JPWO2007086331A1 - 多層ボトルの充填方法 - Google Patents
多層ボトルの充填方法 Download PDFInfo
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- JPWO2007086331A1 JPWO2007086331A1 JP2007555918A JP2007555918A JPWO2007086331A1 JP WO2007086331 A1 JPWO2007086331 A1 JP WO2007086331A1 JP 2007555918 A JP2007555918 A JP 2007555918A JP 2007555918 A JP2007555918 A JP 2007555918A JP WO2007086331 A1 JPWO2007086331 A1 JP WO2007086331A1
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- Prior art keywords
- multilayer
- bottle
- layer
- filling
- barrier layer
- Prior art date
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Abstract
Description
50℃≦Tg≦100℃ (1)
Wb≦1重量% (2)
(ただし、Tgは該バリア層のガラス転移点であり、Wbはカールフィッシャー法にて235℃で30分測定した該バリア層の水分率である)
を満たす多層ボトルに保存物を充填する工程を含む多層ボトルの充填方法に関する。
また、本発明は、前記充填方法により得られる充填済み多層ボトルに関する。
OTR(平均値)≦0.2cc・mm/(m2・day・atm)
を満たすことが好ましい。
上記OTRは、より好ましくはOTR≦0.15cc・mm/(m2・day・atm)、さらに好ましくはOTR≦0.10cc・mm/(m2・day・atm)、特に好ましくはOTR≦0.08cc・mm/(m2・day・atm)である。このような酸素バリア性能を示すバリア層を使用することで、得られるボトルのガスバリア性能が良好となり、保存物の消費期限を長くすることができる。
50℃≦Tg≦100℃ (1)
Wb≦1重量% (2)
を満たす必要がある。
ガラス転移点および水分率の測定方法は後述する。
(I)多層プリフォームの表面を90〜110℃に加熱する、
(II)該加熱された多層プリフォームを金型内でロッドにより縦方向に延伸しつつ、多段階に圧力を変えて高圧空気をブローする、
(III)該多段階ブローの一段階目の圧力(一次ブロー圧力)が、0.5〜2.0MPaである、および
(IV)該多段階にブローの最終段階の圧力(二次ブロー圧力)が、2〜4MPaである
を満たす方法で多層プリフォームを2軸延伸ブロー成形することにより多層ボトルを製造することが特に好ましい。
ここで、配向度は、アッベ屈折計を用いて23℃で測定したバリア層の屈折率から下記式により求められる。
配向度=[{n(x)+n(y)}/2−n(z)]×1000
(n(x):ボトル高さ方向の屈折率、n(y):ボトル周方向の屈折率、n(z):厚み方向の屈折率)
また、同様に求めた底部バリア層の配向度(平均値)は好ましくは20〜45、より好ましくは25〜45である。
0≦b/a×100≦200
(a:胴部バリア層平均厚み(μm)、b:底部バリア層平均厚み(μm))
さらに好ましくは0≦b/a×100≦150である。
b/a×100の値が100より大きいときは、底部バリア層の厚みは胴部バリア層の厚みよりも厚いことを意味し、100よりも小さいとき底部バリア層の厚みは胴部バリア層厚みよりも薄いことを意味する。0のときは底部にバリア層が存在しないことを意味するが、この場合、底部全体にバリア層が存在しないと、ボトルのバリア性が低下するので、接地部に近い部分のみバリア層が存在せず、その他の底部にはバリア層が存在することが好ましい。
なお、多層プリフォームを製造する方法は、上記方法だけに限定されるものではない。
Wp≦1重量% (3)
を満たすことが好ましい。
条件3は、Wp≦0.7重量%であることがより好ましく、Wp≦0.5重量%であることがさらに好ましく、Wp≦0.3重量%であることが特に好ましい。Wpの下限値は通常0.005重量%である。上記範囲であると、多層プリフォームから多層ボトルへのブロー成形が容易であり、ブロー工程中でのバリア層の結晶化を抑制し、耐層間剥離性が良好となるため好ましい。また、多層ボトルの水分率が低くなるため好ましい。さらに吸湿によるバリア層の白化を防止できるので好ましい。
ASTM D2463−95 ProcedureBに基づき、容器の落下試験により層間剥離高さを求めて評価した。層間剥離高さが高いほど、耐層間剥離性が良好であることを示す。まず、多層容器に水を満たしキャップをした後、多層容器を落下させ層間剥離の有無を目視で判定した。多層容器は底部が床に接触するように垂直落下させた。落下高さを15cm間隔で増減させながらテストを繰り返した。テストボトル数は30本。
23℃、相対湿度50%の雰囲気下にてASTM D3985に準じて測定した。測定は、モダンコントロールズ社製、OX−TRAN 10/50Aを使用した。尚、バリア層のOTRは成形したボトルを丁寧に解体し、バリア層のみ取り出し測定した。なお、バリア層のみを取り出すのが困難なときは、ポリエステルA層とバリア層からなるボトル胴部をシート状に切断し、多層でOTRを測定した後に、顕微鏡などを用いて、各層の厚みを測定して、既知のポリエステルA層のOTR値を利用して、バリア層のみのOTR値を計算することができる。または、ボトルのOTR、ボトルの表面積および各層厚みからバリア層のOTRを計算することができる。
ボトルを丁寧に解体し、バリア層のみを取り出し、DSC(示差走査熱量測定)法により測定した。測定には島津製作所(株)製DSC−50を用い、約5mgのサンプルを10℃/分の昇温速度で室温から300℃まで加熱した際のDSC曲線から求めた。ガラス転移点としては、いわゆる中点温度(Tgm)を採用した。なお、Tgmとは広く知られているように、DSC曲線において、ガラス状態ならびに過冷却状態(ゴム状態)の各ベースラインの接線と転移スロープの接線との2つの交点の中点温度である。
ボトルまたはプリフォームを丁寧に解体し、バリア層のみを取り出し、平沼産業(株)製AQ−2000を用い、カールフィッシャー法により水分率を測定した。測定温度は235℃、測定時間は30分であった。
DSC(示差走査熱量測定)法により測定した。島津製作所(株)製DSC−50を用い、約5mgのサンプルを10℃/分の昇温速度で室温から300℃まで加熱した際に得られる発熱ピークから求めた。
アタゴ製アッベ屈折計DR−M2を使用し、23℃にてナトリウムD線(589nm)を使用し、バリア層の屈折率を測定した後、前述の式により配向度を求めた。
多層ボトルの底部のペタロイド形状が、金型から良好に転写されているか否か目視で判断した。
下記の条件により、ポリエステル層/バリア層/ポリエステル層からなる3層プリフォーム(27g)を射出成形し、冷却した。得られた多層プリフォームのバリア層の水分率は、0.12重量%であった。冷却後速やかに、得られたプリフォームを加熱し2軸延伸ブロー成形を行い多層ボトルを得た。多層ボトル(水を充填する直前)のバリア層の特性を第1表に示す。
得られた多層ボトルに速やかに水(23℃)を充填し、耐層間剥離性を評価した。結果を第1表に示す。
ポリエチレンテレフタレート(日本ユニペット製 RT543C)
固有粘度:0.75dl/g(フェノール/テトラクロロエタン=6/4(重量比)の混合溶媒を使用し、30℃で測定)
ポリアミドMXD6(三菱ガス化学製 MXナイロンS6007(固相重合品))
相対粘度:2.70
全長95mm
外径22mm
肉厚4.2mm
3層プリフォームの製造には、名機製作所(株)製の射出成形機(型式:M200、4個取り)を使用した。
スキン側射出シリンダー温度:280℃
コア側射出シリンダー温度 :260℃
金型内樹脂流路温度 :280℃
金型冷却水温度 :15℃
プリフォーム中のバリア樹脂の割合:5重量%
全長223mm
外径65mm
内容積500ml
底部形状:ペタロイドタイプ
胴部ディンプル:無し
2軸延伸ブロー成形はフロンティア社製ブロー成形機(型式:EFB1000ET)を使用した。
プリフォーム加熱温度:101℃
延伸ロッド用圧力:0.5MPa
一次ブロー圧力:1.1MPa
二次ブロー圧力:2.5MPa
一次ブロー遅延時間:0.34sec
一次ブロー時間:0.30sec
二次ブロー時間:2.0sec
ブロー排気時間:0.6sec
金型温度:30℃
実施例1と同様にして得た多層ボトルを、第1表に記載した条件下で保存した。保存後かつ水を充填する直前のTg、水分率およびOTR、および、耐層間剥離性を第1表に示す。
比較例1で得られた多層ボトル(バリア層のTgが48℃、水分率が3重量%)を30℃の真空下で乾燥し、バリア層のTgを70℃、水分率を0.8重量%にした。得られた多層ボトルに速やかに水を充填し、耐層間剥離性を評価した。結果を第1表に示す。なお、結晶化熱量が上記した好ましい範囲(2〜20J/g)外であるが、これは乾燥時に結晶化が進行したためと考えられる。そのため、バリア層の水分率が1重量%を超えないように制御した場合と比べて、耐層間剥離性の向上効果が幾分低くなったものと考えられる。
実施例1と同様にして得た多層ボトルに水を充填後、比較例1と同様に14日間保存し、その後、耐層間剥離性を評価した。層間剥離高さは283cmであり、実施例1と同等の結果であった。
あらかじめ口栓部を加熱結晶化したプリフォームをブローし、金型温度145℃で5秒間ヒートセットした以外は実施例1と同様にして多層ボトルを得た。バリア層のTgは86℃、水分率は0.1重量%、OTRは0.056cc・mm/(m2・day・atm)であった。得られたボトルに85℃の水をホットフィル後、耐層間剥離性を評価した。層間剥離高さは270cmであった。
実施例1と同様にして得た多層プリフォーム100本を第2表記載の条件で保存し、バリア層の水分率を調整した。保存後のプリフォームを、実施例1と同様にブロー成形し多層ボトルを得た。得られた多層ボトルを23℃、50%RHで1日間保存した後、直ちに水(23℃)を充填し、耐層間剥離性を評価した。水を充填する直前のバリア層のTg、水分率、層間剥離性を第2表に示す。得られた多層プリフォーム、多層ボトルに白化は観察されなかった(実施例8〜12)。比較例3では、保存後のプリフォームのバリア層が一部白化していた。
なお、多層プリフォームの保存に使用したポリエチレン製の袋の口はインシュロックにて封をし(実施例10と11)、アルミラミネートフィルムからなる袋の場合は口をヒートシールした(実施例12)。また、保存は乾燥剤(シリカゲル200gを含む不織布の袋)の存在下で行った(実施例10)。
実施例1と同様にして多層ボトルを製造し、水を充填した。製造条件および測定結果を第3〜5表に示す。
実施例14〜16および比較例4〜5
ブロー成形条件を変更した以外は実施例13と同様の操作を繰り返した。比較例4では、一段階ブロー成形した。製造条件および測定結果を第3〜5表に示す。なお、比較例5ではブロー成形により多層ボトルを得ることはできなかった。
Claims (16)
- 最外層、最内層、および最外層と最内層との間に位置する少なくとも1層のバリア層を有し、該最外層および最内層が、テレフタル酸を80モル%以上含むジカルボン酸成分およびエチレングリコールを80モル%以上含むジオール成分を重合して得た熱可塑性ポリエステル樹脂により主として構成され、かつ、下記条件1および2:
50℃≦Tg≦100℃ (1)
Wb≦1重量% (2)
(ただし、Tgは該バリア層のガラス転移点であり、Wbはカールフィッシャー法にて235℃で30分測定した該バリア層の水分率である)
を満たす多層ボトルに保存物を充填する工程を含む多層ボトルの充填方法。 - 前記Wbが0.01〜1重量%である請求項1記載の充填方法。
- 前記多層ボトルが、多層プリフォームを、ホットパリソン法あるいはコールドパリソン法にてブロー成形して得られる請求項1記載の充填方法。
- 前記多層ボトルをブロー金型内でヒートセットする請求項3記載の内容物充填方法。
- 前記多層プリフォームのバリア層の水分率が1重量%以下である請求項3記載の充填方法。
- 前記多層プリフォームのバリア層の水分率が0.005〜1重量%である請求項3記載の充填方法。
- 前記多層プリフォームを、JIS K7129で規定される水蒸気透過度が20g/m2・day以下のフィルムからなる袋に保存し、次いで、多層ボトルにブロー成形する請求項3記載の充填方法。
- 前記多層プリフォームの保存を乾燥剤の存在下で行う請求項7記載の充填方法。
- ブロー成形で多層ボトルを製造してから7日以内に保存物を充填する請求項3記載の充填方法。
- ブロー成形多層ボトルにインラインで保存物を充填する請求項3記載の充填方法。
- 前記充填をホットフィルにより行う請求項1記載の充填方法。
- 前記充填をアセプティック(無菌)充填により行う請求項1記載の充填方法。
- 前記保存物が、ビールまたは炭酸飲料である請求項1記載の充填方法。
- 前記バリア層が、メタキシリレンジアミンを70モル%以上含むジアミン成分と、炭素数4〜20のα,ω−直鎖脂肪族ジカルボン酸を50モル%以上含むジカルボン酸成分とを重縮合して得られるポリアミドにより主として構成される請求項1記載の充填方法。
- 前記多層ボトルを、下記I〜IVの条件:
(I)多層プリフォームの表面を90〜110℃に加熱する、
(II)該加熱された多層プリフォームを金型内でロッドにより縦方向に延伸しつつ、多段階に圧力を変えて高圧空気をブローする、
(III)該多段階ブローの一段階目の圧力(一次ブロー圧力)が、0.5〜2.0MPaである、および
(IV)該多段階にブローの最終段階の圧力(二次ブロー圧力)が、2〜4MPaである
を満たす方法で多層プリフォームを2軸延伸ブロー成形することにより製造する請求項1記載の充填方法。 - 請求項1に記載の充填方法により得られる充填済み多層ボトル。
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