JP6962196B2 - ポリアミド樹脂製複合成形品およびその製造方法 - Google Patents
ポリアミド樹脂製複合成形品およびその製造方法 Download PDFInfo
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- JP6962196B2 JP6962196B2 JP2017548238A JP2017548238A JP6962196B2 JP 6962196 B2 JP6962196 B2 JP 6962196B2 JP 2017548238 A JP2017548238 A JP 2017548238A JP 2017548238 A JP2017548238 A JP 2017548238A JP 6962196 B2 JP6962196 B2 JP 6962196B2
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- polyamide resin
- fiber
- molded product
- polyamide
- base material
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Description
[1]強化繊維基材に含浸用ポリアミド樹脂を含浸させた繊維強化ポリアミド樹脂基材と、ポリアミド樹脂組成物からなるポリアミド樹脂成形品とが、少なくとも一部で接合した複合成形品であって、前記含浸用ポリアミド樹脂の溶融必要熱量(前記繊維強化ポリアミド樹脂基材を熱アニール処理した場合は、該熱アニール処理後の繊維強化ポリアミド樹脂基材から算出した溶融必要熱量とする)が300<Q<425(J/g)であり、Fedorsの式から算出される前記含浸用ポリアミド樹脂の溶解度パラメータ(SP値)が11<σ<13.2((cal/cm3)1/2)であるポリアミド樹脂製複合成形品。
[2]前記含浸用ポリアミド樹脂が、ポリアミド6成分30〜90重量%とポリアミド66成分70〜10重量%とからなるポリアミド共重合体を含む[1]に記載のポリアミド樹脂製複合成形品。
[3]前記ポリアミド樹脂組成物がポリアミド樹脂100重量部に対し、充填材10〜250重量部を含む[1]または[2]のいずれかに記載のポリアミド樹脂製複合成形品。
[4]前記ポリアミド樹脂組成物の主成分がポリアミド6樹脂である[1]〜[3]のいずれかに記載のポリアミド樹脂製複合成形品。
[5]前記強化繊維基材が一方向に配列した連続の強化繊維からなる[1]〜[4]のいずれかに記載のポリアミド樹脂製複合成形品。
[6]前記強化繊維が炭素繊維であり、前記繊維強化ポリアミド樹脂基材中の繊維含有量が10〜70体積%である[5]に記載のポリアミド樹脂製複合成形品。
[7]強化繊維基材に含浸用ポリアミド樹脂を含浸させた繊維強化ポリアミド樹脂基材を予め金型内に配置し、該金型にポリアミド樹脂組成物を射出成形して溶融接合するポリアミド樹脂製複合成形品の製造方法であって、前記含浸用ポリアミド樹脂の溶融必要熱量(前記繊維強化ポリアミド樹脂基材を熱アニール処理した場合は、該熱アニール処理後の繊維強化ポリアミド樹脂基材から算出した溶融必要熱量とする)が300<Q<425(J/g)であり、Fedorsの式から算出される前記含浸用ポリアミド樹脂の溶解度パラメータ(SP値)が11<σ<13.2((cal/cm3)1/2)であるポリアミド樹脂製複合成形品の製造方法。
[8]前記含浸用ポリアミド樹脂が、ポリアミド6成分30〜90重量%とポリアミド66成分70〜10重量%とからなるポリアミド共重合体を含む[7]に記載のポリアミド樹脂製複合成形品の製造方法。
[9]前記ポリアミド樹脂組成物が、ポリアミド樹脂100重量部に対し、充填材10〜250重量部を含む[7]または[8]に記載のポリアミド樹脂製複合成形品の製造方法。
[10]前記ポリアミド樹脂組成物の主成分がポリアミド6樹脂である請求項[7]〜[9]のいずれかに記載のポリアミド樹脂製複合成形品の製造方法。
[11]前記強化繊維基材が一方向に配列した連続の強化繊維からなる請求項[7]〜[10]のいずれかに記載のポリアミド樹脂製複合成形品の製造方法。
[12]前記強化繊維が炭素繊維であり、前記繊維強化ポリアミド樹脂基材中の繊維含有量が10〜70体積%である[11]に記載のポリアミド樹脂製複合成形品の製造方法。
ここで、Δei、Δvtは各々の原子又は原子団の蒸発エネルギー(cal/mol)、及びモル体積(cm3/mol)である。
ここで、δcoは共重合体のSP値、δ1、δ2・・・δnは共重合体を構成する各モノマーのFedors法により算出されるSP値、W1、W2・・・Wnは共重合体を構成する各モノマーの重量分率である。
また、融点を示さないナイロン樹脂(例えば非晶性ナイロン樹脂)の溶融必要熱量Qamは下記式(4)から算出される。
ここで、Cpは比熱容量(J/℃・g)、Tmは融点(℃)、Tgはガラス転移点(℃)、ΔHは溶融熱(J/g)である。また、CpはJIS K 7123−1987(2006年)に準じて測定した値、Tm、TgはJIS K 7121−1987(2006年)に準じて測定した値、ΔHはJIS K 7122−1987(2006年)に準じて測定した値である。いずれも示差走査熱量測定(DSC)で測定する。
含浸用ポリアミド樹脂について、式(3)および式(4)を用い、溶融必要熱量QおよびQamを算出した。比熱容量については、降温速度10℃でJIS K 7123−1987(2006年)に準じて測定し、融点Tmおよびガラス転移点Tgについては、昇温速度20℃で、JIS K 7121―1987(2006年)に準じて測定し、溶融熱については、昇温速度20℃で、JIS K 7122―1987(2006年)に準じて測定を行った。いずれの測定も(株)パーキンエルマー製結晶化温度測定機Diamond−DSCを用いた。
含浸用ポリアミド樹脂について、式(1)および式(2)を用い、SP値δおよびδcoを算出した。
表に示すポリアミド樹脂組成物を80℃で12時間真空乾燥し、射出成形機((株)日本製鋼所製J110AD−110H)を用いて、シリンダー温度:ポリアミド樹脂組成物の融点+35℃(実施例7は260℃)、金型温度:60℃の条件で、図1に示したような形状の試験片を作製できる金型に適切な大きさに切削した表に示す繊維強化ポリアミド樹脂基材を配置し、射出溶着により、繊維強化ポリアミド樹脂基材の両端とポリアミド樹脂成形品が接合されたポリアミド樹脂製複合成形品を得た。この成形品は、全体としてISO Type−A規格の形状であった。溶着性を評価する片側の溶着面の面積を40mm2とし、引張速度を1mm/分にすること以外はISO527−1、−2に従い、引張試験を行った。3回測定を行い、破断までの最大荷重の平均値を溶着力として評価した。なお、溶着力が低く、成形時や評価前に剥離したものについては×を記載した。
表に示すポリアミド樹脂組成物を80℃で12時間真空乾燥し、射出成形機((株)日本製鋼所製J110AD−110H)を用いて、シリンダー温度:300℃、金型温度:120℃の条件で、150mm長×50mm幅×3mm厚の平板金型の両面に適切な大きさに切削した表に示す繊維強化ポリアミド樹脂基材を配置し、射出溶着により、ポリアミド樹脂成形品の両側に繊維強化ポリアミド樹脂基材を有するサンドイッチ構造のポリアミド製複合成形品を得た。前記繊維強化ポリアミド樹脂基材は、強化繊維軸方向がポリアミド樹脂製複合成形品の長手方向と略並行となるように配置した。
繊維強化ポリアミド樹脂基材を片側に配置すること以外は上記曲げ弾性率と同様の方法で150mm長×50mm幅×3mm厚のポリアミド樹脂製複合成形品の試験片を得た。
A:5mm未満。
B:5mm以上10mm未満。
C:10mm以上。
繊維強化ポリアミド樹脂基材は以下の方法で製造した。強化繊維束が巻かれたボビンを16本準備し、それぞれボビンから連続的に糸道ガイドを通じて強化繊維束を送り出した。連続的に送り出された強化繊維束に、含浸ダイ内において、含浸用ポリアミド樹脂を充填したフィーダーから定量供給された含浸用ポリアミド樹脂を含浸させた。強化繊維には、炭素繊維束(東レ(株)製“トレカ”(登録商標)T700S−12K)を用い、含浸用ポリアミド樹脂には表1、2に記載のものを用いた。含浸ダイ内で含浸用ポリアミド樹脂を含浸した強化繊維を、引取ロールを用いて含浸ダイのノズルから連続的に引き抜いた。引き抜かれた強化繊維束は、冷却ロールを通過して含浸用ポリアミド樹脂が冷却固化され、繊維強化ポリアミド樹脂基材として巻取機に巻き取られた。得られた繊維強化ポリアミド樹脂基材の厚さは0.3mmであり、強化繊維方向は一方向に配列していた。また、繊維強化ポリアミド樹脂基材中の強化繊維の含有量は50体積%であった。
強化繊維としてガラス繊維を用いること以外は実施例1と同様の方法でポリアミド樹脂製複合成形品を作製し、各種特性を評価した。
表1に記載の強化繊維、含浸用ポリアミド樹脂を用いて繊維強化ポリアミド樹脂基材を以下の方法で作製した。
表1中のポリアミド組成物および含浸用ポリアミド樹脂を用いること、ポリアミド樹脂組成物の製造方法においてバレル温度を300℃にすること以外は実施例1と同様の方法で作製したポリアミド樹脂組成物を用いて、ポリアミド樹脂製複合成形品を作製し、各種特性を評価した。
処理温度180℃、処理時間30分の条件で熱アニール処理した繊維強化ポリアミド樹脂基材を用いること以外は実施例1と同様の方法でポリアミド樹脂製複合成形品を作製し、各種特性を評価した。
含浸用ポリアミド樹脂が、ポリアミド6および下記参考例1をそれぞれ25重量%、75重量%混合したものということ以外は実施例1と同様の方法でポリアミド樹脂製複合成形品を作製し、各種特性を評価した。
炭素繊維:東レ(株)製“トレカ”(登録商標)T700S−12K
(充填材)
ガラス繊維:日本電気硝子(株)製T−275H、円形断面、断面直径10.5μm、表面処理シラン系カップリング剤、繊維長3mm
(ポリアミド樹脂)
ポリアミド6:東レ(株)製CM1001、ηr=2.35
ポリアミド66:東レ(株)製E3000F、ηr=2.48
ポリアミド610:東レ(株)製CM2001、ηr=2.70
ポリアミド12:EMS製Grilamid L 20、中粘度グレード
ポリアミド6I/6T:EMS製Grivory G 21、ηr=2.00 。
30Lのステンレス製オートクレーブに、ポリアミド6/66塩(ε−カプロラクタム/ヘキサメチレンジアミン−アジピン酸の等モル塩の80%水溶液)を85/15重量部で配合し、安息香酸(ポリアミド6/66塩10kgに対して1.86g)を投入して、内温250℃、内圧1.5〜2.0MPaに保って3時間重合した。その後徐々に放圧しながら内圧を常圧に戻し、内温を270〜280℃に上げ、更に1時間重合させた。得られたポリアミド6/66樹脂をオートクレーブの下部からストランドで抜き出し、ペレタイズした後、80℃で24時間真空乾燥した。得られたポリアミド6/66の相対粘度ηrは2.35、融点は194℃であった。
ポリアミド6/66塩を90/10重量部にすること以外は参考例1と同様の方法でポリアミド6/66を得た。得られたポリアミド6/66樹脂の相対粘度ηrは2.35、融点は199℃であった。
ポリアミド6/66塩を40/60重量部にすること以外は参考例1と同様の方法でポリアミド6/66を得た。得られたポリアミド6/66樹脂の相対粘度ηrは2.35、融点は170℃であった。
ポリアミド6/66塩を30/70重量部にすること以外は参考例1と同様の方法でポリアミド6/66を得た。得られたポリアミド6/66樹脂の相対粘度ηrは2.35、融点は182℃であった。
ポリアミド6/66塩を95/5重量部にすること以外は参考例1と同様の方法でポリアミド6/66を得た。得られたポリアミド6/66樹脂の相対粘度ηrは2.35、融点は254℃であった。
ポリアミド6/66塩を5/95重量部にすること以外は参考例1と同様の方法でポリアミド6/66を得た。得られたポリアミド6/66樹脂の相対粘度ηrは2.35、融点は212℃であった。
2 ポリアミド樹脂成形品
3 溶着面
Claims (12)
- 強化繊維基材に含浸用ポリアミド樹脂を含浸させた繊維強化ポリアミド樹脂基材と、ポリアミド樹脂組成物からなるポリアミド樹脂成形品とが、少なくとも一部で接合した複合成形品であって、前記含浸用ポリアミド樹脂の溶融必要熱量(前記繊維強化ポリアミド樹脂基材を熱アニール処理した場合は、該熱アニール処理後の繊維強化ポリアミド樹脂基材から算出した溶融必要熱量とする)が300<Q<425(J/g)であり、Fedorsの式から算出される前記含浸用ポリアミド樹脂の溶解度パラメータ(SP値)が11<σ<13.2((cal/cm3)1/2)であるポリアミド樹脂製複合成形品。
- 前記含浸用ポリアミド樹脂が、ポリアミド6成分30〜90重量%とポリアミド66成分70〜10重量%とからなるポリアミド共重合体を含む請求項1に記載のポリアミド樹脂製複合成形品。
- 前記ポリアミド樹脂組成物がポリアミド樹脂100重量部に対し、充填材10〜250重量部を含む請求項1または2に記載のポリアミド樹脂製複合成形品。
- 前記ポリアミド樹脂組成物の主成分がポリアミド6樹脂である請求項1〜3のいずれかに記載のポリアミド樹脂製複合成形品。
- 前記強化繊維基材が一方向に配列した連続の強化繊維からなる請求項1〜4のいずれかに記載のポリアミド樹脂製複合成形品。
- 前記強化繊維が炭素繊維であり、前記繊維強化ポリアミド樹脂基材中の繊維含有量が10〜70体積%である請求項5に記載のポリアミド樹脂製複合成形品。
- 強化繊維基材に含浸用ポリアミド樹脂を含浸させた繊維強化ポリアミド樹脂基材を予め金型内に配置し、該金型にポリアミド樹脂組成物を射出成形して溶融接合するポリアミド樹脂製複合成形品の製造方法であって、前記含浸用ポリアミド樹脂の溶融必要熱量(前記繊維強化ポリアミド樹脂基材を熱アニール処理した場合は、該熱アニール処理後の繊維強化ポリアミド樹脂基材から算出した溶融必要熱量とする)が300<Q<425(J/g)であり、Fedorsの式から算出される前記含浸用ポリアミド樹脂の溶解度パラメータ(SP値)が11<σ<13.2((cal/cm3)1/2)であるポリアミド樹脂製複合成形品の製造方法。
- 前記含浸用ポリアミド樹脂が、ポリアミド6成分30〜90重量%とポリアミド66成分70〜10重量%とからなるポリアミド共重合体を含む請求項7に記載のポリアミド樹脂製複合成形品の製造方法。
- 前記ポリアミド樹脂組成物が、ポリアミド樹脂100重量部に対し、充填材10〜250重量部を含む請求項7または8に記載のポリアミド樹脂製複合成形品の製造方法。
- 前記ポリアミド樹脂組成物の主成分がポリアミド6樹脂である請求項7〜9のいずれかに記載のポリアミド樹脂製複合成形品の製造方法。
- 前記強化繊維基材が一方向に配列した連続の強化繊維からなる請求項7〜10のいずれかに記載のポリアミド樹脂製複合成形品の製造方法。
- 前記強化繊維が炭素繊維であり、前記繊維強化ポリアミド樹脂基材中の繊維含有量が10〜70体積%である請求項11に記載のポリアミド樹脂製複合成形品の製造方法。
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