JP6980234B2 - 樹脂組成物、成形体、積層体、ガスバリア材、コーティング材及び接着剤 - Google Patents
樹脂組成物、成形体、積層体、ガスバリア材、コーティング材及び接着剤 Download PDFInfo
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- JP6980234B2 JP6980234B2 JP2019506230A JP2019506230A JP6980234B2 JP 6980234 B2 JP6980234 B2 JP 6980234B2 JP 2019506230 A JP2019506230 A JP 2019506230A JP 2019506230 A JP2019506230 A JP 2019506230A JP 6980234 B2 JP6980234 B2 JP 6980234B2
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- VSWALKINGSNVAR-UHFFFAOYSA-N naphthalen-1-ol;phenol Chemical compound OC1=CC=CC=C1.C1=CC=C2C(O)=CC=CC2=C1 VSWALKINGSNVAR-UHFFFAOYSA-N 0.000 description 1
- NXPPAOGUKPJVDI-UHFFFAOYSA-N naphthalene-1,2-diol Chemical compound C1=CC=CC2=C(O)C(O)=CC=C21 NXPPAOGUKPJVDI-UHFFFAOYSA-N 0.000 description 1
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- JFNLZVQOOSMTJK-KNVOCYPGSA-N norbornene Chemical compound C1[C@@H]2CC[C@H]1C=C2 JFNLZVQOOSMTJK-KNVOCYPGSA-N 0.000 description 1
- 125000003518 norbornenyl group Chemical group C12(C=CC(CC1)C2)* 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical group CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- MSRJTTSHWYDFIU-UHFFFAOYSA-N octyltriethoxysilane Chemical compound CCCCCCCC[Si](OCC)(OCC)OCC MSRJTTSHWYDFIU-UHFFFAOYSA-N 0.000 description 1
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- 239000003960 organic solvent Substances 0.000 description 1
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- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- XUWHAWMETYGRKB-UHFFFAOYSA-N piperidin-2-one Chemical compound O=C1CCCCN1 XUWHAWMETYGRKB-UHFFFAOYSA-N 0.000 description 1
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- 125000003367 polycyclic group Chemical group 0.000 description 1
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- 239000003381 stabilizer Substances 0.000 description 1
- 238000007655 standard test method Methods 0.000 description 1
- 238000006467 substitution reaction Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 150000003509 tertiary alcohols Chemical class 0.000 description 1
- YLQBMQCUIZJEEH-UHFFFAOYSA-N tetrahydrofuran Natural products C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
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- 238000002834 transmittance Methods 0.000 description 1
- WUMSTCDLAYQDNO-UHFFFAOYSA-N triethoxy(hexyl)silane Chemical compound CCCCCC[Si](OCC)(OCC)OCC WUMSTCDLAYQDNO-UHFFFAOYSA-N 0.000 description 1
- CPUDPFPXCZDNGI-UHFFFAOYSA-N triethoxy(methyl)silane Chemical compound CCO[Si](C)(OCC)OCC CPUDPFPXCZDNGI-UHFFFAOYSA-N 0.000 description 1
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 1
- NBXZNTLFQLUFES-UHFFFAOYSA-N triethoxy(propyl)silane Chemical compound CCC[Si](OCC)(OCC)OCC NBXZNTLFQLUFES-UHFFFAOYSA-N 0.000 description 1
- JXUKBNICSRJFAP-UHFFFAOYSA-N triethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CCO[Si](OCC)(OCC)CCCOCC1CO1 JXUKBNICSRJFAP-UHFFFAOYSA-N 0.000 description 1
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- JLGNHOJUQFHYEZ-UHFFFAOYSA-N trimethoxy(3,3,3-trifluoropropyl)silane Chemical compound CO[Si](OC)(OC)CCC(F)(F)F JLGNHOJUQFHYEZ-UHFFFAOYSA-N 0.000 description 1
- GFKCWAROGHMSTC-UHFFFAOYSA-N trimethoxy(6-trimethoxysilylhexyl)silane Chemical compound CO[Si](OC)(OC)CCCCCC[Si](OC)(OC)OC GFKCWAROGHMSTC-UHFFFAOYSA-N 0.000 description 1
- ZNOCGWVLWPVKAO-UHFFFAOYSA-N trimethoxy(phenyl)silane Chemical compound CO[Si](OC)(OC)C1=CC=CC=C1 ZNOCGWVLWPVKAO-UHFFFAOYSA-N 0.000 description 1
- HQYALQRYBUJWDH-UHFFFAOYSA-N trimethoxy(propyl)silane Chemical compound CCC[Si](OC)(OC)OC HQYALQRYBUJWDH-UHFFFAOYSA-N 0.000 description 1
- BPSIOYPQMFLKFR-UHFFFAOYSA-N trimethoxy-[3-(oxiran-2-ylmethoxy)propyl]silane Chemical compound CO[Si](OC)(OC)CCCOCC1CO1 BPSIOYPQMFLKFR-UHFFFAOYSA-N 0.000 description 1
- AAAQKTZKLRYKHR-UHFFFAOYSA-N triphenylmethane Chemical compound C1=CC=CC=C1C(C=1C=CC=CC=1)C1=CC=CC=C1 AAAQKTZKLRYKHR-UHFFFAOYSA-N 0.000 description 1
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- 239000002023 wood Substances 0.000 description 1
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Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08K—Use of inorganic or non-macromolecular organic substances as compounding ingredients
- C08K9/00—Use of pretreated ingredients
- C08K9/02—Ingredients treated with inorganic substances
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
- C08G—MACROMOLECULAR COMPOUNDS OBTAINED OTHERWISE THAN BY REACTIONS ONLY INVOLVING UNSATURATED CARBON-TO-CARBON BONDS
- C08G18/00—Polymeric products of isocyanates or isothiocyanates
- C08G18/06—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen
- C08G18/70—Polymeric products of isocyanates or isothiocyanates with compounds having active hydrogen characterised by the isocyanates or isothiocyanates used
- C08G18/72—Polyisocyanates or polyisothiocyanates
- C08G18/80—Masked polyisocyanates
- C08G18/8003—Masked polyisocyanates masked with compounds having at least two groups containing active hydrogen
- C08G18/8048—Masked polyisocyanates masked with compounds having at least two groups containing active hydrogen with compounds of C08G18/34
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B1/00—Layered products having a non-planar shape
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/043—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of metal
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/08—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin
- B32B15/095—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of synthetic resin comprising polyurethanes
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/10—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of wood
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- B—PERFORMING OPERATIONS; TRANSPORTING
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- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B15/00—Layered products comprising a layer of metal
- B32B15/04—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B15/12—Layered products comprising a layer of metal comprising metal as the main or only constituent of a layer, which is next to another layer of the same or of a different material of paper or cardboard
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- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
- B32B—LAYERED PRODUCTS, i.e. PRODUCTS BUILT-UP OF STRATA OF FLAT OR NON-FLAT, e.g. CELLULAR OR HONEYCOMB, FORM
- B32B21/00—Layered products comprising a layer of wood, e.g. wood board, veneer, wood particle board
- B32B21/04—Layered products comprising a layer of wood, e.g. wood board, veneer, wood particle board comprising wood as the main or only constituent of a layer, which is next to another layer of the same or of a different material
- B32B21/042—Layered products comprising a layer of wood, e.g. wood board, veneer, wood particle board comprising wood as the main or only constituent of a layer, which is next to another layer of the same or of a different material of wood
-
- B—PERFORMING OPERATIONS; TRANSPORTING
- B32—LAYERED PRODUCTS
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Description
一実施形態の樹脂組成物は、ウレタン樹脂と、リチウム部分固定型スメクタイトとを含有する。
スメクタイトとは、層構造を有するフィロケイ酸塩鉱物(層状粘土鉱物)の一種である。スメクタイトの具体的な構造としては、モンモリロナイト、バイデライト、サポナイト、ヘクトライト、スティーブンサイト、ソーコナイト等の構造が知られている。これらのうち、粘土材料の構造としてはモンモリロナイト及びスティーブンサイトからなる群より選択される少なくとも一種の構造が好ましい。これらの構造は、八面体シートの金属元素の一部に、低原子価金属元素との同型置換、欠陥等を有する。そのため、八面体シートが負に帯電している。その結果、これらの構造は八面体シートに空きサイトを有しており、これらの構造を有するスメクタイトでは、後述するようにリチウムイオンが移動後に安定して存在できる。
ウレタン樹脂とはウレタン結合を有する化合物であり、GPC(ゲルパーミエーションクロマトグラフィー)によるポリスチレン換算の重量平均分子量は特に限定はないが、500〜1000000であることが好ましい。ウレタン結合は、例えば、ポリイソシアネート化合物と1分子中に2個以上の水酸基を含有するポリオールとを、反応させることで得ることができる。すなわち、ウレタン樹脂は、ポリオールとポリイソシアネートの反応物であることが好ましい。
樹脂組成物は、更に修飾剤を含有してもよい。修飾剤としては、カップリング剤、シラン化合物、酸無水物等が挙げられる。樹脂組成物がこれらの修飾剤を含有する場合、リチウム部分固定型スメクタイトの濡れ性が向上し、樹脂組成物への分散性が向上する。修飾剤は、1種を単独で用いてよく、複数種を組み合わせて用いてもよい。
第一の実施形態の樹脂組成物は、式(1)で表される化合物Aと式(2)で表される化合物Bとの反応物(重付加物)である、カルボキシル基を有するウレタン樹脂P1と、リチウム部分固定型スメクタイトと、を含有する。
第二の実施形態の樹脂組成物は、ウレタン樹脂P1と化合物Cとの反応物(例えば、ウレタン樹脂P1が有するカルボキシル基と化合物Cが有するエポキシ基との反応により得られる反応生成物)であるウレタン樹脂P2と、リチウム部分固定型スメクタイトと、を含有する。第二の実施形態における、リチウム部分固定型スメクタイト、並びに、ウレタン樹脂P2を構成する化合物A、化合物B及び化合物Cの詳細は第一の実施形態と同じである。
第三の実施形態の樹脂組成物は、脂環骨格を有するウレタン樹脂と、リチウム部分固定型スメクタイトとを含有する。
第四の実施形態の樹脂組成物は、上記式(1)で表される化合物Aと、上記式(2)で表される化合物Bと、リチウム部分固定型スメクタイトと、を含有し、好ましくは、エポキシ基を有する化合物Cを更に含有する。
実施形態の成形体は、上述した樹脂組成物を成形して得ることができる。成形体は、樹脂組成物からなっていてよく、樹脂組成物の硬化物からなっていてもよい。成形方法は任意であり、用途によって適時選択すればよい。成形体の形状に制限はなく、板状、シート状、又はフィルム状であってもよく、立体形状を有していてもよく、基材に塗布されたものであってもよく、基材と基材の間に存在する形で成形されたものであってもよい。
実施形態の積層体は、上述した成形体を基材上に備えるものである。積層体は2層構造であってもよく、3層構造以上であってもよい。
撹拌装置、温度計、冷却管、滴下装置を備えたガラスフラスコに、DMPA(2,2−ジメチロールプロパン酸、東京化成工業株式会社製)90質量部、溶媒としてメチルエチルケトン54質量部、及び、テトラヒドロフラン81質量部を仕込み、窒素気流下にて攪拌した。次いで、XDI(キシリレンジイソシアネート、商品名:タケネート500、三井化学株式会社製)(タケネートは登録商標。以下同じ)56質量部を仕込み、60℃に昇温した。1時間撹拌した後、40℃以下まで温度を下げてから、更にXDI56質量部を仕込み、再度60℃に昇温した。赤外分光法でイソシアネート基の消失が確認されるまで反応を継続した。次いで、希釈溶媒としてメタノール168質量部を加え、カルボキシル基を有するウレタン樹脂「DMPA/XDI」を40質量%含有するポリウレタン溶液1を得た。
撹拌装置、温度計、冷却管及び滴下装置を備えたガラスフラスコに、TCDDM(トリシクロデカンジメタノール、東京化成工業株式会社製)79.1質量部、溶媒としてMEK(メチルエチルケトン)52.9質量部を仕込み、窒素気流下にて攪拌しながら60℃に昇温した。次いで、フラスコ内を60℃に保ちながらXDI(キシリレンジイソシアネート、商品名:タケネート500、三井化学株式会社製)47.9質量部を1時間かけて滴下した。滴下終了後、60℃で5時間攪拌した後、赤外分光法によりイソシアネート基の消失を確認した。次いで、MEK51質量部を加え、脂環骨格を有するウレタン樹脂「TCDDM/XDI」を55質量%含有するポリウレタン溶液2を得た。
シランカップリング剤2.4質量部、水0.5質量部、2−プロパノール123質量部、及び0.1mol/lの塩酸0.1質量部を混合し2時間撹拌することによりシランカップリング剤溶液1を調製した。
シランカップリング剤25質量部、水5.5質量部、2−プロパノール1278質量部、及び0.1mol/lの塩酸1.3部を混合し2時間撹拌することによりシランカップリング剤溶液2を調製した。
シランカップリング剤を5.8質量部、水1.3質量部、2−プロパノール76.5質量部、及び0.1mol/lの塩酸2.4質量部を混合し2時間撹拌することによりシランカップリング剤溶液3を調製した。
ポリカーボネートジオール(商品名:デュラノールT5651、旭化成株式会社製)1.00質量部に対して、上記リチウム部分固定型スメクタイト分散スラリーを1.74質量部、アセトンを4.27質量部、2−プロパノールを0.48質量部、及びシランカップリング剤溶液1を1.26質量部加え、8時間撹拌保持した。次いで、TMP−XDI(キシリレンジイソシアネート−トリメチロールプロパンアダクト体、商品名:タケネートD―110N、三井化学株式会社製、固形分量:75質量%)を0.73質量部加えた。これにより、実施例1の樹脂組成物を得た。これを塗工液1とした。
ポリカーボネートジオール(商品名:デュラノールT5651、旭化成株式会社製)1.00質量部に対して、リチウム部分固定型スメクタイトを18.1質量部、アセトン44.4を質量部、2−プロパノールを5.00質量部、及びシランカップリング剤溶液2を13.1質量部加え、8時間撹拌保持した。次いで、TMP−XDI(キシリレンジイソシアネート−トリメチロールプロパンアダクト体、商品名:タケネートD―110N、三井化学株式会社製、固形分量:75質量%)を0.73質量部加えた。これにより、実施例2の樹脂組成物を得た。これを塗工液2とした。
ポリカーボネートジオール(商品名:デュラノールT5651、旭化成株式会社製)の代わりにポリテトラメチレンエーテルグリコール(PTMG1000、三菱ケミカル株式会社製、平均分子量1000)を用い、配合量を表2に記載の配合量(単位:質量部)に変更したこと以外は、実施例1と同様の方法により実施例3の樹脂組成物を得た。これを塗工液3とした。
容器中に、ポリウレタン溶液1を2.5質量部、上記リチウム部分固定型スメクタイト分散スラリーを1.1質量部、メタノールを0.5質量部、及びアセトニトリルを1.1質量部加え、8時間撹拌保持した。これにより、実施例4の樹脂組成物を得た。これを塗工液4とした。
容器中に、ポリウレタン溶液1を2.5質量部、上記リチウム部分固定型スメクタイト分散スラリーを0.35質量部、メタノールを0.5質量部、アセトニトリルを0.35質量部、及び硬化触媒としてトリフェニルホスフィンを0.013質量部加え、8時間撹拌保持した。次いで、レゾルシノールジグリシジルエーテル(商品名:デナコールEX201、ナガセケムテックス株式会社製)(デナコールは登録商標。以下同じ)を0.32質量部加えた。これにより、実施例5の樹脂組成物を得た。これを塗工液5とした。
各成分の配合量を表3に記載の配合量(単位:質量部)に変更したこと以外は、実施例5と同様の方法により実施例6〜10の樹脂組成物を得た。これらを塗工液6〜10とした。また、塗工液1に代えて塗工液6〜10をそれぞれ用いたこと以外は、実施例1と同様にして、PETフィルム上に実施例6〜10の樹脂組成物の成形体を形成し、実施例6〜10の積層フィルムを得た。
容器中に、ポリウレタン溶液1を2.5質量部、上記リチウム部分固定型スメクタイト分散スラリーを1.49質量部、メタノールを0.5質量部、アセトニトリルを1.49質量部、及び硬化触媒としてトリフェニルホスフィンを0.014質量部加え、8時間撹拌保持した。次いで、3’,4’−エポキシシクロヘキシルメチル 3,4−エポキシシクロヘキサンカルボキシレート(商品名:セロキサイド 2021P、株式会社ダイセル製)(セロキサイドは登録商標)を0.36質量部加えた。これにより、実施例11の樹脂組成物を得た。これを塗工液11とした。
ポリウレタン溶液2を3.5質量部、上記リチウム部分固定型スメクタイト分散スラリーを2.65質量部、MEKを4.86質量部、アセトニトリルを2.65質量部、及びシランカップリング剤溶液3を0.86質量部加え、8時間撹拌保持した。次いで、XDI(キシリレンジイソシアネート、商品名:タケネート500、三井化学株式会社製)を0.46質量部加えた。これにより、実施例12の樹脂組成物を得た。これを塗工液12とした。
ポリウレタン溶液2を3.5質量部、上記リチウム部分固定型スメクタイト分散スラリーを27.8質量部、MEKを2.0質量部、アセトンを27.8質量部、及びシランカップリング剤溶液3を9.1質量部加え、8時間撹拌保持した。次いで、XDI(キシリレンジイソシアネート、商品名:タケネート500、三井化学株式会社製)を0.46質量部加えた。これにより、実施例13の樹脂組成物を得た。これを塗工液13とした。
ポリカーボネートジオール(商品名:デュラノールT5651、旭化成株式会社製)1.00質量部に対して、上記天然モンモリロナイトを3.62質量部、アセトンを44.4質量部、2−プロパノールを5.00質量部、及びシランカップリング剤溶液1を13.1質量部加え、8時間撹拌保持した。次いで、TMP−XDI(キシリレンジイソシアネート−トリメチロールプロパンアダクト体、商品名:タケネートD―110N、三井化学株式会社製、固形分量:75質量%)を0.73質量部加えた。これにより、比較例1の樹脂組成物を得た。これを比較塗工液1とした。
上記リチウム部分固定型スメクタイト分散スラリー及びシランカップリング剤溶液1を用いなかったこと以外は、実施例1と同様にして、比較例2の樹脂組成物を得た。これを比較塗工液2とした。塗工液1に代えて比較塗工液2を用いたこと以外は、実施例1と同様にして、PETフィルム上に比較例2の樹脂組成物の成形体を形成し、比較例2の積層フィルムを得た。
上記リチウム部分固定型スメクタイト分散スラリー及びシランカップリング剤溶液1を用いなかったこと以外は、実施例3と同様にして、比較例3の樹脂組成物を得た。これを比較塗工液3とした。塗工液1に代えて比較塗工液3を用いたこと以外は、実施例1と同様にして、PETフィルム上に比較例3の樹脂組成物の成形体を形成し、比較例3の積層フィルムを得た。
ポリウレタン溶液1を2.5質量部、上記天然モンモリロナイトを3.12質量部、メタノールを0.5質量部、アセトニトリルを3.12質量部、及び硬化触媒としてトリフェニルホスフィンを0.013質量部加え、8時間撹拌保持した。次いで、レゾルシノールジグリシジルエーテル(商品名:デナコールEX201、ナガセケムテックス株式会社製)を0.32質量部加えた。これにより、比較例4の樹脂組成物を得た。これを比較塗工液4とした。
ポリウレタン溶液1を2.5質量部、メタノールを0.5質量部、アセトニトリルを0.46質量部、及び硬化触媒としてトリフェニルホスフィンを0.013質量部加え、8時間撹拌保持した。次いで、レゾルシノールジグリシジルエーテル(商品名:デナコールEX201、ナガセケムテックス株式会社製)を0.32質量部加えた。これにより、比較例5の樹脂組成物を得た。これを比較塗工液5とした。
ポリウレタン溶液2を3.5質量部、上記天然モンモリロナイトを5.6質量部、MEK2.0質量部、アセトンを27.8質量部、及びシランカップリング剤溶液3を9.1質量部加え、8時間撹拌保持した。次いで、XDI(キシリレンジイソシアネート、商品名:タケネート500、三井化学株式会社製)を0.46質量部加えた。これにより、比較例6の樹脂組成物を得た。これを比較塗工液6とした。
上記リチウム部分固定型スメクタイト分散スラリー、アセトニトリル及びシランカップリング剤溶液3を用いなかったこと以外は、実施例12と同様にして、比較例7の樹脂組成物を得た。これを比較塗工液7とした。塗工液1に代えて比較塗工液7を用いたこと以外は、実施例1と同様にして、PETフィルム上に比較例7の樹脂組成物の成形体を形成し、比較例7の積層フィルムを得た。
実施例1〜13及び比較例1〜7の積層フィルムについて成膜性、酸素透過性及び水蒸気透過性を評価した。評価結果は表1〜4に示す。なお、成膜性、酸素透過性及び水蒸気透過性の評価は以下の方法で実施した。
成膜性は、積層フィルムの塗工面が平滑である場合は「A」、塗工面が平滑でない場合は「B」と評価した。
酸素透過率の測定は、JIS−K7126(等圧法)に準じ、モコン社製酸素透過率測定装置OX−TRAN1/50を用いて、温度23℃、湿度0%RHの雰囲気下、及び、温度23℃、湿度90%RHの雰囲気下で実施した。なお、RHとは相対湿度を表す。
水蒸気透過率の測定は、JIS−K7129に準じ、イリノイ社製水蒸気透過率測定装置7001を用いて、温度40℃、湿度90%RHの雰囲気下で測定した。
Claims (15)
- カルボキシル基を有するウレタン樹脂と、リチウム部分固定型スメクタイトと、エポキシ基を有する化合物Cと、を含有する、樹脂組成物。
- 前記ウレタン樹脂は、ポリオールとポリイソシアネートの反応物である、請求項1に記載の樹脂組成物。
- 前記式(1)のX1は、ベンゼン環構造又はナフタレン環構造を表す、請求項3に記載の樹脂組成物。
- 前記化合物Cは、芳香環構造又は脂環構造と、2個以上のエポキシ基と、を有する、請求項1〜4のいずれか一項に記載の樹脂組成物。
- 前記リチウム部分固定型スメクタイトは、陽イオン交換容量が1〜70meq/100gである、請求項1〜8のいずれか一項に記載の樹脂組成物。
- 前記リチウム部分固定型スメクタイトの含有量は、前記樹脂組成物の不揮発分全量に対し、3〜70質量%である、請求項1〜9のいずれか一項に記載の樹脂組成物。
- 請求項1〜10のいずれか一項に記載の樹脂組成物の成形体。
- 基材と、該基材上に設けられた請求項11に記載の成形体と、を備える積層体。
- 請求項1〜10のいずれか一項に記載の樹脂組成物を含むガスバリア材。
- 請求項1〜10のいずれか一項に記載の樹脂組成物を含むコーティング材。
- 請求項1〜10のいずれか一項に記載の樹脂組成物を含む接着剤。
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