1、KBM−403(エポキシシラン、商品名KBM−403、3−グリシドキシプロピルトリメトキシシラン、信越化学社製)、2−プロパノールおよび重水を混合した。
(測定条件)
分析装置:ECZ400S/L1 (JEOL RESONANCE)
プローブ:液体サンプル用 標準仕様 φ5mm
測定核:1H(プロトン)
溶媒:D2O
測定チューブ:NORELL社 ST500−7 (φ5mm×178mm)
積算回数:128scan
解析ソフト:ALLICE V2(JEOL RESONANCE)
2 基材
3 金属蒸着層
4 ポリウレタン層
Claims (3)
- キシリレンジイソシアネートおよび/または水添キシリレンジイソシアネートを含むポリイソシアネート成分と、炭素数2〜6のジオール、および、カルボキシ基を含有する活性水素基含有化合物を含むポリオール成分との反応生成物であるイソシアネート基末端プレポリマーと、鎖伸長剤との反応生成物であるポリウレタン樹脂を含有するポリウレタンディスパージョンを含む主剤と、エポキシシランを含む硬化剤とを含有するコーティング組成物を調製する調製工程、
前記調製工程で得られた前記コーティング組成物を、プラスチック基材および無機質層を備える複合フィルムの前記無機質層に対して塗布する塗布工程、および、
前記塗布工程で得られた前記コーティング組成物の塗膜を、40℃以上230℃以下で加熱養生し、前記主剤および前記硬化剤を反応させることにより、ポリウレタン層を得る加熱工程
を備えることを特徴とする、ガスバリア性積層体の製造方法。 - 前記コーティング組成物において、
前記ポリウレタン樹脂が有するカルボキシ基に対する、前記エポキシシランが有するエポキシ基の当量比(エポキシ基/カルボキシ基)が、0.05以上2.0以下である
ことを特徴とする、ガスバリア性積層体の製造方法。 - 前記主剤と前記硬化剤とを含有する前記コーティング組成物の数平均分子量が、10万未満である
ことを特徴とする、ガスバリア性積層体の製造方法。
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WO2022030534A1 (ja) * | 2020-08-07 | 2022-02-10 | 三井化学株式会社 | 積層体および食品包装材 |
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