JP7032676B2 - 積層体および押出成形品 - Google Patents
積層体および押出成形品 Download PDFInfo
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- JP7032676B2 JP7032676B2 JP2020178295A JP2020178295A JP7032676B2 JP 7032676 B2 JP7032676 B2 JP 7032676B2 JP 2020178295 A JP2020178295 A JP 2020178295A JP 2020178295 A JP2020178295 A JP 2020178295A JP 7032676 B2 JP7032676 B2 JP 7032676B2
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- fluororubber
- layer
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- laminate
- polytetrafluoroethylene
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Description
また、本開示では、架橋させる際の収縮を抑制することができる押出成形品を提供することを目的とする。
本開示の積層体において、前記フッ素ゴム組成物が、さらに、パーオキサイド架橋剤を含有することが好ましい。
本開示の積層体において、前記ポリマー層が、フッ素樹脂を含有することが好ましい。
本開示の積層体において、前記フッ素樹脂の燃料透過係数が2.0g・mm/m2/day以下であることが好ましい。
本開示の積層体において、前記フッ素ゴム層と前記ポリマー層とが直接接着していることが好ましい。
本開示の積層体は、チューブまたはホースであることが好ましい。
本開示の押出成形品において、前記フッ素ゴム、前記ポリテトラフルオロエチレンおよび塩基性の多官能化合物を含有するフッ素ゴム組成物から形成されることが好ましい。
本開示の押出成形品において、前記フッ素ゴム組成物が、さらに、パーオキサイド架橋剤を含有することが好ましい。
本開示の押出成形品は、チューブまたはホースであることが好ましい。
また、本開示によれば、架橋させる際の収縮を抑制することができる押出成形品を提供することができる。
フッ素ゴム層は、フッ素ゴム組成物から形成される層である。フッ素ゴム層は、通常、フッ素ゴム組成物を成形して未架橋フッ素ゴム層を得た後、架橋処理して得られるものである。
フッ素ゴムは、通常、主鎖を構成する炭素原子に結合しているフッ素原子を有し、且つゴム弾性を有する非晶質の重合体からなる。上記フッ素ゴムは、1種の重合体からなるものであってもよいし、2種以上の重合体からなるものであってもよい。フッ素ゴムは、通常、明確な融点を有さないものである。
VdFおよび含フッ素エチレン性単量体単位(a)と共重合可能な単量体由来の共重合単位(但し、VdF単位は除く。)は、VdF単位と含フッ素エチレン性単量体(a)由来の共重合単位の合計量に対して、0~10モル%であることが好ましい。
CHX1=CX2Rf1 (1)
(式中、X1およびX2は、一方がHであり、他方がFであり、Rf1は、炭素数1~12の直鎖または分岐したフルオロアルキル基)で表される化合物、一般式(2):
CFX=CXOCF2OR1 (2)
(式中、Xは、同一または異なり、H、FまたはCF3を表し、R1は、直鎖または分岐した、H、Cl、BrおよびIからなる群より選択される少なくとも1種の原子を1~2個含んでいてもよい炭素数が1~6のフルオロアルキル基、若しくは、H、Cl、BrおよびIからなる群より選択される少なくとも1種の原子を1~2個含んでいてもよい炭素数が5または6の環状フルオロアルキル基を表す。)で表されるフルオロビニルエーテルなどの含フッ素単量体が挙げられる。これらのなかでも、CH2=CFCF3、式(2)で表されるフルオロビニルエーテル、TFE、HFPおよびPAVEからなる群より選択される少なくとも1種であることが好ましく、TFE、HFPおよびPAVEからなる群より選択される少なくとも1種であることがより好ましい。
CF2=CFO(CF2CFY1O)p-(CF2CF2CF2O)q-Rf (3)
(式中、Y1はFまたはCF3を表し、Rfは炭素数1~5のパーフルオロアルキル基を表す。pは0~5の整数を表し、qは0~5の整数を表す。)で表される化合物であることが好ましい。
PAVEとしては、パーフルオロ(メチルビニルエーテル)またはパーフルオロ(プロピルビニルエーテル)であることがより好ましく、パーフルオロ(メチルビニルエーテル)であることが更に好ましい。これらをそれぞれ単独で、または任意に組み合わせて用いることができる。
R2IxBry
(式中、xおよびyはそれぞれ0~2の整数であり、かつ1≦x+y≦2を満たすものであり、R2は、炭素数1~16の飽和若しくは不飽和のフルオロ炭化水素基、炭素数1~16の飽和若しくは不飽和のクロロフルオロ炭化水素基、炭素数1~3の炭化水素基、または、ヨウ素原子若しくは臭素原子で置換されていてもよい炭素数3~10の環状炭化水素基であり、これらは酸素原子を含んでいてもよい)で表される化合物が挙げられる。
ムーニー粘度は、ASTM-D1646に準拠して測定することができる。
測定機器:ALPHA TECHNOLOGIES社製のMV2000E型
ローター回転数:2rpm
測定温度:100℃
フッ素ゴム組成物は、ポリテトラフルオロエチレン(PTFE)を含有する。
さらに、上記の範囲内の比表面積を有するPTFEを用いることによって、フッ素ゴム中にPTFEを単一粒子の状態で容易に分散させることができる。
CF2=CF-ORf (I)
(式中、Rfは、パーフルオロ有機基を表す。)で表されるパーフルオロ不飽和化合物などが挙げられる。本明細書において、上記「パーフルオロ有機基」とは、炭素原子に結合する水素原子が全てフッ素原子に置換されてなる有機基を意味する。上記パーフルオロ有機基は、エーテル酸素を有していてもよい。
(式中、nは、1~4の整数を表す。)で表される基であるものなどが挙げられる。
フッ素ゴム組成物は、塩基性の多官能化合物を含有し、これによって、フッ素ゴム層とポリマー層とがより強固に接着する。塩基性の多官能化合物は、1つの分子中に同一または異なる構造の2つ以上の官能基を有し、塩基性を示す化合物である。
フッ素ゴム組成物は、リン化合物を含有してもよい。フッ素ゴム組成物がリン化合物を含有することによって、フッ素ゴム層とポリマー層とが一層強固に接着する。リン化合物は、1分子中に少なくとも1つのリン原子を含む化合物であり、たとえば、ホスフィン類、リン酸エステル類、ホスファゼン類、ホスフィンオキシド類、ホスホン酸エステル類、ホスフィン酸エステル類などが挙げられる。
フッ素ゴム組成物は、シリカを含有してもよい。フッ素ゴム組成物がシリカを含有することによって、フッ素ゴム層とポリマー層とが一層強固に接着する。シリカとしては、塩基性シリカ、酸性シリカを用いることができ、接着性の観点から、塩基性シリカを用いる方が好ましい。塩基性シリカとしては、カープレックス1120(DSLジャパン社製)、Sidistar R300(エルケム社製)、Silene732D(PPG Industries社製)、Inhibisil75(PPG Industries社製)などが挙げられる。また、フッ素ゴム層とポリマー層が一層強固に接着することから、平均粒径が大きなシリカを用いることが好ましい。平均粒径が大きなシリカとしては、Sidistar R300(エルケム社製)、Sidistar T120U(エルケム社製)、アドマファインシリーズ(アドマテックス社製)、エクセリカシリーズ(トクヤマ社製)などが挙げられる。
フッ素ゴム組成物は、フッ素ゴム層とポリマー層とがより強固に接着することから、さらに、架橋剤を含むことも好ましい。架橋剤としては、パーオキサイド架橋剤などを目的に応じて選択することができる。上記フッ素ゴム組成物は、パーオキサイド架橋剤を含むことが好ましい。
ポリマー層とは、フッ素ゴム層とは異なる層であって、ポリマー(ただし、フッ素ゴムを除く)から形成される層である。
(フッ素樹脂シートの作製方法)
樹脂ペレットを、それぞれ、直径120mmの金型に入れ、300℃に加熱したプレス機にセットし、約2.9MPaの圧力で溶融プレスして、厚さ0.12mmのフッ素樹脂シートを得、そのシートを直径45mm、厚み120μmに加工する。
CTFE/TFE/PAVE共重合体とは、実質的にCTFE、TFEおよびPAVEのみからなる共重合体である。
CTFE/TFE/PAVE共重合体において、PAVE単位は、全単量体単位の0.5モル%以上であることが好ましく、5モル%以下であることが好ましい。
フッ素ゴム層の厚みは限定されないが、たとえば、100μm以上であることが好ましい。フッ素ゴム層の厚みの上限としては、たとえば、5000μmである。
ゴム混練り装置としては、ロール、ニーダー、バンバリーミキサー、インターナルミキサー、二軸押し出し機などを用いることができる。
混合は、フッ素ゴムと、塩基性の多官能化合物と、ポリテトラフルオロエチレンとに加え、必要に応じて、架橋剤、架橋助剤、共架橋剤、架橋促進剤、充填剤などのその他添加剤とともに混合するものであってよい。
混合の温度は、たとえば、20~200℃である。また、上記混合の時間は、たとえば、2~80分である。
本開示の積層体は、上述したフッ素ゴム層(以下、フッ素ゴム層(A)ということがある)および上述したポリマー層(以下、ポリマー層(B)ということがある)を備える。
基本構造であり、従来、ポリマー層(B)とフッ素ゴム層(A)を積層させるには、層間(フッ素ゴム層-フッ素樹脂層)の接着が不充分なため、樹脂側において表面処理を施したり、別途接着剤を層間に塗布したり、テープ状のフィルムを巻き付けて固定したりなどと工程が複雑になりがちであったが、そのような複雑な工程を組まずに、架橋することにより架橋接着が起こり化学的に強固な接着が得られる。
フッ素ゴム層(A)-ポリマー層(B)-フッ素ゴム層(A)の3層構造、および、フッ素ゴム層(A)-ポリマー層(B)-ゴム層(C1)の3層構造がある。
シール性が要求される場合、たとえば燃料配管などの接合部は、シール性保持のためにゴム層を両側に配置することが望ましい。内外層のゴム層は同じ種類であっても、違う種類であってもよい。
フッ素ゴム層(A)-ポリマー層(B)-ゴム層(C1)の3層構造の場合、ゴム層(C1)は、アクリロニトリルブタジエンゴム、水素化アクリロニトリルブタジエンゴム、エピクロルヒドリンゴム、または、アクリロニトリルブタジエンゴムとアクリル系ゴムの混合物からなる層であることが好ましい。
また、燃料配管をフッ素ゴム層(A)-ポリマー層(B)-ゴム層(C1)の3層構造とし、ゴム層(C1)としてフッ素ゴム層を設け、ゴム層(C1)を配管の内層にすることにより、耐薬品性、燃料低透過性が向上する。
ポリマー層(B)-フッ素ゴム層(A)-ポリマー層(B)の3層構造が挙げられる。内外層の樹脂層は同じ種類であっても、違う種類であってもよい。
(2)~(4)の3層構造に加えて、さらに任意のフッ素ゴム層(A)またはゴム層(C1)、ポリマー層(B)を目的に応じて積層してもよい。また、金属箔などの層を設けてもよいし、フッ素ゴム層(A)とポリマー層(B)との層間以外には接着剤層を介在させてもよい。
また、耐圧向上の目的で、補強糸などの補強層を適宜設けてもよい。
レーザー回折式粒度分布測定装置(日本レーザー社製)を用い、カスケードは使用せず、圧力0.1MPa、測定時間3秒で粒度分布を測定し、得られた粒度分布積算の50%に対応する値を平均粒径とした。
BET法により、表面分析計(商品名:BELSORP-miniII、マイクロトラック・ベル社製)を用いて測定した。尚、キャリアガスとして、窒素30%、ヘリウム70%の混合ガスを用い、冷却は液体窒素を用いて行った。
エスアイアイ・ナノテクノロジー社製の示差走査熱量測定機RDC220(DSC)を用い、事前に標準サンプルとして、インジウム、鉛を用いて温度校正した上で、PTFE粉末約3mgをアルミ製パン(クリンプ容器)に入れ、200ml/分のエアー気流下で、250~380℃の温度領域を10℃/分で昇温させて示差走査熱量測定を行い、上記領域における融解熱量の極小点を融点とした。
ASTM D 1238に準拠し、フローテスター(島津製作所社製)および2φ-8Lのダイを用い、予め380℃で5分間加熱しておいた2gの試料を0.7MPaの荷重にて上記温度に保って測定を行った。
熱風循環式電気炉中で、PTFEを300℃で2時間加熱して、加熱前の試料の質量に対する加熱後の試料の減量の割合を算出した。
19F-NMR分析により測定した。
CTFE/TFE/PPVE共重合体のMFRは、メルトインデクサー(東洋精機製作所社製)を用い、297℃、5kg加重下で直径2mm、長さ8mmのノズルから単位時間(10分間)に流出するポリマーの重量(g)を測定した。
CTFE/TFE/PPVE共重合体のペレットを、直径120mmの金型に入れ、300℃に加熱したプレス機にセットし、約2.9MPaの圧力で溶融プレスして、厚さ0.12mmのシートを得た。得られたシートを、直径45mm、厚み120μmのシートに加工した。CE10(イソオクタンとトルエンとの容量比50:50の混合物にエタノール10容量%を混合した燃料)を18mL投入した内径40mmφ、高さ20mmのSUS316製の透過係数測定用カップに得られたシートを組み入れ、60℃における質量変化を1000時間まで測定した。時間あたりの質量変化(測定初期における質量変化が一定の部分)、接液部のシートの表面積およびシートの厚さから燃料透過係数(g・mm/m2/day)を算出した。
得られた積層体を幅10mm×長さ40mm×3セットの短冊状に切断し、フッ素樹脂シートを剥がして掴みしろとした試料片を作成した。この試験片について、フッ素ゴム層とフッ素樹脂層との境界面の接着強度を含まず、接着面のみの接着強度を測定するために、フッ素ゴム層とフッ素樹脂層の界面を一度ゆっくりと手で引っ張ることにより2~3mm掴みしろを増やしてから、オートグラフ(島津製作所社製 AGS-J 5kN)を使用して、JIS K-6256(加硫ゴムの接着試験方法)に記載の方法に準拠し、25℃において50mm/minの引張速度で剥離試験を行い、接着強度を測定し、得られたN=3のデータの平均値を算出した。
実施例および比較例で作製したフッ素ゴムシートを押出し方向に対して、幅70mm×長さ40mmに切断し、得られた試験片を、電気炉加熱により、170℃で30分間架橋させた。架橋後の試験片の長さを測定して、次式により収縮率を算出した。
収縮率(%)=(架橋前の試験片の長さ-架橋後の試験片の長さ)/(架橋前の試験片の長さ)
(フッ素樹脂シートの作製)
以下の物性を有するCTFE/TFE/PPVE共重合体を、280℃で10分プレスすることによって、フッ素樹脂シート(厚み0.12mm)を作製した。
CTFE/TFE/PPVE=21.3/76.3/2.4(モル%)
MFR=29.2g/10分
燃料透過係数=0.4g・mm/m2/day
フッ素ゴム組成物の作製に用いた材料の詳細を以下に示す。
カーボンブラック:Thermax N-990、カンカーブ社製
架橋助剤:トリアリルイソシアヌレート(TAIC)、日本化成社製
架橋剤:パーオキサイド架橋剤、パーヘキサ25B、日油社製
塩基性多官能化合物:N,N’-ジシンナミリデン-1,6-ヘキサメチレンジアミン(V-3)、ダイキン工業社製
ホスフィン:クロロジフェニルホスフィン、東京化成工業社製
シリカ:Sidistar R300、エルケム社製
表2に示す材料を、8インチオープンロールを用いて混練することにより、約2mmの厚みのシート状のフッ素ゴム組成物(フッ素ゴムシート)を得た。
厚み約2mmのフッ素ゴムシートと、厚み約0.12mmのフッ素樹脂シートを重ね合わせ、片方の端部に幅約50mmのフッ素樹脂フィルム(厚さ10μm)を両シートの間に挟んだ後、170℃で30分間プレスすることにより、シート状の積層体を得た。結果を表2に示す。
さらに、実施例2以外の実施例においても、実施例2と同様に、フッ素ゴム中に単一粒子の状態でPTFEが分散していることが確認された。各実施例のフッ素ゴムシートは、各比較例のフッ素ゴムシートと比較して、架橋の際のフッ素ゴムシートの収縮率が非常に低いことが分かる。
また、以上の結果から、フッ素ゴム層中で単一粒子の状態でPTFEを分散させることによって、架橋させる際の収縮を抑制することができる押出成形品を提供できることが分かる。
Claims (14)
- フッ素ゴム層とポリマー層とを備える積層体であって、
前記フッ素ゴム層が、フッ素ゴム、塩基性の多官能化合物、および、ポリテトラフルオロエチレンを含有するフッ素ゴム組成物から形成されており、
前記ポリテトラフルオロエチレンが、前記フッ素ゴム層中で単一粒子の状態で分散している積層体。 - フッ素ゴム層とポリマー層とを備える積層体であって、
前記フッ素ゴム層が、フッ素ゴム、塩基性の多官能化合物、および、ポリテトラフルオロエチレンを含有するフッ素ゴム組成物から形成されており、
前記ポリテトラフルオロエチレンの比表面積が8m2/g未満であり、前記ポリテトラフルオロエチレンの平均粒径が、0.01~1000μmであり、前記ポリテトラフルオロエチレンの380℃における溶融粘度が、1×10 1 ~7×10 5 Pa・sである積層体。 - 前記ポリテトラフルオロエチレンの380℃における溶融粘度が、1×101~7×105Pa・sである請求項1に記載の積層体。
- 前記フッ素ゴム組成物が、さらに、パーオキサイド架橋剤を含有する請求項1~3のいずれかに記載の積層体。
- 前記ポリマー層が、フッ素樹脂を含有する請求項1~4のいずれかに記載の積層体。
- 前記フッ素樹脂の燃料透過係数が2.0g・mm/m2/day以下である請求項5に記載の積層体。
- 前記フッ素ゴム層と前記ポリマー層とが直接接着している請求項1~6のいずれかに記載の積層体。
- チューブまたはホースである請求項1~7のいずれかに記載の積層体。
- フッ素ゴム、および、ポリテトラフルオロエチレンを含有する押出成形品であって、前記ポリテトラフルオロエチレンが前記押出成形品中で単一粒子の状態で分散しており、チューブまたはホースである押出成形品。
- フッ素ゴム、および、ポリテトラフルオロエチレンを含有する押出成形品であって、前記ポリテトラフルオロエチレンの比表面積が8m2/g未満であり、前記ポリテトラフルオロエチレンの平均粒径が、0.01~1000μmであり、前記ポリテトラフルオロエチレンの380℃における溶融粘度が、1×10 1 ~7×10 5 Pa・sであり、チューブまたはホースである押出成形品。
- 前記ポリテトラフルオロエチレンの380℃における溶融粘度が、1×101~7×105Pa・sである請求項9に記載の押出成形品。
- 前記フッ素ゴム、前記ポリテトラフルオロエチレンおよび塩基性の多官能化合物を含有するフッ素ゴム組成物から形成される請求項9~11のいずれかに記載の押出成形品。
- 前記フッ素ゴム組成物が、さらに、パーオキサイド架橋剤を含有する請求項12に記載の押出成形品。
- 請求項9~13のいずれかに記載の押出成形品から形成されるフッ素ゴム層と、ポリマー層とを備える押出積層体。
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