JP2016056914A - 断熱材及びその製造方法 - Google Patents
断熱材及びその製造方法 Download PDFInfo
- Publication number
- JP2016056914A JP2016056914A JP2014185213A JP2014185213A JP2016056914A JP 2016056914 A JP2016056914 A JP 2016056914A JP 2014185213 A JP2014185213 A JP 2014185213A JP 2014185213 A JP2014185213 A JP 2014185213A JP 2016056914 A JP2016056914 A JP 2016056914A
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- Prior art keywords
- resin
- heat
- insulating material
- thermoplastic resin
- heat insulating
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Abstract
【解決手段】耐熱性繊維からなる繊維層が積層した積層体からなり、前記繊維層は熱硬化性樹脂により固められており、前記積層体は、前記熱硬化性樹脂の耐熱温度よりも低い耐熱温度を有する熱可塑性樹脂を含まない又は微量含有することを特徴とする断熱材。
【選択図】図3
Description
1.耐熱性繊維からなる繊維層が積層した積層体からなり、前記繊維層は熱硬化性樹脂により固められており、
前記積層体は、前記熱硬化性樹脂の耐熱温度よりも低い耐熱温度を有する熱可塑性樹脂を含まない又は微量含有することを特徴とする断熱材。
2.前記積層体が熱可塑性樹脂を微量含有し、熱可塑性樹脂の含量は7質量%以下であることを特徴とする1に記載の断熱材。
3.耐熱性繊維からなるシートに熱硬化性樹脂を含浸させてプリプレグを作製するプリプレグ作製工程であって、前記プリプレグが、前記熱硬化性樹脂の耐熱温度よりも低い耐熱温度を有する熱可塑性樹脂を含まない又は微量含有するプリプレグ作製工程と、
前記プリプレグを複数枚積層して積層体を作製する積層体作製工程と、
前記積層体を、前記熱硬化性樹脂の硬化温度以上の温度で、プレス成形するプレス工程とを含むことを特徴とする断熱材の製造方法。
4.前記プリプレグが熱可塑性樹脂を微量含有し、熱可塑性樹脂の含量は7質量%以下であることを特徴とする3に記載の断熱材の製造方法。
5.耐熱性繊維からなる繊維層が積層した積層体からなり、前記繊維層は熱硬化性樹脂により固められており、
前記積層体は、熱可塑性樹脂を含まない又は微量含有し、
前記熱硬化性樹脂は、熱硬化性フェノール樹脂、エポキシ樹脂、メラミン樹脂、ユリア樹脂、不飽和ポリエステル樹脂、アルキド樹脂、ポリウレタン樹脂、熱硬化性ポリイミド樹脂、シリコーン樹脂から選択される1以上であり、
前記熱可塑性樹脂は、アクリル樹脂、ポリビニルアルコール、ポリ塩化ビニル、ポリスチレン、ポリエチレン、ポリプロピレン、PET樹脂、PBT樹脂から選択される1以上であることを特徴とする断熱材。
ここで、上記の「耐熱温度」とは、樹脂の物理的性状を保持できる上限の温度(例えば樹脂材料に軟化・変形が生じる温度、或いは樹脂材料に熱分解が生じる温度等)である。具体的には、耐熱温度とは、物理的耐熱性の観点では軟化温度やガラス転移点等の温度であり、化学的耐熱性の観点では、加熱時の重量減少等が生じる温度である。より詳細には、本発明の耐熱温度は、熱可塑性樹脂と熱硬化性樹脂とで各々異なる。本発明の熱可塑性樹脂の耐熱温度は、所定の加熱条件(加熱時間、昇温速度)下で軟化する軟化温度、又は、組成成分の結合が切れて樹脂自体が変質劣化する温度である熱分解温度(具体的には所定率(5%又は10%)重量減少温度、荷重たわみ温度、所定率(例えば2%)厚さ変化率温度、樹脂材料の形状(膨れ、ひび割れ、曲がり)・色の外観判定による温度)である。本発明の熱硬化性樹脂の耐熱温度は、前記所定の加熱条件下で硬化する硬化温度、又は、組成成分の結合が切れて樹脂自体が変質劣化する温度である熱分解温度(具体的には所定率(5%又は10%)重量減少温度、荷重たわみ温度、所定率(例えば2%)厚さ変化率温度、樹脂材料の形状(膨れ、ひび割れ、曲がり)・色の外観判定による温度)である。さらに特定すると、本発明の熱可塑性樹脂及び熱硬化性樹脂の耐熱温度は、一定時間加熱した際の重量減少が10%以下になる温度である。
この点、具体的には、断熱材の繊維層が、例えば保形のためのサイジング剤やバインダー等として、熱硬化性樹脂の耐熱温度よりも低い耐熱温度を有する熱可塑性樹脂を所定量含む場合、高温下では熱可塑性樹脂の可塑性によってクリープ(材料変形)を生じ易く、かかるクリープによる疲労のため構造的強度が弱くなる。
また、断熱材が例えば金型装置の断熱板として用いられる場合には、金型装置のプレス成型時の加熱・加圧によって断熱板にクリープが生じると、断熱板と金型装置の被取付体との間に隙間が生じ、金型装置の圧力が不安定になる。
さらに、高温化で熱可塑性樹脂が熱分解されると、その分解の際の発熱によりさらに分解が進む。このような熱分解によって熱可塑性樹脂の消失が進むと、繊維層の接着強度が弱まり繊維層が解けやすい状態となって耐熱性及び摩耗性の低下や更なる強度低下をもたらす。
従って、本発明の断熱材では、熱可塑性樹脂を含まない又は熱可塑性樹脂の含量を微量にするという構成を採用することによって、熱可塑性樹脂が断熱材の耐熱性、耐摩耗性、強度(曲げ強度)を低減させることを抑制できる。換言すれば、本発明の断熱材では、熱可塑性樹脂を含まない又は熱可塑性樹脂の含量を微量にするという構成を採用することによって、耐熱性、耐摩耗性、強度(曲げ強度)を高めることできる。
熱硬化性樹脂として、熱硬化性フェノール樹脂、エポキシ樹脂、メラミン樹脂、ユリア樹脂、不飽和ポリエステル樹脂、アルキド樹脂、ポリウレタン樹脂、熱硬化性ポリイミド樹脂、シリコーン樹脂等から選ばれる一種以上を挙げることができる。
熱可塑性樹脂として、アクリル樹脂、ポリビニルアルコール、ポリ塩化ビニル、ポリスチレン、ポリエチレン、ポリプロピレン、PET樹脂、PBT樹脂等から選ばれる一種以上を挙げられる。尚、上記の熱可塑性樹脂は、上記の熱硬化性樹脂より、耐熱温度が低い。
ここで、上記の熱可塑性樹脂及び熱硬化性樹脂に鑑みて、本発明の断熱材は、耐熱性繊維からなる繊維層が積層した積層体からなり、前記繊維層は熱硬化性樹脂により固められており、前記積層体は、熱可塑性樹脂を含まない又は微量含有し、前記熱硬化性樹脂は、熱硬化性フェノール樹脂、エポキシ樹脂、メラミン樹脂、ユリア樹脂、不飽和ポリエステル樹脂、アルキド樹脂、ポリウレタン樹脂、熱硬化性ポリイミド樹脂、シリコーン樹脂から選択される1以上であり、前記熱可塑性樹脂は、アクリル樹脂、ポリビニルアルコール、ポリ塩化ビニル、ポリスチレン、ポリエチレン、ポリプロピレン、PET樹脂、PBT樹脂から選択される1以上であるように構成することができる。
本発明の断熱材は、繊維と熱硬化性樹脂以外に硬化剤,硬化促進剤、無機充填剤、触媒等を含むことができる。
硬化剤(熱硬化性樹脂、熱可塑性樹脂を含まない)としては、ヘキサメチレンテトラミン等のアミン類や、有機過酸化物等の過酸化物等を挙げることができる。
硬化促進剤としては、リン系化合物、第3級アミン、イミダゾール、有機酸金属塩、ルイス酸、アミン錯塩等から選ばれる1種以上を挙げることができる。
図1に示す例においては、耐熱性シート1を巻回した状態で保持するホルダーHから耐熱性シート1をローラー等により引き出しつつ、熱硬化性樹脂2を満たした含浸槽Tに浸漬して所定量の熱硬化性樹脂2を含浸させ、その後、乾燥機Dで乾燥した後に、切断機Cで所定サイズに切断することにより、目的とするプリプレグ3を製造することができる。
ペーパーの坪量は、通常、20〜430g/m2である。本発明において、坪量(g/m2)は、JIS P 8124の規定に基づいて算出される値を意味する。
マットは表面に凹凸があるため積層した場合、互いにからみ強度が増すため好ましい。また、バインダーを用いずに製造できるので、コストを低減できる。
耐熱性シート1がマットで構成される場合、マットから得られるプリプレグの坪量は、例えば150〜10000g/m2とすることができる。
プリプレグの坪量(g/m2)は、100cm四方の正方形状のプリプレグの質量(g)から算出される値を意味する。
図2に示す例においては、耐熱性シートに熱硬化性樹脂を含浸してなるプリプレグ3を所望枚数枚積層して積層物Lを5個形成し、得られた5個のプリプレグの積層物Lを、各積層物間にスペーサーを介した状態でプレス機Pのプレス板間に積み重ねた上で、プリプレグを構成する熱硬化性樹脂の熱硬化温度以上の温度条件下、プリプレグ1枚当たりの平均厚みが所望厚みになるように加圧して熱圧プレスすることにより、目的とする断熱材4を得ることができる。
図2に示す態様においては、上記積層物Lを5個積み重ねた状態で熱圧プレス成形しているが、積層物Lは、通常、1〜20個程度積み重ねた状態で熱圧プレス成形することができる。
圧縮率(%)=(熱圧成形後のプリプレグ1枚あたりの平均厚み(mm)/熱圧成形に供したプリプレグ1枚の平均厚み(mm))×100
このために、断熱材は、同量の繊維及び熱硬化性樹脂を含有する断熱材に比較して、精度の高い良好な加工性を有するとともに、優れた曲げ強度、靱性、厚さ精度等を発揮し得ると考えられる。
断熱材の密度は、縦120mm×横40mm×得られた断熱材の厚さに切り出した試験片の寸法(m3)及び重量(kg)から求めた値を意味する。
断熱材の熱伝導率は、JIS A 1412−2:1999第2部 熱流計法HFM法で測定した値を意味する。
曲げ強度は、JIS C2210−1975の繊維強化樹脂の曲げ試験に基づいて測定した値を意味する。
シャルピー衝撃値が上記範囲内にあることにより、十分な靱性を発揮することができる。
(1)プリプレグの作製
図1に示す装置を用い、ホルダーHに巻き付けた耐熱性マット1(平均厚さ6mm、平均幅1050mm、平均長さ30mm、密度120kg/m3)をローラーで引き出しつつ、熱硬化性樹脂2であるレゾール型フェノール樹脂(熱硬化温度150℃)を満たした含浸槽Tに浸漬した。耐熱性マット1は、ガラス繊維をニードルパンチで絡合して得たものである。その後、乾燥機Dで60〜130℃で乾燥し、次いで切断機Cで切断することにより、ガラス繊維製マットに由来する繊維40質量%、レゾール型フェノール樹脂60質量%を含有するシート状(板状)のプリプレグ3を複数枚作製した。
(1)で得たプリプレグ3を13枚積層した積層物Lを5個作製し、得られた5個の積層物Lを、図2に示すように、各積層物間にスペーサーを介した状態でプレス機Pのプレス板間に積み重ねた上で、150℃の温度条件下で2時間(又は200℃の温度条件下で1時間)熱圧プレス成形することにより、シート状又は板状(例えば、縦2000mm、横1000mm、厚さ22mmの断熱材4を得た。断熱材4はマットのガラス繊維が熱硬化性樹脂で固められ、熱可塑性樹脂は含んでいなかった。
本発明の断熱材は、熱可塑性樹脂の含量が少ないことにより、耐摩耗性、耐熱性に優れることを、この実験例で示す。
実施例1において、耐熱性マット1の代わりにポバール系合成樹脂(熱可塑性樹脂)とアクリル系合成樹脂(熱可塑性樹脂)を16質量%含むガラス繊維製ペーパー(平均厚さ0.78mm、坪量110g/m2)を用いた他は、実施例1と同様にして、平均厚さ0.84mm、縦2110mm、横1050mmのプリプレグを複数枚作製した。さらに、得られたプリプレグを57枚積層した積層物Lを作製した他は、実施例1と同様にして、縦2070mm、横1020mm、厚さ12mmの断熱材Bを得た。
得られた断熱材Bは、繊維を42質量%、レゾール型フェノール樹脂を50質量%、熱可塑性樹脂を8質量%含有していた。
断熱材に用いた、樹脂の耐熱温度は以下のようにして測定した。汎用のオーブン等の加熱機器及び汎用の重量測定装置を用いて、所定の加熱時間において樹脂材料を加熱した際に当該材料に10%重量減少が生じたときの温度を耐熱温度として測定した。なお、TG(熱重量測定装置)を用いて耐熱温度を測定することも可能である。
以下、実施例1で得られた断熱材を、断熱材Aと呼ぶ。
断熱材A,Bを、240℃の雰囲気下で50時間及び70時間加熱した。その後、常温に戻して、摩耗量を測定した。具体的には、テーバー型磨耗試験装置を用いて、断熱材を磨耗輪に接触させ、断熱材を摩耗輪に対して回転させた。磨耗輪と接触した部分が削れるので、試験前後の断熱材の重量変化を測定して、磨耗量(g)を求めた。結果を図3に示す。
断熱材A,Bをオーブンに入れて、180℃で16MPa、及び200℃で15MPaの、熱と圧力をかけ、厚さの変化を測定した。結果を図4に示す。
以上、図3〜図5に示されるように、断熱材に含まれる熱可塑性樹脂が8質量%以上であると、断熱材の磨耗性、耐熱性(重量減少、厚さ変化)の低下が顕著であり、断熱材に含まれる熱可塑性樹脂は、少なくとも7質量%以下であることが好ましい。
2 熱硬化性樹脂
3 プリプレグ
4 断熱材
Claims (5)
- 耐熱性繊維からなる繊維層が積層した積層体からなり、前記繊維層は熱硬化性樹脂により固められており、
前記積層体は、前記熱硬化性樹脂の耐熱温度よりも低い耐熱温度を有する熱可塑性樹脂を含まない又は微量含有することを特徴とする断熱材。 - 前記積層体が熱可塑性樹脂を微量含有し、熱可塑性樹脂の含量は7質量%以下であることを特徴とする請求項1に記載の断熱材。
- 耐熱性繊維からなるシートに熱硬化性樹脂を含浸させてプリプレグを作製するプリプレグ作製工程であって、前記プリプレグが、前記熱硬化性樹脂の耐熱温度よりも低い耐熱温度を有する熱可塑性樹脂を含まない又は微量含有するプリプレグ作製工程と、
前記プリプレグを複数枚積層して積層体を作製する積層体作製工程と、
前記積層体を、前記熱硬化性樹脂の硬化温度以上の温度で、プレス成形するプレス工程とを含むことを特徴とする断熱材の製造方法。 - 前記プリプレグが熱可塑性樹脂を微量含有し、熱可塑性樹脂の含量は7質量%以下であることを特徴とする請求項3に記載の断熱材の製造方法。
- 耐熱性繊維からなる繊維層が積層した積層体からなり、前記繊維層は熱硬化性樹脂により固められており、
前記積層体は、熱可塑性樹脂を含まない又は微量含有し、
前記熱硬化性樹脂は、熱硬化性フェノール樹脂、エポキシ樹脂、メラミン樹脂、ユリア樹脂、不飽和ポリエステル樹脂、アルキド樹脂、ポリウレタン樹脂、熱硬化性ポリイミド樹脂、シリコーン樹脂から選択される1以上であり、
前記熱可塑性樹脂は、アクリル樹脂、ポリビニルアルコール、ポリ塩化ビニル、ポリスチレン、ポリエチレン、ポリプロピレン、PET樹脂、PBT樹脂から選択される1以上であることを特徴とする断熱材。
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