JPWO2012070441A1 - 積層体およびその製造方法 - Google Patents
積層体およびその製造方法 Download PDFInfo
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- JPWO2012070441A1 JPWO2012070441A1 JP2012545696A JP2012545696A JPWO2012070441A1 JP WO2012070441 A1 JPWO2012070441 A1 JP WO2012070441A1 JP 2012545696 A JP2012545696 A JP 2012545696A JP 2012545696 A JP2012545696 A JP 2012545696A JP WO2012070441 A1 JPWO2012070441 A1 JP WO2012070441A1
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Abstract
Description
特に、フィルム基材、ポリ乳酸基材などを用いても、塗工性、密着性良く基材上に形成でき、かつ、基材と微細セルロース繊維層との密着の経時劣化を抑えた積層材料を提供できる。それにより、耐候、耐熱、耐水性も向上した積層体を得ることができる。
図1のように、本発明の積層体(10)は、少なくとも、基材(1)と、基材(1)の一方の面に、アンカー層(2)と、カルボキシル基を有する微細セルロース繊維を含む微細セルロース繊維層(3)とをこの順に積層して構成されている。アンカー層(2)および微細セルロース繊維層(3)は、基材(1)の両面にそれぞれ積層されていてもよい。
原料としては、セルロース素材を用いる。セルロース素材は、粉砕、爆砕、膨潤、精製、漂白、溶解再生、アルカリ処理などの前処理を施していてもよい。特に、セルロース素材としては、ガスバリア性の高い塗膜や強度のある塗膜を得る場合は、セルロースIの結晶構造を有する天然由来のセルロースを用いることが好ましい。原料となる天然由来のセルロースとしては、木材パルプ、非木材パルプ、綿パルプ、バクテリアセルロース、ホヤセルロースなどがある。
セルロースへのカルボキシル基の導入方法としては、一般的に知られる化学的な改質方法を用いることができる。カルボキシメチル化で知られるように、セルロースの水酸基をエステル化・エーテル化してカルボキシル基を導入する手法、水酸基から酸化反応によりカルボキシル基を導入する方法などを選択することができる。
特に、ガスバリア性の高い塗膜を得るためや、結晶構造を崩さずにカルボキシル基を導入するためには、中でも、ニトロキシラジカル誘導体を触媒とし、次亜ハロゲン酸塩や亜ハロゲン酸塩などを共酸化剤として用いる手法が好ましい。特に、TEMPO(2,2,6,6−テトラメチルピペリジノオキシラジカル)を触媒とし、アルカリ条件下、好ましくはpH9以上pH11以下の範囲で、次亜塩素酸ナトリウムと臭化ナトリウムを含む水系媒体中で行われるTEMPO酸化法が、試薬の入手しやすさ、コスト、反応の安定性の点から好適である。上記のTEMPO酸化法においては、反応の進行に伴いアルカリが消費されるため、随時アルカリ水溶液を添加して、系内のpHを一定に保つとよい。
TEMPO類および臭化ナトリウムは、反応の際に触媒量だけ用いればよく、反応後に回収することも可能である。また、上記の反応系では理論上の副生成物は塩化ナトリウムのみであり、廃液の処理も容易で環境への負荷が小さい。
酸化反応停止後、生成した酸化セルロースは、ろ過により反応液中から回収することができる。反応停止後の酸化セルロースにおいて、カルボキシル基は、共酸化剤やpH調整用の無機アルカリに由来する金属イオンを対イオンとした塩を形成している。回収の方法としては、カルボキシル基が塩を形成したまま濾別する方法、反応液に酸を添加しpH3以下に調整しカルボン酸としてから濾別する方法、有機溶剤を添加し凝集させた後に濾別する方法がある。その中でも、ハンドリング性や収率、廃液処理の点からカルボン酸に変換し回収する方法が好適である。また、後述する微細セルロース繊維組成物調製の際にも、対イオンとして金属イオンを含有しないほうが溶剤との混和性に優れるため、カルボン酸に変換し回収する方法が好適である。
回収した酸化セルロースは、洗浄を繰り返すことにより精製でき、触媒や副生成物である塩化ナトリウム、イオンなどの残渣を取り除くことができる。このとき、洗浄液としては水が好ましく、さらに塩酸などを用いpH3以下、より好ましくはpH1.8以下の酸性条件に調整し洗浄を行った後、水による洗浄を行うと、金属イオンを上記分析方法における検出限界量以下とすることができる。または、残存する金属イオン量をより低減させるため、酸性条件での洗浄を複数回行ってもよい。また、セルロース中に塩等が残留していると、後述の分散工程にて分散しにくくなるため、水洗浄は複数回洗浄を行うことが好ましい。
洗浄した酸化セルロースを微細化する工程としては、まず、酸化セルロースを分散媒である水系媒体に浸漬する。この時、浸漬した液のpHは、例えば、4以下となる。酸化セルロースは水系媒体に不溶であり、浸漬した時点では不均一な懸濁液となっている。
また、微細セルロース繊維のカルボキシル基は、塩を形成せず、カルボキシル基の状態、すなわち、「−COOH」の状態で存在していても、反応が進行しやすいため好ましい。
分散処理後の微細セルロース繊維は、数平均繊維径(繊維の短軸方向の幅)が、好ましくは0.001μm以上0.200μm以下であり、より好ましくは0.001μm以上0.050μm以下である。微細セルロース繊維の数平均繊維径は、走査型電子顕微鏡(SEM)や原子間力顕微鏡(AFM)により確認できる。分散が不十分・不均一で、一部に繊維径の大きいものが含まれていると、微細セルロース繊維を含む塗液を製膜した際、膜の透明性や平滑性が著しく低下してしまう問題がある。
AmM(OR)n−m
(式中、Aは炭素数1個以上10個以下の炭素主鎖1種類以上で構成され、Mは金属元素、Rはアルキル基であり、nは金属元素の酸化数、mは置換数(0≦m<n)を表す)で示される有機金属化合物または該有機金属化合物の加水分解物あるいは重合体である。具体的には、TiやZr、Siの金属アルコキシドが挙げられ、特に珪素アルコキシドが良好な性能を示す。テトラメトキシシラン、テトラエトキシシラン、テトラプロポキシシラン等のテトラアルコキシ体又はその重合物、トリメトキシシラン、トリエトキシシラン、トリプロポキシシラン等のトリアルコキシ体又はその重合物、ジメトキシシラン、ジエトキシシラン等のジアルコキシ体又はその重合物、その他、C−Si結合をもつメチルトリメトキシシラン、メチルトリエトキシシラン、メチルジメトキシシラン等、又は、官能基を有するものとして、ビニルトリメトキシシラン、ビニルトリエトキシシラン、γ−メタクリロキシプロピルトリメトキシシラン、γ−グリシドキシプロピルトリメトキシシラン、β(3,4−エポキシシクロヘキシル)エチルトリメトキシシラン、γ−メルカプトプロピルトリメトキシシラン、γ−アミノプロピルトリエトキシシラン、N−β−(アミノエチル)−γ−アミノプロピルトリメトキシシランなどが挙げられる。
また、アンカー層に含まれる樹脂のカルボキシル基は、塩を形成せず、カルボキシル基の状態、すなわち、「−COOH」の状態で存在していても、低温で反応が進行するため好ましい。
また、カルボジイミド基、オキサゾリン基は、室温など低温で緩やかに反応するため、ポリ乳酸などの基材とアンカー層、微細セルロース繊維との密着を経時で安定させることができる。特に、アンカー層を形成するときの乾燥温度を80℃以下の低温でとどめ、その上に微細セルロース繊維層を設けることで、アンカー層中の未反応のカルボジイミド基、オキサゾリン基が、基材や微細セルロース繊維層の劣化や密着性の低下を防ぐことができる。アンカー層を形成するときの乾燥温度は、劣化や密着性の低下を防ぐ効果が大きいことと、特に、基材として耐熱性が低いポリ乳酸などを用いる場合は、基材の変形を最小限に抑えるという面でも、60℃以下にすることがより好ましい。
また、反応性化合物の分子量の上限は特に特定されないが、アンカー層の塗液粘度や膜強度、熱特性を考慮し、適宜調整される。
微細セルロース繊維層上への熱可塑性樹脂層の形成方法としては、熱可塑性樹脂層であるフィルムを、2液硬化型ウレタン樹脂などの接着剤を用いて、微細セルロース繊維層の表面に貼り合わせるドライラミネート法等を用いることが一般的であるが、コーティング、ノンソルベントラミネート、ウェットラミネート、押し出しラミネートなどいずれも公知の方法により積層することもできる。
このように、熱可塑性樹脂層は、微細セルロース繊維層の表面に、接着層を介して設けることが好ましい。また、微細セルロース繊維層と熱可塑性樹脂層との間には、接着層のほかに、印刷層など他の層を設けてもよい。
セルロースとして汎用的に入手可能な針葉樹漂白パルプを用いた。
セルロース60g(絶乾質量換算)を蒸留水1000gに加え撹拌し、膨潤させた後ミキサーにより解繊した。ここに、蒸留水2200gと、予め蒸留水400gに溶解させたTEMPOを0.6g、臭化ナトリウム6gの溶液を加え、2mol/L濃度の次亜塩素酸ナトリウム水溶液172gを滴下により添加し、酸化反応を開始した。反応温度は常に20℃以下に維持した。反応中は系内のpHが低下するが、0.5NのNaOH水溶液を逐次添加し、pH10に調整した。そして、4時間反応させた時点で、エタノール60gを添加し、反応を停止した。続いて、反応液に0.5NのHClを滴下しpHを2まで低下させた。ナイロンメッシュを用いてこの反応液をろ過し、固形分をさらに水で数回洗浄し、反応試薬や副生成物を除去し、固形分濃度7%の水を含有した酸化セルロース1を得た。
反応温度を30℃とする以外は、調製方法1と同様の調製方法により、酸化セルロース2を得た。
絶乾質量換算で0.2gの凍結乾燥した酸化セルロースをビーカーに量りとり蒸留水を加えて60gとした。0.1MのNaCl水溶液を0.5mL加え、0.5Mの塩酸でpHを2とした後0.5MのNaOH水溶液を滴下して伝導度測定を行った。測定はpHが11程度になるまで続けた。弱酸の中和段階に相当する部分がカルボキシル基量となるので、得られた伝導度曲線からNaOHの添加量を読み取ると、酸化セルロース1および2のカルボキシル基の含有量は、それぞれ1.6mmol/g、2.5mmol/gであった。
上記により調製した固形分濃度7%の酸化セルロース1を57.14g(固形分4g)に蒸留水と、0.1Nのアンモニア水溶液を加え、pH10の酸化セルロース懸濁液400gとした。調製した懸濁液を回転刃つきミキサーにて60分間処理し、微細セルロース繊維分散液1を得た。
上記により調製した固形分濃度7%の酸化セルロース1を57.14g(固形分4g)に蒸留水と0.5N水酸化ナトリウム水溶液を加え、pH6.8の酸化セルロース懸濁液400gとした。調製した懸濁液を高圧ホモジナイザーにて処理し、微細セルロース分散液2を得た。
上記により調製した固形分濃度7%の酸化セルロース2を57.14g(固形分4g)に蒸留水と無機層状鉱物(モンモリロナイト)を固形分で2g、0.5N水酸化ナトリウム水溶液を加え、pH8の酸化セルロース懸濁液400gとした。調製した懸濁液を回転刃つきミキサーにて20分間処理し、微細セルロース繊維分散液3を得た。
下記樹脂1〜7と下記添加剤1〜3の組み合わせにより、樹脂100重量部に対し添加剤10重量部を混合し、アンカー層を形成するための塗液(アンカー層形成用塗液)1〜10を調製した。アンカー層形成用塗液における樹脂1〜7と添加剤1〜3の組み合わせ、用いた溶媒および固形分濃度を表3に示す。
樹脂1・・・ポリエスター WR−961
(カルボキシル基含有ポリエステル、アンモニウム塩型、酸価60−70)
日本合成化学製
樹脂2・・・ポリエスター WR−901
(硫酸ナトリウム基含有ポリエステル、酸価5以下)
日本合成化学製
樹脂3・・・アローベース SB−1010
(カルボキシル基含有酸変性ポリオレフィン、アンモニウム塩型、
酸価12以上)
ユニチカ製
樹脂4・・・NT−ハイラミック
(ポリウレタン)
大日精化製
樹脂5・・・バイロエコール BE−600
(ポリ乳酸)
東洋紡績製
樹脂6・・・キトサン
大日精化製
樹脂7・・・ダイヤナール BR−107
(アクリル)
三菱レイヨン製
添加剤1・・・SV−02
(水溶性ポリカルボジイミド 分子量1000以上)
日清紡製
添加剤2・・・エポクロスWS−500
(オキサゾリン 分子量70000)
日本触媒製
添加剤3・・・タケネートA65
(イソシアネート)
三井化学製
添加剤4・・・EX614
(エポキシ)
ナガセケムテックス製
基材として、表面をコロナ処理した厚み25μmのポリ乳酸フィルムを用意した。基材のコロナ処理面上に、アンカー層形成用塗液1〜9をバーコーターを用いて塗布した後、60℃で20分間乾燥処理することにより、厚み約0.2μmのアンカー層を形成した。
アンカー層上に、微細セルロース繊維分散液1をバーコーターを用いて塗布した後、60℃で20分間乾燥処理することにより、厚み約0.2μmの微細セルロース繊維層を形成した。
さらに、微細セルロース繊維層上に、ウレタンポリオール系接着剤を用いて、ドライラミネートにより、熱溶着可能な熱可塑性樹脂層である厚み70μmのポリプロピレンフィルムを貼り合わせて、基材/アンカー層/微細セルロース繊維層/接着層/熱可塑性樹脂層の積層体を得た。
基材として、表面をコロナ処理した厚み25μmのポリエチレンテレフタレートフィルムを用意した。基材のコロナ処理面上に、アンカー層形成用塗液2、3、4をバーコーターを用いて塗布した後、80℃で20分間乾燥処理することにより、厚み約0.2μmのアンカー層を形成した。
アンカー層上に、微細セルロース繊維分散液2をバーコーターを用いて塗布した後、100℃で20分間乾燥処理することにより、厚み約0.2μmの微細セルロース繊維層を形成した。
さらに、微細セルロース繊維層上に、ウレタンポリオール系接着剤を用いて、ドライラミネートにより、熱可塑性樹脂層である厚み70μmのポリプロピレンフィルムを貼り合わせて、基材/アンカー層/微細セルロース繊維層/接着層/熱可塑性樹脂層の積層体を得た。
基材として、表面をコロナ処理した厚み20μmの延伸ポリプロピレンフィルムを用意した。基材のコロナ処理面上に、アンカー層形成用塗液4をバーコーターを用いて塗布した後、80℃で20分間乾燥処理することにより、厚み約1μmのアンカー層を形成した。
アンカー層上に、微細セルロース繊維分散液3をバーコーターを用いて塗布した後、80℃で20分間乾燥処理することにより、厚み約0.5μmの微細セルロース繊維層を形成した。
さらに、微細セルロース繊維層上に、ウレタンポリオール系接着剤を用いて、ドライラミネートにより、熱可塑性樹脂層である厚み70μmのポリプロピレンフィルムを貼り合わせて、基材/アンカー層/微細セルロース繊維層/接着層/熱可塑性樹脂層の積層体を得た。
基材のコロナ処理面上にアンカー層を形成せず、直接微細セルロース繊維分散液1をバーコーターを用いて塗布した以外は、実施例1〜9と同様にして積層体を得た。
アンカー層形成用塗液として、アンカー層形成用塗液9を用いた以外は、実施例10〜12と同様にして積層体を得た。なお、アンカー層形成用塗液10は塗工性が悪く、形成したアンカー層に直接微細セルロース繊維分散液を塗布することが困難であったため、アンカー層表面にコロナ処理を過剰に加え、その後微細セルロース繊維層を設けた。
実施例1〜13および比較例1、2の積層体を作製する際の、微細セルロース繊維分散液を塗布する工程において、実施例1〜13では、微細セルロース繊維分散液の塗れ性が良好で、特にはじきやムラ等が観察されることはなかった。また、比較例2では、アンカー層表面にコロナ処理を過剰に加えたため、微細セルロース繊維分散液の塗れ性はある程度良好であった。
一方、比較例1では、塗れ性が悪く、微細セルロース繊維分散液のはじきやムラが目視で観察できた。
積層体の酸素透過度(cm3/m2/day/atm)を、25℃、40%RH雰囲気下で、酸素透過度測定装置MOCON OX−TRAN 2/21(モダンコントロール社製)を用いて測定することで、通常条件下での酸素バリア性を評価した。
積層体の水蒸気透過度(g/m2/day)を、40℃、90%RH雰囲気下で、JIS Z0208に準拠し、カップ法により測定することで、高湿度条件での水蒸気バリア性を評価した。
積層体を幅15mm長さ100mmの短冊状に切りとり、剥離速度300mm/min.におけるT型剥離強度を測定した。
積層体を40℃90%の環境下で1週間保管し、前述の密着性試験の方法と同様に密着性を評価した。
また、密着性に関しても、実施例のものは良好な結果を示しており、経時安定性に関しても良好な結果を示した。また、これらの効果は、アンカー層に反応性化合物が含まれるもの、アンカー層形成用塗液の塗布後の乾燥温度を60℃以下で加工したものほど大きい結果となった。
2・・・アンカー層
3・・・微細セルロース繊維層
4・・・接着層
5・・・熱可塑性樹脂層
10、20・・・積層体
Claims (13)
- 少なくとも、基材と、前記基材の一方の面に、アンカー層と、カルボキシル基を有する微細セルロース繊維を含む微細セルロース繊維層とをこの順に設けた積層体であって、
前記アンカー層が、カルボキシル基、スルホン酸基、アミノ基または水酸基を有する樹脂を少なくとも1種類以上含むことを特徴とする積層体。 - 前記微細セルロース繊維が、酸化反応によりカルボキシル基が導入された酸化セルロースであり、前記カルボキシル基の含有量が、0.1mmol/g以上5.5mmol/g以下であることを特徴とする請求項1に記載の積層体。
- 前記微細セルロース繊維の数平均繊維径が、0.001μm以上0.200μm以下であることを特徴とする請求項2に記載の積層体。
- 前記微細セルロース繊維のカルボキシル基が、アンモニウム塩またはアミン塩を形成していることを特徴とする請求項3に記載の積層体。
- 前記アンカー層に含まれる樹脂が、ポリエステル樹脂、ポリアミド樹脂、ポリウレタン樹脂、ポリアクリル酸樹脂もしくはポリオレフィン樹脂またはこれらの共重合体であることを特徴とする請求項3に記載の積層体。
- 前記アンカー層が、カルボキシル基を有する樹脂を少なくとも含み、前記樹脂のカルボキシル基が、アンモニウム塩またはアミン塩を形成していることを特徴とする請求項3に記載の積層体。
- 前記アンカー層が、更に、カルボジイミド基、オキサゾリン基、イソシアネート基またはエポキシ基を有する反応性化合物を含むことを特徴とする請求項5に記載の積層体。
- 前記基材が、ポリエステル樹脂からなり、前記アンカー層が、カルボキシル基を有するポリエステル樹脂と、カルボジイミド基またはオキサゾリン基を有する反応性化合物とを含むことを特徴とする請求項7に記載の積層体。
- 前記基材を構成するポリエステル樹脂が、ポリ乳酸であることを特徴とする請求項8に記載の積層体。
- 前記反応性化合物の分子量が、1000以上であることを特徴とする請求項7に記載の積層体。
- 前記アンカー層に含まれる樹脂の酸価が、12以上であることを特徴とする請求項7に記載の積層体。
- 前記アンカー層の厚みが、3nm以上10μm以下であることを特徴とする請求項11に記載の積層体。
- 少なくとも、基材と、前記基材の一方の面に、アンカー層と、カルボキシル基を有する微細セルロース繊維を含む微細セルロース繊維層とをこの順に設けた積層体の製造方法であって、
前記基材の一方の面に、カルボキシル基、スルホン酸基、アミノ基または水酸基を有する樹脂を少なくとも1種類以上と、カルボジイミド基、オキサゾリン基、イソシアネート基またはエポキシ基を有する反応性化合物とを含む塗液を用いて塗膜を形成する工程と、
前記塗膜を80℃以下で乾燥させて前記アンカー層を形成する工程と、
前記アンカー層の上に前記微細セルロース繊維層を形成する工程と
を備えることを特徴とする積層体の製造方法。
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