JP7044994B1 - 共重合体、射出成形体、被圧縮部材および被覆電線 - Google Patents
共重合体、射出成形体、被圧縮部材および被覆電線 Download PDFInfo
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- JP7044994B1 JP7044994B1 JP2021161368A JP2021161368A JP7044994B1 JP 7044994 B1 JP7044994 B1 JP 7044994B1 JP 2021161368 A JP2021161368 A JP 2021161368A JP 2021161368 A JP2021161368 A JP 2021161368A JP 7044994 B1 JP7044994 B1 JP 7044994B1
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Classifications
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08F114/26—Tetrafluoroethene
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08F—MACROMOLECULAR COMPOUNDS OBTAINED BY REACTIONS ONLY INVOLVING CARBON-TO-CARBON UNSATURATED BONDS
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- C08L—COMPOSITIONS OF MACROMOLECULAR COMPOUNDS
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- C08L27/02—Compositions of homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Compositions of derivatives of such polymers not modified by chemical after-treatment
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
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- C09D127/00—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers
- C09D127/02—Coating compositions based on homopolymers or copolymers of compounds having one or more unsaturated aliphatic radicals, each having only one carbon-to-carbon double bond, and at least one being terminated by a halogen; Coating compositions based on derivatives of such polymers not modified by chemical after-treatment
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- C—CHEMISTRY; METALLURGY
- C09—DYES; PAINTS; POLISHES; NATURAL RESINS; ADHESIVES; COMPOSITIONS NOT OTHERWISE PROVIDED FOR; APPLICATIONS OF MATERIALS NOT OTHERWISE PROVIDED FOR
- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
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- C—CHEMISTRY; METALLURGY
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- C09K—MATERIALS FOR MISCELLANEOUS APPLICATIONS, NOT PROVIDED FOR ELSEWHERE
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- H01B3/18—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances
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- H01B3/443—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from vinylhalogenides or other halogenoethylenic compounds
- H01B3/445—Insulators or insulating bodies characterised by the insulating materials; Selection of materials for their insulating or dielectric properties mainly consisting of organic substances plastics; resins; waxes vinyl resins; acrylic resins from vinylhalogenides or other halogenoethylenic compounds from vinylfluorides or other fluoroethylenic compounds
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- H01M—PROCESSES OR MEANS, e.g. BATTERIES, FOR THE DIRECT CONVERSION OF CHEMICAL ENERGY INTO ELECTRICAL ENERGY
- H01M50/00—Constructional details or processes of manufacture of the non-active parts of electrochemical cells other than fuel cells, e.g. hybrid cells
- H01M50/10—Primary casings, jackets or wrappings of a single cell or a single battery
- H01M50/183—Sealing members
- H01M50/19—Sealing members characterised by the material
- H01M50/198—Sealing members characterised by the material characterised by physical properties, e.g. adhesiveness or hardness
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- B29K2027/00—Use of polyvinylhalogenides or derivatives thereof as moulding material
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Abstract
Description
I:吸光度
K:補正係数
t:フィルムの厚さ(mm)
150℃面圧(MPa)=(t2-t1)/t1×E’
t1:圧縮変形させる前の試験片の元の高さ(mm)×50%
t2:圧縮変形させた後の試験片の高さ(mm)
E’:150℃での貯蔵弾性率(MPa)
ジノルマルプロピルパーオキシジカーボネート、ジイソプロピルパーオキシジカーボネート、ジsec-ブチルパーオキシジカーボネート、ジ-2-エトキシエチルパーオキシジカーボネートなどのジアルキルパーオキシカーボネート類;
t-ブチルパーオキシイソブチレート、t-ブチルパーオキシピバレートなどのパーオキシエステル類;
ジt-ブチルパーオキサイドなどのジアルキルパーオキサイド類;
ジ[フルオロ(またはフルオロクロロ)アシル]パーオキサイド類;
などが代表的なものとしてあげられる。
食品包装用フィルム、食品製造工程で使用する流体移送ラインのライニング材、パッキン、シール材、シート等の食品製造装置用流体移送部材;
薬品用の薬栓、包装フィルム、薬品製造工程で使用される流体移送ラインのライニング材、パッキン、シール材、シート等の薬液移送部材;
化学プラントや半導体工場の薬液タンクや配管の内面ライニング部材;
自動車の燃料系統並びに周辺装置に用いられるO(角)リング・チューブ・パッキン、バルブ芯材、ホース、シール材等、自動車のAT装置に用いられるホース、シール材等の燃料移送部材;
自動車のエンジン並びに周辺装置に用いられるキャブレターのフランジガスケット、シャフトシール、バルブステムシール、シール材、ホース等、自動車のブレーキホース、エアコンホース、ラジエーターホース、電線被覆材等のその他の自動車部材;
半導体製造装置のO(角)リング、チューブ、パッキン、バルブ芯材、ホース、シール材、ロール、ガスケット、ダイヤフラム、継手等の半導体装置用薬液移送部材;
塗装設備用の塗装ロール、ホース、チューブ、インク用容器等の塗装・インク用部材;
飲食物用のチューブ又は飲食物用ホース等のチューブ、ホース、ベルト、パッキン、継手等の飲食物移送部材、食品包装材、ガラス調理機器;
廃液輸送用のチューブ、ホース等の廃液輸送用部材;
高温液体輸送用のチューブ、ホース等の高温液体輸送用部材;
スチーム配管用のチューブ、ホース等のスチーム配管用部材;
船舶のデッキ等の配管に巻き付けるテープ等の配管用防食テープ;
電線被覆材、光ファイバー被覆材、太陽電池の光起電素子の光入射側表面に設ける透明な表面被覆材および裏面剤等の各種被覆材;
ダイヤフラムポンプのダイヤフラムや各種パッキン類等の摺動部材;
農業用フィルム、各種屋根材・側壁等の耐侯性カバー;
建築分野で使用される内装材、不燃性防火安全ガラス等のガラス類の被覆材;
家電分野等で使用されるラミネート鋼板等のライニング材;
本開示の共重合体は高い貯蔵弾性率(E’)を有するため、共重合体を含有する被覆層は、長期間の使用にも耐えることができる。
さらに、本開示の共重合体は、欠陥が少ない被覆層を形成することができ、被覆する心線を腐食させにくく、スパークを生じさせるような被覆層の欠陥数が増加するなどの成形不良も発生させにくく、電気特性にも優れている。したがって、本開示の共重合体を含有する被覆層を備える被覆電線は、電気特性に優れており、被覆層の絶縁特性にも優れている。被覆層が高温でも軟化しにくいため、高温においても優れた電気特性を維持することができる。
近年、より過酷な作業環境で使用できる、言い換えると260℃を超える連続使用温度を有する共重合体が必要とされている。油田やガス田における数多くの現実世界の工業用途においては、建設工事などで遭遇する極度に高い作動温度に耐えるために、260℃を超える連続使用温度を有する溶融加工可能なポリマー材料を有する必要性が生じつつある。例えば、深掘を行う場合、データ通信ケーブルは、ダウンホール坑井内で280℃以上の温度に曝露させられる可能性がある。
本開示の共重合体を含有する成形体は、280℃の連続使用温度を有することを可能にする。本開示の共重合体を含有する成形体は、280℃という極めて高い温度においても融解することなく、成形体からなる被覆層が熱負荷に起因する破裂若しくは割れ目を形成せず被覆を保ち、連続的に使用できる。そのため、本開示の共重合体を含有する成形体は、最高温度が280℃以上となる環境で用いられる被覆電線が備える、被覆層としての使用に適する。
各単量体単位の含有量は、NMR分析装置(たとえば、ブルカーバイオスピン社製、AVANCE300 高温プローブ)により測定した。
ASTM D1238に従って、メルトインデクサーG-01(東洋精機製作所社製)を用いて、372℃、5kg荷重下で内径2.1mm、長さ8mmのノズルから10分間あたりに流出するポリマーの質量(g/10分)を求めた。
共重合体のペレットを、コールドプレスにより成形して、厚さ0.25~0.30mmのフィルムを作製した。このフィルムをフーリエ変換赤外分光分析装置〔FT-IR(Spectrum One、パーキンエルマー社製)〕により40回スキャンし、分析して赤外吸収スペクトルを得、完全にフッ素化されて官能基が存在しないベーススペクトルとの差スペクトルを得た。この差スペクトルに現れる特定の官能基の吸収ピークから、下記式(A)に従って試料における炭素原子1×106個あたりの官能基数Nを算出した。
N=I×K/t (A)
I:吸光度
K:補正係数
t:フィルムの厚さ(mm)
参考までに、本開示における官能基について、吸収周波数、モル吸光係数および補正係数を表2に示す。モル吸光係数は低分子モデル化合物のFT-IR測定データから決定したものである。
示差走査熱量計(商品名:X-DSC7000、日立ハイテクサイエンス社製)を用いて、昇温速度10℃/分で200℃から350℃までの1度目の昇温を行い、続けて、冷却速度10℃/分で350℃から200℃まで冷却し、再度、昇温速度10℃/分で200℃から350℃までの2度目の昇温を行い、2度目の昇温過程で生ずる溶融曲線のピークから融点を求めた。
動的粘弾性装置DVA-220(アイティー計測制御社製)を用いた動的粘弾性測定を行い求めた。昇温速度2℃/分、周波数10Hzで測定し、tanδ値のピークにおける温度をガラス転移温度として求めた。
174L容積のオートクレーブに純水51.8Lを投入し、充分に窒素置換を行った後、パーフルオロシクロブタン40.9kgとパーフルオロ(プロピルビニルエーテル)(PPVE)1.49kg、メタノール4.00kgとを仕込み、系内の温度を35℃、攪拌速度を200rpmに保った。次いで、テトラフルオロエチレン(TFE)を0.64MPaまで圧入した後、ジ-n-プロピルパーオキシジカーボネートの50%メタノール溶液0.103kgを投入して重合を開始した。重合の進行とともに系内圧力が低下するので、TFEを連続供給して圧力を一定にし、PPVEをTFEの供給1kg毎に0.036kg追加投入した。TFEの追加投入量が40.9kgに達したところで重合を終了させた。未反応のTFEを放出して、オートクレーブ内を大気圧に戻した後、得られた反応生成物を水洗、乾燥して42.4kgの粉末を得た。
PPVEを1.55kg、メタノールを4.30kg、PPVEをTFEの供給1kg毎に0.037kg追加投入に変更した以外は、実施例1と同様にしてペレットを得た。
PPVEを1.60kg、メタノールを3.90kg、PPVEをTFEの供給1kg毎に0.038kg追加投入に変更し、乾燥粉末42.5kgを得た以外は、実施例1と同様にしてペレットを得た。
PPVEを1.66kg、メタノールを3.59kg、PPVEをTFEの供給1kg毎に0.040kg追加投入に変更し、乾燥粉末42.5kgを得た以外は、実施例1と同様にしてペレットを得た。
174L容積のオートクレーブに純水26.6Lを投入し、充分に窒素置換を行った後、パーフルオロシクロブタン30.4kgとパーフルオロ(プロピルビニルエーテル)(PPVE)0.93kg、メタノール4.51kgとを仕込み、系内の温度を35℃、攪拌速度を200rpmに保った。次いで、テトラフルオロエチレン(TFE)を0.58MPaまで圧入した後、ジ-n-プロピルパーオキシジカーボネートの50%メタノール溶液0.021kgを投入して重合を開始した。重合の進行とともに系内圧力が低下するので、TFEを連続供給して圧力を一定にし、PPVEをTFEの供給1kg毎に0.035kg追加して8時間重合を継続した。TFEを放出して、オートクレーブ内を大気圧に戻した後、得られた反応生成物を水洗、乾燥して15kgの粉末を得た。
PPVEを1.29kg、メタノールを4.72kg、PPVEをTFEの供給1kg毎に0.033kg追加投入に変更し、乾燥粉末42.3kgを得た以外は、実施例1と同様にしてペレットを得た。
PPVEを1.85kg、メタノールを3.46kg、PPVEをTFEの供給1kg毎に0.043kg追加投入に変更し、乾燥粉末42.6kgを得た以外は、実施例1と同様にしてペレットを得た。
PPVEを1.55kg、メタノールを4.88kg、PPVEをTFEの供給1kg毎に0.037kg追加投入に変更した以外は、実施例1と同様にしてペレットを得た。
PPVEを1.66kg、メタノールを3.10kg、PPVEをTFEの供給1kg毎に0.040kg追加投入に変更し、乾燥粉末42.5kgを得た以外は、実施例1と同様にしてペレットを得た。
ペレットおよびヒートプレス成形機を用いて、厚さ約0.2mmのシート状試験片を作製した。試験カップ(透過面積12.56cm2)内に水を18g入れ、シート状試験片で覆い、PTFEガスケットを挟んで締め付け、密閉した。シート状試験片と水が接するようにして、温度95℃で30日間保持した後取出し、室温で2時間放置後に質量減少量を測定した。次式により、水蒸気透過度(g・cm/m2)を測定した。
水蒸気透過度(g・cm/m2)=質量減少量(g)×シート状試験片の厚さ(cm)/透過面積(m2)
DVA-220(アイティー計測制御社製)を用いた動的粘弾性測定を行い求めた。サンプル試験片として、長さ25mm、幅5mm、厚み0.2mmのヒートプレス成形シートを用いて、昇温速度2℃/分、周波数10Hz条件下で、30℃~250℃の範囲で測定を行い、150℃の貯蔵弾性率(MPa)を読み取った。
金型(内径13mm、高さ38mm)に、上記ペレットを約2g投入した状態で、熱板プレスにて370℃で30分間溶融後、圧力0.2MPa(樹脂圧)で加圧しながら水冷して、高さ約8mmの成形体を作製した。その後、得られた成形体を切削することにより、外径13mm、高さ6mmの試験片を作製した。
復元量(mm)=t2-t1
t1:スペーサの高さ(mm)
t2:圧縮装置から取り外した試験片の高さ(mm)
上記の試験においては、t1=3mmである。
150℃での圧縮試験の結果と150℃における貯蔵弾性率測定の結果から、次式により150℃面圧を求めた。
150℃面圧(MPa)=(t2-t1)/t1×E’
t1:スペーサの高さ(mm)
t2:圧縮装置から取り外した試験片の高さ(mm)
E’:150℃での貯蔵弾性率(MPa)
ペレットおよびヒートプレス成形機を用いて、厚さ約0.1mmのシート状試験片を作製した。得られた試験片を用い、JIS K7126-1:2006に記載の方法に従って、差圧式ガス透過度計(L100-5000型ガス透過度計、Systech illinois社製)を用いて、二酸化炭素透過度の測定を行った。透過面積50.24cm2、試験温度70℃、試験湿度0%RHでの二酸化炭素透過度の数値を得た。得られた二酸化炭素透過度と試験片厚みを用いて、次式より二酸化炭素透過係数を算出した。
二酸化炭素透過係数(cm3・mm/(m2・h・atm))=GTR×d
GTR:二酸化炭素透過度(cm3/(m2・h・atm))
d:試験片厚み(mm)
ペレットおよびヒートプレス成形機を用いて、厚さ約2mmのシートを作製した。13.5mm×38mmの長方形ダンベルを用いて、得られたシートを打ち抜くことにより、3個の試験片を得た。得られた各試験片の長辺の中心に、ASTM D1693に準じて、19mm×0.45mmの刃でノッチを入れた。100mLポリプロピレン製ボトルに、ノッチ試験片3個とエタノール25gを入れ、電気炉にて60℃で720時間加熱後、ノッチ試験片を取り出した。得られたノッチ試験片3個をASTM D1693に準じた応力亀裂試験治具に取り付け、ノッチおよびその周辺を目視で観察し、亀裂の数を数えた。
○:亀裂の数が0個である
×:亀裂の数が1個以上である
各実施例及び比較例で得られたペレットと、平均粒子径が13.5μmの窒化ホウ素(BN)とを用いて、国際公開第03/000972号の実施例に記載の方法と同様にして、BN含有量が、ペレットおよびBNの合計量の0.75重量%となる組成物を作成した。
CAPAC300 19C(Zumbach社製)を用いてオンラインでキャパシタンスを測定した。発泡率は、オンラインのキャパシタンスで管理した。
a)芯導体:軟鋼線導体径0.6mm
b)被覆厚み:0.25mm
c)被覆電線径:1.1mm
d)電線引取速度:80m/分)
e)押出条件:
・シリンダ軸径=35mm,L/D=32の単軸押出成形機
・ダイ(内径)/チップ(外径)=4.7mm/2.2mm
押出機の設定温度:バレル部C-1(330℃)、バレル部C-2(360℃)、バレル部C-3(370℃)、ヘッド部H-1(375℃)、ヘッド部H-2(365℃)、ヘッド部H-3(360℃)。心線予備加熱は90℃に設定した。
f)窒素圧力:30MPa
g)窒素流量:15cc/min
h)キャパシタンス:150±3pF/m
オンラインで、Beta LaserMike Sparktester HFS1220を用いて1500Vの電圧でスパークの測定をした。
4500mあたりのスパーク数が、1の場合を良好、0の場合を最良、2以上の場合を不合格とした。
射出成形機(住友重機械工業社製、SE50EV-A)を使用し、シリンダ温度を390℃、金型温度を190℃、射出速度130mm/sとして、共重合体を射出成形した。金型として、HPM38にCrめっきを施した金型(15mm×15mm×0.6mmtの4個取り)を用いた。得られた射出成形体の表面を目視で観察し、表面平滑性を以下の基準で評価した。
◎:表面に荒れが観察されず平滑である
○:金型のゲート付近に位置していた部分の表面のみに荒れが観察される
×:表面の大部分に荒れが観察される
Claims (5)
- テトラフルオロエチレン単位およびパーフルオロ(プロピルビニルエーテル)単位を含有し、
パーフルオロ(プロピルビニルエーテル)単位の含有量が、全単量体単位に対して、3.4~3.9質量%であり、
メルトフローレートが、29~36g/10分であり、
官能基数が、主鎖炭素数10 6 個あたり、50個超である
共重合体。 - 請求項1に記載の共重合体を含有する封止具。
- 請求項1に記載の共重合体を含有する射出成形体。
- 請求項1に記載の共重合体を含有する被圧縮部材。
- 請求項1に記載の共重合体を含有する被覆層を備える被覆電線。
Applications Claiming Priority (2)
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