JP4974557B2 - レトルト処理用紙容器 - Google Patents
レトルト処理用紙容器 Download PDFInfo
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- JP4974557B2 JP4974557B2 JP2006082953A JP2006082953A JP4974557B2 JP 4974557 B2 JP4974557 B2 JP 4974557B2 JP 2006082953 A JP2006082953 A JP 2006082953A JP 2006082953 A JP2006082953 A JP 2006082953A JP 4974557 B2 JP4974557 B2 JP 4974557B2
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- Prior art keywords
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- gas barrier
- layer
- compound
- laminate
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Description
本発明のガスバリア層を構成する組成物は、カルボキシル基およびカルボン酸無水物基から選ばれる少なくとも1つの官能基を含有する重合体を含む組成物からなり、前記少なくとも1つの官能基に含まれる−COO−基の少なくとも一部が2価以上の金属イオンで中和されていること、換言すれば、上記少なくとも1つの官能基の少なくとも一部は、2価以上の金属イオンと塩を構成していることを特徴とする。
ガスバリア層を構成する組成物は、カルボキシル基およびカルボン酸無水物基から選ばれる少なくとも1つの官能基を含有する重合体を含む。該組成物における、重合体の中和物の含有率は、特に限定はなく、たとえば25重量%〜95重量%の範囲とすることができる。この重合体の中和物は、カルボキシル基およびカルボン酸無水物基から選ばれる少なくとも1つの官能基を含む重合体(以下、「カルボン酸含有重合体」という場合がある)に対して、上記少なくとも1つの官能基の少なくとも一部を2価以上の金属イオンで中和することによって得られる重合体である。
化合物(L)には、以下で説明する化合物(A)および/または化合物(B)の少なくとも1種を適用できる。以下、化合物(A)および化合物(B)について説明する。
M1(OR1)nX1 kZ1 m-n-k・・・(I)
化学式(I)中、M1は、Si、Al、Ti、Zr、Cu、Ca、Sr、Ba、Zn、B、Ga、Y、Ge、Pb、P、Sb、V、Ta、W、LaおよびNdから選択される原子を表す。M1は、好ましくはSi、Al、TiまたはZrであり、特に好ましくはSiである。また、化学式(I)中、R1はメチル基、エチル基、n−プロピル基、iso−プロピル基、n−ブチル基、t−ブチル基などのアルキル基であり、好ましくは、メチル基またはエチル基である。また、化学式(I)中、X1はハロゲン原子を表す。X1が表すハロゲン原子としては、例えば、塩素原子、臭素原子、ヨウ素原子などが挙げられるが、塩素原子が好ましい。また、化学式(I)中、Z1は、カルボキシル基との反応性を有する官能基で置換されたアルキル基を表す。ここで、カルボキシル基との反応性を有する官能基としては、エポキシ基、アミノ基、水酸基、ハロゲン原子、メルカプト基、イソシアネート基、ウレイド基、オキサゾリン基またはカルボジイミド基などが挙げられるが、エポキシ基、アミノ基、メルカプト基、イソシアネート基、ウレイド基、またはハロゲン原子が好ましい。このような官能基で置換されるアルキル基としては、前出のものを例示することができる。また、化学式(I)中、mは金属元素M1の原子価と等しい。化学式(I)中、nは0〜(m−1)の整数を表す。また、化学式(I)中、kは0〜(m−1)の整数を表し、1≦n+k≦(m−1)である。
M2(OR2)qR3 p-q-rX2 r・・・(II)
化学式(II)中、M2は、Si、Al、Ti、Zr、Cu、Ca、Sr、Ba、Zn、B、Ga、Y、Ge、Pb、P、Sb、V、Ta、W、LaおよびNdから選択される原子を表すが、好ましくはSi、Al、TiまたはZrであり、特に好ましくはSi、AlまたはTiである。また、化学式(II)中、R2は、メチル基、エチル基、n−プロピル基、iso−プロピル基、n−ブチル基、t−ブチル基などのアルキル基を表すが、好ましくは、メチル基またはエチル基である。また、化学式(II)中、X2はハロゲン原子を表す。X2が表すハロゲン原子としては塩素原子、臭素原子、ヨウ素原子などが挙げられるが塩素原子が好ましい。また、化学式(II)中、R3は、アルキル基、アラルキル基、アリール基またはアルケニル基を表す。R3が表すアルキル基としては、例えば、メチル基、エチル基、n−プロピル基、iso−プロピル基、n−ブチル基、t−ブチル基、n−オクチル基などが挙げられる。また、R3が表すアラルキル基としては、ベンジル基、フェネチル基、トリチル基などが挙げられる。また、R3が表すアリール基としては、フェニル基、ナフチル基、トリル基、キシリル基、メシチル基などが挙げられる。また、R3が表すアルケニル基としては、ビニル基、アリル基などが挙げられる。さらに、化学式(II)中、pは金属元素M2の原子価と等しい。化学式(II)中、qは0〜pの整数を表す。また、化学式(II)中、rは0〜pの整数を表し、1≦q+r≦pである。
ガスバリア層を構成する組成物中の無機成分の含有率は、5〜50重量%の範囲であることが、ガスバリア性が良好となる観点から好ましい。この含有率は、より好ましくは10〜45重量%の範囲であり、さらに好ましくは15〜40重量%の範囲である。組成物中の無機成分の含有率は、該組成物を調製する際に使用する原料の重量から算出することができる。すなわち、化合物(L)、化合物(L)が部分的に加水分解したもの、化合物(L)が完全に加水分解したもの、化合物(L)が部分的に加水分解縮合したもの、化合物(L)が完全に加水分解し、その一部が縮合したもの、あるいはこれらを組み合わせたものなどが完全に加水分解・縮合して金属酸化物になったと仮定し、その金属酸化物の重量を算出する。そして算出された金属酸化物の重量を組成物中の無機成分の重量とみなして、無機成分の含有率を算出する。なお、後述するような金属塩、金属錯体、金属酸化物などの無機添加物を加える場合は、加えた無機添加物の重量を、そのまま無機成分の重量に合算する。金属酸化物の重量の算出をより具体的に説明すると、化学式(I)で示される化合物(A)が完全に加水分解、縮合したときには、組成式が、MO(n+k)/2Z1 m-n-kで表される化合物となる。この化合物のうちMO(n+k)/2の部分が金属酸化物である。Z1については、無機成分に含めず有機成分であるとみなす。また、化学式(II)で示される化合物(B)が完全に加水分解、縮合したときには、組成式が、LO(q+r)/2R3 p-q-rで表される化合物になる。このうち、LO(q+r)/2の部分が金属酸化物である。
以下、本発明の紙容器において、好ましいガスバリア性積層体を製造するための方法について説明する。このように、予めガスバリア性積層体を製造し、これを紙層や耐熱性ポリオレフィン層と積層する方法が工業的に有用である。この方法によれば、本発明のガスバリア性積層体を容易に製造できる。本発明の製造方法に用いられる材料、および積層体の構成は、上述したものと同様であるので、重複する部分については説明を省略する場合がある。
所定の構造を有するブリック型の紙容器について、酸素透過量測定装置(モダンコントロール社製「MOCON OX−TRAN10/50」)を用いて酸素透過度を測定した。具体的には、ブリック型の紙容器の側面から直径6.5cmの円状の試料を切り出し、10cm四方のアルミ箔(厚み30μm)に開けた直径4.5cmの円の上に置き、試料とアルミ箔との間を2液硬化型エポキシ系接着剤で封止したものをセットし、温度20℃、酸素圧1気圧、キャリアガス圧力1気圧の条件下で、酸素透過度(単位:cm3/m2・day・atm)を測定した。このとき、湿度は85%RHの条件を採用し、酸素供給側とキャリアガス側とを同一の湿度とした。
所定の構造を有するブリック型の紙容器(内容量500ml)に蒸留水500gを注入した後、水道水又はイオン交換水で満たされたオートクレーブ中に浸漬し、120℃、30分の条件でレトルト処理を施した。レトルト処理後、加熱を停止し、内部温度が60℃になった時点で、オートクレーブからブリック型の紙容器を取り出し、20℃、85%RHに調湿された部屋でブリック型の紙容器を1時間放置した。その後、ヒートシールされた部分をはさみで切り取り,積層体の表面に付着した水を紙タオルで軽く押し付けるように拭き取った。その後、20℃、85%RHに調湿された部屋にブリック型の紙容器を1週間放置し、得られたブリック型の紙容器から試料を切り出し、上記の(1)酸素バリア性と同様の測定を行うことによって、レトルト処理後の酸素バリア性を評価した。
後述の実施例で作製するガスバリア層(1μm)/AC/OPET(12μm)/AC/ガスバリア層(1μm)からなる積層体について、フーリエ変換赤外分光光度計(株式会社島津製作所製、8200PC)を用いて、ATR(全反射測定)のモードで、ガスバリア層に含まれるC=O伸縮振動のピークを観察した。イオン化前のカルボン酸含有重合体のカルボキシル基のC=O伸縮振動に帰属されるピークは1600cm−1〜1850cm−1の範囲に観察され、イオン化された後のカルボキシル基のC=O伸縮振動は1500cm−1〜1600cm−1の範囲に観察された。そして、それぞれの範囲における最大の吸光度からその比を算出し、その比と予め下記の方法で作成した検量線とを用いてイオン化度を求めた。
数平均分子量150,000のポリアクリル酸を蒸留水に溶解し、所定量の水酸化ナトリウムでカルボキシル基を中和した。得られたポリアクリル酸の中和物の水溶液を、基材上に、イオン化度の測定の対象となる積層体のガスバリア層と同じ厚さになるようにコートし、乾燥させた。基材には、2液型のアンカーコート剤(三井武田ケミカル株式会社製、タケラック3210(商品名)およびタケネートA3072(商品名)、以下ACと略記することがある)を表面にコートした延伸PETフィルム(東レ株式会社製、ルミラー(商品名)。厚さ12μm。以下、「OPET」と略記することがある)を用いた。このようにして、カルボキシル基の中和度が、0〜100モル%間で10モル%ずつ異なる11種類の標準サンプル[積層体(ポリアクリル酸の中和物からなる層/AC/OPET)]を作製した。これらのサンプルについて、フーリエ変換赤外分光光度計(島津製作所製、8200PC)を用いて、ATR(全反射測定)のモードで、赤外吸収スペクトルを測定した。そして、ポリアクリル酸の中和物からなる層に含まれるC=O伸縮振動に対応する2つのピーク、すなわち、1600cm−1〜1850cm−1の範囲に観察されるピークと1500cm−1〜1600cm−1の範囲に観察されるピークとについて、吸光度の最大値の比を算出した。そして、算出した比と、各標準サンプルのイオン化度とを用いて検量線を作成した。
上記で製造した密閉液体紙容器は、120℃、30分のレトルト処理を施しても、処理前と比較して外観に変化はなく、さらに酸素ガスに対するバリア性に優れ、その内容物の変質は認められず、市場における流通に耐え、かつ、貯蔵保存等に優れているものであった。ブリック型紙容器の酸素ガスバリア性を測定したところ、20℃、85%RHでの酸素透過度0.20cc/m2・day・atmと非常に良好な値を示した。また120℃、30分のレトルト処理後の酸素バリア性を測定したところ、20℃、85%RHでの酸素透過度0.40cc/m2・day・atmと非常に良好な値を示した。
以下、溶液(S1)の代わりに溶液(S4)を用いること以外は実施例1の通りの操作を行い、無色透明で外観良好なガスバリア層を有する積層体(4)を得た。
Claims (7)
- 少なくとも紙層、耐熱性ポリオレフィン層、およびガスバリア性積層体からなる層を有する紙容器において、該ガスバリア性積層体は、基材と、基材の少なくとも一方の面に積層されたガスバリア層とを含むガスバリア性積層体であって、該ガスバリア層が、化合物(L)の加水分解縮合物と、カルボキシル基およびカルボン酸無水物基から選ばれる少なくとも1つの官能基を含有する重合体を含む組成物からなり、
前記化合物(L)が、以下の化学式(I)で示される少なくとも1種の化合物(A)と、以下の化学式(II)で示される少なくとも1種の化合物(B)とからなり、
前記化合物(A)/前記化合物(B)のモル比が0.5/99.5〜40/60の範囲であり、
前記少なくとも1つの官能基に含まれる−COO−基の少なくとも一部が2価以上の金属イオンで中和されていることを特徴とする紙容器。
M 1 (OR 1 ) n X 1 k Z m-n-k ・・・(I)
[化学式(I)中、M 1 はSi、Al、Ti、Zr、Cu、Ca、Sr、Ba、Zn、B、Ga、Y、Ge、Pb、P、Sb、V、Ta、W、LaまたはNdを表す。R 1 はアルキル基を表す。X 1 はハロゲン原子を表す。Zは、カルボキシル基との反応性を有する官能基で置換されたアルキル基を表す。mはM 1 の原子価と等しい。nは0〜(m−1)の整数を表す。kは0〜(m−1)の整数を表す。1≦n+k≦(m−1)である。]
M 2 (OR 2 ) q R 3 p-q-r X 2 r ・・・(II)
[化学式(II)中、M 2 はSi、Al、Ti、Zr、Cu、Ca、Sr、Ba、Zn、B、Ga、Y、Ge、Pb、P、Sb、V、Ta、W、LaまたはNdを表す。R 2 はアルキル基を表す。R 3 はアルキル基、アラルキル基、アリール基またはアルケニル基を表す。X 2 はハロゲン原子を表す。pはM 2 の原子価と等しい。qは0〜pの整数を表す。rは0〜pの整数を表す。1≦q+r≦pである。] - 前記化学式(I)において、カルボキシル基との反応性を有する前記官能基が、エポキシ基、アミノ基、ハロゲン基、メルカプト基、イソシアネート基、ウレイド基および水酸基から選ばれる少なくとも1つの官能基である請求項1に記載の紙容器。
- 前記重合体が、ポリアクリル酸およびポリメタクリル酸から選ばれる少なくとも1種の重合体である請求項1または2に記載の紙容器。
- 前記金属イオンが、カルシウムイオン、マグネシウムイオン、バリウムイオンおよび亜鉛イオンから選ばれる少なくとも1つのイオンである請求項1〜3のいずれか1項に記載の紙容器。
- 最内層が無延伸の耐熱性ポリオレフィン層である、請求項1〜4のいずれか1項に記載の紙容器。
- 前記ガスバリア性積層体が、基材と基材の少なくとも一方の面に積層された層の間に、蒸着法で得た無機物からなる層を有する請求項1〜5のいずれか1項に記載の紙容器。
- 前記耐熱性ポリオレフィン層がポリプロピレン層である請求項1〜6のいずれか1項に記載の紙容器。
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