JP2007016093A - 熱可塑性樹脂組成物 - Google Patents
熱可塑性樹脂組成物 Download PDFInfo
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- JP2007016093A JP2007016093A JP2005197279A JP2005197279A JP2007016093A JP 2007016093 A JP2007016093 A JP 2007016093A JP 2005197279 A JP2005197279 A JP 2005197279A JP 2005197279 A JP2005197279 A JP 2005197279A JP 2007016093 A JP2007016093 A JP 2007016093A
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Landscapes
- Compositions Of Macromolecular Compounds (AREA)
Abstract
【解決手段】 熱可塑性樹脂(A成分)47〜98.97重量部、組成物中での粒径が50μm以下の黒鉛(B成分)1〜50重量部、酸性基含有有機化合物(C成分)0.03〜3重量部の合計100重量部からなる樹脂組成物であって、好適には熱可塑性樹脂(A成分)がポリカーボネート樹脂を50%以上含有し、好ましくは更にリン系安定剤(D成分)、難燃剤(E成分)、及び含フッ素滴下防止剤(F成分)からなる群から選ばれる1種以上の成分を含有し、酸性基含有有機化合物がカルボキシル基および/またはその酸無水物基を有するオレフィン系ワックスである熱可塑性樹脂組成物。
【選択図】 なし
Description
例えば、高分子材料に黒鉛化炭素繊維を添加する方法(特許文献1〜3参照)、熱可塑性樹脂にピッチ系炭素繊維と鱗状黒鉛を添加する方法(特許文献4参照)が公知であるが、熱伝導性フィラーは大量に充填しないと充分な熱伝導性を得ることが出来ず、更にこれらの黒鉛化炭素繊維系材料あるいはピッチ系炭素繊維を工業的に安価で大量に得ることが不可能であり実用的ではない。また、熱可塑性樹脂に黒鉛を添加する方法(特許文献5参照)が開示されている。しかしながら、近年の電子機器等の発熱量は増加傾向にあるため更なる高熱伝導化が求められており改良の余地がある。
本発明者は、上記従来技術の問題点に鑑み、鋭意検討した結果、組成物中での粒径が50μm以下の黒鉛、特に膨張黒鉛を粉砕することにより調製した黒鉛と酸性基含有有機化合物とを、ポリカーボネート樹脂を主体とする熱可塑性樹脂に配合することにより、剛性、熱安定性、熱伝導性に優れたポリカーボネート樹脂を主体とする熱可塑性樹脂組成物が得られることを見出し、結果本発明に到達した。
ηsp/c=[η]+0.45×[η]2c(但し[η]は極限粘度)
[η]=1.23×10−4M0.83
c=0.7
(1)該ポリカーボネートを構成する二価フェノール成分100モル%中、4,4’−(m−フェニレンジイソプロピリデン)ジフェノール(以下“BPM”と略称)成分が20〜80モル%(より好適には40〜75モル%、さらに好適には45〜65モル%)であり、かつ9,9−ビス(4−ヒドロキシ−3−メチルフェニル)フルオレン(以下“BCF”と略称)成分が20〜80モル%(より好適には25〜60モル%、さらに好適には35〜55モル%)である共重合ポリカーボネート。
(2)該ポリカーボネートを構成する二価フェノール成分100モル%中、ビスフェノールA成分が10〜95モル%(より好適には50〜90モル%、さらに好適には60〜85モル%)であり、かつBCF成分が5〜90モル%(より好適には10〜50モル%、さらに好適には15〜40モル%)である共重合ポリカーボネート。
(3)該ポリカーボネートを構成する二価フェノール成分100モル%中、BPM成分が20〜80モル%(より好適には40〜75モル%、さらに好適には45〜65モル%)であり、かつ1,1−ビス(4−ヒドロキシフェニル)−3,3,5−トリメチルシクロヘキサン成分が20〜80モル%(より好適には25〜60モル%、さらに好適には35〜55モル%)である共重合ポリカーボネート。
かかる有機ハロゲン系難燃剤としては、ハロゲン化カーボネートオリゴマー、ハロゲン化エポキシ化合物、ハロゲン化ポリスチレン、ハロゲン化トリアジン化合物、ハロゲン化ジフェニルアルカン系化合物、ハロゲン化インダン系化合物、およびハロゲン化芳香族フタルイミド系化合物などが挙げられ、中でもポリカーボネートとの相溶性に優れ、その耐熱性および熱安定性が良好であることからハロゲン化カーボネートオリゴマー、ハロゲン化エポキシ化合物が好ましい。
(ヒンダードフェノール系安定剤)
本発明の樹脂組成物は、更にヒンダードフェノール系安定剤を含有することにより、例えば成形加工時の色相悪化や長期間の使用における色相の悪化などの効果が更に発揮される。ヒンダードフェノール系安定剤としては、例えば、α−トコフェロール、ブチルヒドロキシトルエン、シナピルアルコール、ビタミンE、n−オクタデシル−β−(4’−ヒドロキシ−3’,5’−ジ−tert−ブチルフェル)プロピオネート、2−tert−ブチル−6−(3’−tert−ブチル−5’−メチル−2’−ヒドロキシベンジル)−4−メチルフェニルアクリレート、2,6−ジ−tert−ブチル−4−(N,N−ジメチルアミノメチル)フェノール、3,5−ジ−tert−ブチル−4−ヒドロキシベンジルホスホネートジエチルエステル、2,2’−メチレンビス(4−メチル−6−tert−ブチルフェノール)、2,2’−メチレンビス(4−エチル−6−tert−ブチルフェノール)、4,4’−メチレンビス(2,6−ジ−tert−ブチルフェノール)、2,2’−メチレンビス(4−メチル−6−シクロヘキシルフェノール)、2,2’−ジメチレン−ビス(6−α−メチル−ベンジル−p−クレゾール)2,2’−エチリデン−ビス(4,6−ジ−tert−ブチルフェノール)、2,2’−ブチリデン−ビス(4−メチル−6−tert−ブチルフェノール)、4,4’−ブチリデンビス(3−メチル−6−tert−ブチルフェノール)、トリエチレングリコール−N−ビス−3−(3−tert−ブチル−4−ヒドロキシ−5−メチルフェニル)プロピオネート、1,6−へキサンジオールビス[3−(3,5−ジ−tert−ブチル−4−ヒドロキシフェニル)プロピオネート]、ビス[2−tert−ブチル−4−メチル6−(3−tert−ブチル−5−メチル−2−ヒドロキシベンジル)フェニル]テレフタレート、3,9−ビス{2−[3−(3−tert−ブチル−4−ヒドロキシ−5−メチルフェニル)プロピオニルオキシ]−1,1,−ジメチルエチル}−2,4,8,10−テトラオキサスピロ[5,5]ウンデカン、4,4’−チオビス(6−tert−ブチル−m−クレゾール)、4,4’−チオビス(3−メチル−6−tert−ブチルフェノール)、2,2’−チオビス(4−メチル−6−tert−ブチルフェノール)、ビス(3,5−ジ−tert−ブチル−4−ヒドロキシベンジル)スルフィド、4,4’−ジ−チオビス(2,6−ジ−tert−ブチルフェノール)、4,4’−トリ−チオビス(2,6−ジ−tert−ブチルフェノール)、2,2−チオジエチレンビス−[3−(3,5−ジ−tert−ブチル−4−ヒドロキシフェニル)プロピオネート]、2,4−ビス(n−オクチルチオ)−6−(4−ヒドロキシ−3’,5’−ジ−tert−ブチルアニリノ)−1,3,5−トリアジン、N,N’−ヘキサメチレンビス−(3,5−ジ−tert−ブチル−4−ヒドロキシヒドロシンナミド)、N,N’−ビス[3−(3,5−ジ−tert−ブチル−4−ヒドロキシフェニル)プロピオニル]ヒドラジン、1,1,3−トリス(2−メチル−4−ヒドロキシ−5−tert−ブチルフェニル)ブタン、1,3,5−トリメチル−2,4,6−トリス(3,5−ジ−tert−ブチル−4−ヒドロキシベンジル)ベンゼン、トリス(3,5−ジ−tert−ブチル−4−ヒドロキシフェニル)イソシアヌレート、トリス(3,5−ジ−tert−ブチル−4−ヒドロキシベンジル)イソシアヌレート、1,3,5−トリス(4−tert−ブチル−3−ヒドロキシ−2,6−ジメチルベンジル)イソシアヌレート、1,3,5−トリス2[3(3,5−ジ−tert−ブチル−4−ヒドロキシフェニル)プロピオニルオキシ]エチルイソシアヌレート、およびテトラキス[メチレン−3−(3’,5’−ジ−tert−ブチル−4−ヒドロキシフェニル)プロピオネート]メタンなどが例示される。これらはいずれも入手容易である。上記ヒンダードフェノール系安定剤は、単独でまたは2種以上を組合せて使用することができる。
本発明の熱可塑性樹脂組成物は、塗装などを施すことなく使用される場合がある。かかる場合には良好な耐光性を要求される場合があり、かかる場合に紫外線吸収剤の配合が効果的である。
本発明の樹脂組成物においては、上記紫外線吸収剤と更に光安定剤を併用することができる。かかる光安定剤としては、例えばビス(2,2,6,6−テトラメチル−4−ピペリジル)セバケート、ビス(1,2,2,6,6−ペンタメチル−4−ピペリジル)セバケート、テトラキス(2,2,6,6−テトラメチル−4−ピペリジル)−1,2,3,4−ブタンテトラカルボキシレート、テトラキス(1,2,2,6,6−ペンタメチル−4−ピペリジル)−1,2,3,4−ブタンテトラカルボキシレート、ポリ{[6−(1,1,3,3−テトラメチルブチル)アミノ−1,3,5−トリアジン−2,4−ジイル][(2,2,6,6−テトラメチルピペリジル)イミノ]ヘキサメチレン[(2,2,6,6−テトラメチルピペリジル)イミノ]}、およびポリメチルプロピル3−オキシ−[4−(2,2,6,6−テトラメチル)ピペリジニル]シロキサンなどに代表されるヒンダードアミン系の光安定剤が例示される。上記光安定剤は単独であるいは2種以上の混合物を用いてもよい。光安定剤の配合量は(A)〜(C)成分の合計100重量部に対して0.0005〜3重量部が好ましく、0.01〜2重量部がより好ましく、0.02〜1重量部が更に好ましい。
本発明の樹脂組成物には、本発明の効果を発揮する範囲において、強化フィラーとしてB成分以外の各種充填材を配合することができる。例えば、炭酸カルシウム、ガラス繊維、ガラスビーズ、ガラスバルーン、ガラスミルドファイバー、ガラスフレーク、炭素繊維、炭素フレーク、カーボンビーズ、カーボンミルドファイバー、グラファイト、気相成長法極細炭素繊維(繊維径が0.1μm未満)、カーボンナノチューブ(繊維径が0.1μm未満であり、中空状)、フラーレン、金属フレーク、金属繊維、金属コートガラス繊維、金属コート炭素繊維、金属コートガラスフレーク、シリカ、金属酸化物粒子、金属酸化物繊維、金属酸化物バルーン、並びに各種ウイスカー(チタン酸カリウムウイスカー、ホウ酸アルミニウムウイスカー、および塩基性硫酸マグネシウムなど)などが例示される。これらの強化フィラーは1種もしくは2種以上を併用して含むものであってもよい。
本発明の樹脂組成物には、他の樹脂やエラストマーを本発明の効果を発揮する範囲において、少割合使用することもできる。
かかる他の樹脂としては、例えばポリエチレンテレフタレート、ポリブチレンテレフタレート等のポリエステル樹脂、ポリアミド樹脂、ポリイミド樹脂、ポリエーテルイミド樹脂、ポリウレタン樹脂、シリコーン樹脂、ポリフェニレンエーテル樹脂、ポリフェニレンスルフィド樹脂、ポリスルホン樹脂、ポリエチレン、ポリプロピレン等のポリオレフィン樹脂、ポリスチレン樹脂、アクリロニトリル/スチレン共重合体(AS樹脂)、アクリロニトリル/ブタジエン/スチレン共重合体(ABS樹脂)、ポリメタクリレート樹脂、フェノール樹脂、エポキシ樹脂等の樹脂が挙げられる。
本発明の熱可塑性樹脂組成物を製造するには、任意の方法が採用される。例えばA成分〜F成分、および任意に他の成分をそれぞれV型ブレンダー、ヘンシェルミキサー、メカノケミカル装置、押出混合機などの予備混合手段を用いて充分に混合した後、場合により押出造粒器やブリケッティングマシーンなどにより造粒を行い、その後ベント式二軸ルーダーに代表される溶融混練機で溶融混練、およびペレタイザー等の機器によりペレット化する方法が挙げられる。
上記の方法で得られた樹脂組成物の熱伝導率は0.6〜7.0W/mKであり、好ましくは0.8〜7.0W/mKであり、1.0〜7.0W/mKがより好ましい。
本発明の熱可塑性樹脂組成物からなる成形品は、通常そのペレットを射出成形して得ることができる。かかる射出成形においては、通常の成形方法だけでなく、射出圧縮成形、射出プレス成形、ガスアシスト射出成形、発泡成形(超臨界流体を注入する方法を含む)、インサート成形、インモールドコーティング成形、断熱金型成形、急速加熱冷却金型成形、二色成形、サンドイッチ成形、および超高速射出成形などを挙げることができる。また成形はコールドランナー方式およびホットランナー方式のいずれも選択することができる。
また本発明の熱可塑性樹脂組成物を回転成形やブロー成形などにより成形品とすることも可能である。
さらに本発明によれば、熱可塑性樹脂組成物をプレス成形などにより成形品とすることも可能である。
さらに本発明の成形品には、各種の表面処理を行うことが可能である。表面処理としては、ハードコート、撥水・撥油コート、親水性コート、帯電防止コート、紫外線吸収コート、赤外線吸収コート、並びにメタライジング(蒸着など)などの各種の表面処理を行うことができる。表面処理方法としては、液剤のコーティングの他、蒸着法、溶射法、およびメッキ法が挙げられる。蒸着法としては物理蒸着法および化学蒸着法のいずれも使用できる。物理蒸着法としては真空蒸着法、スパッタリング、およびイオンプレーティングが例示される。化学蒸着(CVD)法としては、熱CVD法、プラズマCVD法、および光CVD法などが例示される。特に本発明の樹脂組成物は、ハウジング成形品に好適であることから、電磁波遮蔽用メッキが施されることが好ましく、本発明の樹脂組成物はかかるメッキ特性においても良好である。
(i)剛性(曲げ弾性率)
ISO178に準拠して曲げ弾性率(MPa)を測定した。試験片形状は、長さ80mm×幅10mm×厚み4mmであった。
(ii)外観
角板(150mm×150mm×3mmt)をシリンダー温度300℃、金型温度70℃の型締力150Tの射出成形機により成形し、シルバーストリークの有無を観察した。評価はパージ直後から10ショット目までを廃棄し、その後20ショットまでの成形品をシルバーストリーク評価用とし、評価基準はシルバーストリークが一度でも発生したものは×、一度も発生しなかったものは○として評価した。
(iii)熱伝導率
JIS R 2618に記載の非定常熱線法(プローブ法)に準拠し、京都電子工業(株)製迅速熱伝導測定計 QTM−500にて測定した(試験片形状:150mm×75mm×10mm)。
(A成分)
A−1:ビスフェノールAおよび末端停止剤としてp−tert−ブチルフェノール、並びにホスゲンから界面重縮合法で合成した直鎖状芳香族ポリカーボネート樹脂パウダー(帝人化成(株)製:パンライトL−1225WP(商品名)、粘度平均分子量22,500)
A−2:アクリロニトリル−スチレン共重合体樹脂(第一毛織(株)製:STAREX HF5670(商品名))
A−3:ABS樹脂(日本エイアンドエル(株)製 塊状重合品:サンタック UT−61(商品名))
A−4:PET樹脂(帝人化成(株)製:TR−8580(商品名))
A−5:PBT樹脂(ウインテックポリマー(株)製:700FP(商品名))
(B成分)
B−1:膨張黒鉛(西村黒鉛(株)製:E40(商品名)平均粒径 350μm)
B−2:膨張黒鉛(西村黒鉛(株)製:平均粒径 750μm)
B−3:膨張黒鉛(日本黒鉛(株)製:GR15(商品名)平均粒径15μm)
(B成分以外)
B−4:天然黒鉛(西村黒鉛(株)製 No.5098:平均粒径 350μm)
(C成分)
C−1:無水マレイン酸とα−オレフィンとの共重合体からなる酸変性オレフィンワックス(三菱化学(株)製:ダイヤカルナDC30M)
C−2:無水マレイン酸(和光純薬工業(株)製、試薬特級)
(D成分)
D−1:リン系安定剤(大八化学工業(株)製:TMP トリメチルホスフェート)
(E成分)
E−1:ブロム化ビスフェノールAのカーボネートオリゴマー(帝人化成(株)製;ファイヤガードFG−7000(商品名))
E−2:ビスフェノールAビス(ジフェニルホスフェート)(大八化学工業(株)製CR−741(商品名))
(F成分)
F−1:フィブリル形成能を有するポリテトラフルオロエチレン(ダイキン工業(株)製 ポリフロンMPA FA500(商品名))
表1〜表3に示す組成でポリカーボネート樹脂、アクリロニトリル−スチレン共重合体樹脂、ABS樹脂、PET樹脂、PBT樹脂、膨張黒鉛、酸変性オレフィンワックスおよび無水マレイン酸、並びに他の成分をタンブラーを用いて均一に混合して予備混合物を作成した。尚、タンブラーに供給する際、各成分は以下の濃度となるようにA−1のパウダーと均一に混合したマスターを作成し、かかるマスターをタンブラーに供給した。すなわちC−1、C−2、D−1、およびF−1は10重量%のマスターとした。得られた予備混合物を径30mmφのベント式二軸押出機[(株)日本製鋼所製TEX30XSST]の第1供給口(スクリュー根元部)に供給し、シリンダー温度280℃、スクリュー回転数180rpm、吐出量13kg/h、およびベント減圧度3kPaで溶融押出してペレット化した。
Claims (18)
- 熱可塑性樹脂(A成分)47〜98.97重量部、組成物中での粒径が50μm以下の黒鉛(B成分)1〜50重量部、及び酸性基含有有機化合物(C成分)0.03〜3重量部の合計100重量部からなることを特徴とする熱可塑性樹脂組成物。
- 黒鉛が膨張黒鉛を粉砕して調製した黒鉛である請求項1記載の熱可塑性樹脂組成物。
- 熱可塑性樹脂(A成分)がポリカーボネート樹脂を50重量%以上含有する熱可塑性樹脂である請求項1または2記載の熱可塑性樹脂組成物。
- 熱可塑性樹脂(A成分)が、ポリカーボネート樹脂(A−1成分)並びに、スチレン系樹脂(A−2成分)およびポリエステル系樹脂(A−3成分)からなる群より選ばれる少なくとも1種の熱可塑性樹脂よりなり、A−1〜A−3の合計100重量部に対して、A−1成分が50重量部以上である請求項1〜3のいずれか1項に記載の熱可塑性樹脂組成物。
- 膨張黒鉛の平均粒径が0.1〜1000μmである請求項2〜4のいずれか1項に記載の熱可塑性樹脂組成物。
- 膨張黒鉛の平均粒径が25〜1000μmである請求項2〜4のいずれか1項に記載の熱可塑性樹脂組成物。
- 膨張黒鉛が、比容積100cc/g以上の膨張黒鉛を圧縮処理した後、粉砕した膨張黒鉛である請求項2〜6のいずれか1項に記載の熱可塑性樹脂組成物。
- 酸性基含有有機化合物が、酸性基含有滑剤である請求項1〜7のいずれか1項に記載の熱可塑性樹脂組成物。
- 酸性基含有有機化合物が、カルボキシル基および/またはその酸無水物基を有するオレフィン系ワックスである請求項1〜8のいずれか1項に記載の熱可塑性樹脂組成物。
- (A)〜(C)成分の合計100重量部あたり、リン系安定剤(D成分)0.01〜1重量部を含有してなる請求項1〜9のいずれか1項に記載の熱可塑性樹脂組成物。
- (A)〜(C)成分の合計100重量部あたり、難燃剤(E成分)1〜30重量部を含有してなる請求項1〜10のいずれか1項に記載の熱可塑性樹脂組成物。
- 難燃剤が有機ハロゲン系難燃剤である請求項11記載の熱可塑性樹脂組成物。
- 難燃剤がリン系難燃剤である請求項11記載の熱可塑性樹脂組成物。
- (A)〜(C)成分の合計100重量部あたり、含フッ素滴下防止剤(F成分)0.01〜1重量部を含有してなる請求項1〜13のいずれか1項に記載の熱可塑性樹脂組成物。
- 熱伝導率が0.6〜7.0W/mKである請求項1〜14のいずれか1項に記載の熱可塑性樹脂組成物。
- 請求項1〜15のいずれか1項に記載の熱可塑性樹脂組成物からなる射出成形品。
- 請求項1〜15のいずれか1項に記載の熱可塑性樹脂組成物からなるプレス成形品。
- 請求項1〜15のいずれか1項に記載の熱可塑性樹脂組成物からなる押出成形品。
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