JP5543789B2 - 熱伝導性ポリアルキレンテレフタレート系樹脂組成物および樹脂成形体 - Google Patents
熱伝導性ポリアルキレンテレフタレート系樹脂組成物および樹脂成形体 Download PDFInfo
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- JP5543789B2 JP5543789B2 JP2010011830A JP2010011830A JP5543789B2 JP 5543789 B2 JP5543789 B2 JP 5543789B2 JP 2010011830 A JP2010011830 A JP 2010011830A JP 2010011830 A JP2010011830 A JP 2010011830A JP 5543789 B2 JP5543789 B2 JP 5543789B2
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- CYTQBVOFDCPGCX-UHFFFAOYSA-N trimethyl phosphite Chemical compound COP(OC)OC CYTQBVOFDCPGCX-UHFFFAOYSA-N 0.000 description 1
- QXJQHYBHAIHNGG-UHFFFAOYSA-N trimethylolethane Chemical compound OCC(C)(CO)CO QXJQHYBHAIHNGG-UHFFFAOYSA-N 0.000 description 1
- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 description 1
- WTLBZVNBAKMVDP-UHFFFAOYSA-N tris(2-butoxyethyl) phosphate Chemical compound CCCCOCCOP(=O)(OCCOCCCC)OCCOCCCC WTLBZVNBAKMVDP-UHFFFAOYSA-N 0.000 description 1
- GTOWTBKGCUDSNY-UHFFFAOYSA-K tris[[ethyl(methyl)phosphoryl]oxy]alumane Chemical compound [Al+3].CCP(C)([O-])=O.CCP(C)([O-])=O.CCP(C)([O-])=O GTOWTBKGCUDSNY-UHFFFAOYSA-K 0.000 description 1
- CMPGARWFYBADJI-UHFFFAOYSA-L tungstic acid Chemical compound O[W](O)(=O)=O CMPGARWFYBADJI-UHFFFAOYSA-L 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 229940116269 uric acid Drugs 0.000 description 1
- 238000005292 vacuum distillation Methods 0.000 description 1
- UKRDPEFKFJNXQM-UHFFFAOYSA-N vinylsilane Chemical compound [SiH3]C=C UKRDPEFKFJNXQM-UHFFFAOYSA-N 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 125000005023 xylyl group Chemical group 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- MXMCTPBQIJWVBA-UHFFFAOYSA-L zinc;dimethylphosphinate Chemical compound [Zn+2].CP(C)([O-])=O.CP(C)([O-])=O MXMCTPBQIJWVBA-UHFFFAOYSA-L 0.000 description 1
- PJEUXMXPJGWZOZ-UHFFFAOYSA-L zinc;diphenylphosphinate Chemical compound [Zn+2].C=1C=CC=CC=1P(=O)([O-])C1=CC=CC=C1.C=1C=CC=CC=1P(=O)([O-])C1=CC=CC=C1 PJEUXMXPJGWZOZ-UHFFFAOYSA-L 0.000 description 1
- WMLXDIOQDFWKAO-UHFFFAOYSA-L zinc;methyl(phenyl)phosphinate Chemical compound [Zn+2].CP([O-])(=O)C1=CC=CC=C1.CP([O-])(=O)C1=CC=CC=C1 WMLXDIOQDFWKAO-UHFFFAOYSA-L 0.000 description 1
- GLDFMLDAWXHNQU-UHFFFAOYSA-L zinc;methyl(propyl)phosphinate Chemical compound [Zn+2].CCCP(C)([O-])=O.CCCP(C)([O-])=O GLDFMLDAWXHNQU-UHFFFAOYSA-L 0.000 description 1
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- Compositions Of Macromolecular Compounds (AREA)
Description
(B)窒化硼素及び/又は珪酸マグネシウム塩からなる無機化合物10〜100質量部、
(C)ガラス繊維:20〜90質量部、
(D)アニオン部分が下記式(1)または式(2)で表され、カチオン部分がアルミニウムイオンまたはカルシウムイオンであるホスフィン酸塩10〜60質量部、
(A)ポリアルキレンテレフタレート系樹脂
本発明に用いる(A)ポリアルキレンテレフタレート系樹脂は、(A−1)ポリアルキレンテレフタレート樹脂(いわゆる、ホモポリマー)、(A−2)ポリテトラメチレンエーテルグリコール共重合ポリエステル樹脂、(A−3)ダイマー酸共重合ポリエステル樹脂、および(A−4)イソフタル酸共重合ポリエステル樹脂から構成される。
本発明に用いる(A−1)ポリアルキレンテレフタレート樹脂とは、いわゆるホモポリマーであって、テレフタル酸が全ジカルボン酸成分の50モル%以上を占め、エチレングリコールまたは1,4−ブタンジオールが全ジオールの50質量%以上を占める樹脂をいう。テレフタル酸は全ジカルボン酸成分の80モル%以上を占めるのが好ましく、95モル%以上を占めるのがさらに好ましい。エチレングリコール又は1,4−ブタンジオールは全ジオール成分の80モル%以上を占めるのが好ましく、95モル%以上を占めるのがさらに好ましい。
イソフタル酸共重合ポリエステル樹脂は、1,4−ブタンジオールを主とするグリコールと、テレフタル酸及びイソフタル酸を主とするジカルボン酸を共重合した、共重合ポリエステルである。
本発明に用いる、(B)窒化硼素及び/又は珪酸マグネシウム塩からなる無機化合物は、(B−1)窒化硼素、及び/又は(B−2)珪酸マグネシウム塩からなる無機化合物であり、本発明の樹脂組成物における熱伝導性を大きく向上させるために重要なものである。
本発明に用いる(B−1)窒化硼素としては、c−BN(閃亜鉛鉱構造)、w−BN(ウルツ鉱構造)、h−BN(六方晶構造)、r−BN(菱面体晶構造)等の複数の公知の安定構造を有する窒化硼素を用いることが出来る。中でも六方晶構造の窒化硼素は、成形品を得る際に用いる成形機、及び、金型の摩耗が低減できるので好ましい。
本発明に用いる(B−2)珪酸マグネシウム塩としては、合成物の他、珪酸マグネシウムを主成分とする鉱物、具体的には例えば、タルク、セピオライト、更には、アルミニウム成分も含んだアパタルジャイトなどが挙げられる。本発明においては中でも、熱伝導性の観点から、タルクを用いることが好ましい。
本発明に用いる(C)ガラス繊維は、Aガラス、Cガラス、Eガラス等の組成からなるものが好ましく、特に、Eガラス(無アルカリガラス)がポリアルキレンテレフタレート系樹脂の熱安定性に悪影響を及ぼさない点で好ましい。また一般的には、取り扱いの容易さや、高い強度・剛性および耐熱性を有する成形物を与える点などから、短繊維タイプ(チョップドストランド)のガラス繊維を使用することが好ましい。特に、耐衝撃特性が要求される樹脂成形体の場合には、樹脂成形体中のガラス繊維の繊維長をより長く保つ点から、長繊維タイプのものを使用することが好ましい。これらの充填剤は、単独で又は二種以上組み合わせて使用できる。
本発明においては、難燃剤として(D)ホスフィン酸塩金属を用いる。本発明に用いる(D)ホスフィン酸塩とは、アニオン部分が以下の式(1)又は(2)で表され、カチオン部分がカルシウムイオン、マグネシウムイオン、アルミニウムイオン又は亜鉛イオンの何れかであればよく、中でもカルシウムイオン又はアルミニウムイオンであることが好ましく、特にアルミニウムイオンであることが好ましい。
ウム、メチル−n−プロピルホスフィン酸亜鉛、メタンジ(メチルホスフィン酸)カルシウム、メタンジ(メチルホスフィン酸)マグネシウム、メタンビス(メチルホスフィン酸)アルミニウム、メタンビス(メチルホスフィン酸)亜鉛、ベンゼン−1,4−ビス(メチルホスフィン酸)カルシウム、ベンゼン−1,4−ビス(メチルホスフィン酸)マグネシウム、ベンゼン−1,4−ビス(メチルホスフィン酸)アルミニウム、ベンゼン−1,4−ビス(メチルホスフィン酸)亜鉛、メチルフェニルホスフィン酸カルシウム、メチルフェニルホスフィン酸マグネシウム、メチルフェニルホスフィン酸アルミニウム、メチルフェニルホスフィン酸亜鉛、ジフェニルホスフィン酸カルシウム、ジフェニルホスフィン酸マグネシウム、ジフェニルホスフィン酸アルミニウム、ジフェニルホスフィン酸亜鉛が挙げられる。
本発明においては更に、上述した(A)ポリアルキレンテレフタレート系樹脂に対して(B)〜(D)成分の他に(E)難燃剤を含有させても良く、具体的には、(E−1)リン酸エステル、(E−2)アミノ基含有トリアジン類の塩からなる窒素系難燃剤、(E−3)25℃で固体状態にあるオルガノシロキサン重合体、及び(E−4)硼酸金属塩からなる群より選ばれる少なくとも1つの難燃剤を、各々特定量含有させてもよく、そしてこれらを併用してもよい。
本発明に用いるリン酸エステルの具体例としては、トリメチルホスフェート、トリエチルホスフェート、トリブチルホスフェート、トリオクチルホスフェート、トリブトキシエチルホスフェート、トリフェニルホスフェート、トリクレジルホスフェート、クレジルジフェニルホスフェート、オクチルジフェニルホスフェート等が挙げられる。
また本発明においては、窒素系難燃剤であるアミノ基含有トリアジン類(アミノ基を有するトリアジン類)の塩を配合することによって、比較的少量のホスフィン酸塩の配合で所望の難燃効果を発現させることが出来るので好ましい。
本発明に用いる(E−3)25℃で固体状態にあるオルガノシロキサン重合体の代表的なものは、いわゆるシリコーンレジンであり、その組成は下記式(4)で示される。
(R1SiO3/2)a(R2 2SiO2/2)b(R3 3SiO1/2)c(SiO4/2)d(XO1/2)e (4)
本発明のポリエステル系樹脂組成物は(E−4)硼酸金属塩を含有することが好ましい。本発明に用いられる成分(B−4)硼酸金属塩とは、通常用いる処理条件下で安定であり、揮発成分のないものが好ましい。硼酸金属塩としては硼酸のアルカリ金属塩(例えば、四硼酸ナトリウム、メタ硼酸カリウム等)あるいはアルカリ土類金属塩(例えば、硼酸カルシウム、オルト硼酸マグネシウム、オルト硼酸バリウム、硼酸亜鉛等)等が挙げられる。これらの中でも好ましくは、硼酸亜鉛である。硼酸亜鉛は、一般に、2ZnO・3B2O3・xH2O(x=3.3〜3.7)で示される。水和硼酸亜鉛としては好ましくは、2ZnO・3B2O3・3.5H2Oの式をもつものであり、かつ260℃またはそれより高い温度まで安定なものである。
(A−1)PBT樹脂:三菱エンジニアリングプラスチックス社製ノバデュラン(登録商標)5007、固有粘度0.70dl/g
1,4−ブタンジオールに代えて、PTMGユニット(数平均分子量=約1016)を20質量%共重合したPBT樹脂(三菱エンジニアリングプラスチックス社製ノバデュラン(登録商標)5510、固有粘度:1.3dl/g
テレフタル酸に代えてダイマー酸10モル%を共重合したPBT樹脂(三菱エンジニアリングプラスチックス社製ノバデュラン(登録商標)P02120、固有粘度0.96
テレフタル酸に代えてイソフタル酸10モル%を共重合したPBT樹脂(三菱エンジニアリングプラスチックス社製ノバデュラン(登録商標)5605、固有粘度1.0
(B−1)窒化硼素:
電気化学工業社製SGP(商品名)、鱗片状、純度:99%、平均粒子径:18μm
松村産業社製ハイフィラー#12C(商品名)、圧縮タルク、平均粒子径:5〜7μm、嵩比重:0.75〜0.9g/ml
(C−1)旭ファイバーグラス社製チョップドストランド03JA−FT592(商品名) 円形断面
ジエチルホスフィン酸アルミニウム:クラリアントジャパン社製OP1240(商品名)
(E−1)リン酸エステル化合物:
レゾルシノール型芳香族リン酸エステル化合物(1,3フェニレンビスジキシレニルホスフェート)、大八化学社製PX200(商品名)
シアヌル酸メラミン、サンケミカル社製MCA(商品名)、平均粒径5μm
フェニルシリコーンレジン、東レ・ダウコーニング社製217Flake(商品名)、25℃で固体状態 軟化点86℃
(E−4−1)硼酸亜鉛:ボラックス・ジャパン社製ファイヤーブレイクZB(商品名)
キンセイマテック社製 硼酸カルシウム鉱(主成分は2CaO・3B2O3・5H2O)、平均粒径5μm
酸化防止剤:ヒンダードフェノール系化合物 チバ・スペシャリティー・ジャパン社製イルガノックス1010(商品名)
ホスファゼン化合物:
環状物を主体とするホスファゼン化合物 伏見製薬所社製FP−100(商品名)
ポリペンタブロモベンジルアクリレート ブロモケム・ファーイースト社製FR−1025(商品名)
三酸化アンチモン:鈴裕化学社製ファイアカットAT−3CN(商品名)
表1に記載の配合比(数値は質量部を示す。)にて、ガラス繊維以外の成分を一括してスーパーミキサー(新栄機械製SK−350型)で混合し、L/D=42の2軸押出機(日本製鋼所社製、TEX30HSST)のホッパーに投入し、(C)ガラス繊維をサイドフィードして、吐出量20kg/時間、スクリュー回転数150rpm、バレル温度260℃の条件下で押出してポリアルキレンテレフタレート系樹脂組成物のペレットを得た。その際のストランドの状態により次の3段階に分類し、◎または○であれば、実用上使用可能である。
○:ほとんどストランド切れなく押出可能。
△:ストランド切れ多発。押出困難。
(1)レーザー印字性:
テストピースに次の条件でNd−YAGレーザーにより、レーザーマーキングを行い、評価した。装置は、日本電気社製 マーカーエンジン SL475H/HFを用い、大出力:50W以上、レーザーマーキングの出力電流値:10Aまたは15A、発振波長:1060nm、超音波Qスイッチ:2KHz、スキャニング速度:200mm/secとした。マーキング図柄は、2枚のプレートに各々、異なるマーキングを施した。1枚のプレートには20×20mmの正方形を塗りつぶす様にマーキングさせ、別の1枚には計10文字のアルファベット(ABCDEFGHIJ)を、フォント5mmでマーキングした。
○:鮮明なマーキングが成されており、容易に認識が可能。
×:全くマーキングが成されてない、又は、印字されているが認識困難
射出成形機(住友重機械工業製、SH100、型締め力100T)により、樹脂温度(パージ樹脂の実測温度):260℃、金型温度:80℃、金型:縦100mm、横100mm、厚み3mmの条件で射出成形した成形品を、抵抗率計((株)アドバンテスト製:R8340デジタル超高抵抗/微少電流計およびR12704レジスティビティ・チェンバ)にて測定した。体積抵抗率はΩ・cmの単位で表示する。この値は1014Ω・cm以上であることが好ましい。
射出成形機( 住友重機械工業製、SH100、型締め力100T) を用いて、樹脂温度(パージ樹脂の実測温度):260℃、金型温度:80℃にて、金型: 縦100mm、横100mm、厚み3mmの成形品を射出成形し、得られた射出成形品を3枚重ねて、迅速熱伝導率測定装置(京都電子工業製、Kemtherm QTM―D3)を用いて、射出成形品の熱伝導率を測定した。
樹脂組成物のスパイラルフロー長さを、射出成形機として住友重機械(株)製SE50を用いて評価した。射出圧力170MPa、射出速度100mm/sec、シリンダー温度270℃、射出時間2sec、冷却7sec、金型温度80℃、サックバック1mmの条件とした。また評価した樹脂成形品の形状は、断面が肉厚1mm、幅1.5mmの、長尺状樹脂成形品であり、渦巻き状となったものである。この渦巻き状長尺樹脂成形品の大きさは、長尺状樹脂成形品の中心間距離として、90mm×105mmである。この渦巻き状長尺樹脂成形品の模式図を図1に示す。
試験片(厚み3mmの平板)について、国際規格 IEC60112に定める試験法によりPTIを決定した。このPTIは、25V刻みの保証電圧の数値である。PTIは固体電気絶縁材料の表面に電界が加わった状態で湿潤汚染されたとき、600Vから100Vの間の電圧におけるトラッキングに対する対抗性を示すものであり、550V以上が要求され、好ましくは600V以上である。
UL試験片(厚み0.75mm)について、アンダーライターズ・ラボラトリーズ(Underwriter’s Laboratories Inc.)のUL−94規格垂直燃焼試験により実施した。難燃性レベルは該規格に従い、V−0>V−1>V−2>HBの順で評価した。Total燃焼時間は、5本の合計燃焼時間(第1接炎時、第2接炎時を含む)である。
表1に記載の配合比(数値は質量部を示す。)にて、ガラス繊維以外の成分を一括してスーパーミキサー(新栄機械社製SK−350型)で混合し、L/D=42の2軸押出機(日本製鋼所社製、TEX30HSST)のホッパーに投入し、(C)ガラス繊維をサイドフィードして、吐出量20kg/時間、スクリュー回転数150rpm、バレル温度260℃の条件下押出してポリアルキレンテレフタレート樹脂組成物のペレットを得た。
上記表より次のことが明白となる。
(1)実施例と比較例を比較すると、本発明の樹脂組成物は、熱伝導率、耐トラッキング特性および、難燃性の全てに優れていることがわかる。
(2)異形断面GFを配合した実施例では、丸断面GFを配合した実施例(実施例1、12)と比較して、熱伝導率が上昇することが分かる。さらに、トータル燃焼時間も減少するという、意外な効果を奏することが分かる。
(3)実施例3〜13の様に、(A)成分に共重合ポリエステル樹脂を併用することで、(併用していない実施例1、2との対比により)、生産性に優れていることが分かる。
(4)実施例10〜13より、オルガノシロキサン共重合体と硼酸金属塩とを併用した場合に、レーザー印字性も優れ、さらにトータル燃焼時間も減少することが分かる。
Claims (6)
- (A)ポリアルキレンテレフタレート系樹脂100質量部に対して、下記(B)〜(D)成分を含むことを特徴とするポリアルキレンテレフタレート系樹脂組成物;
(B)窒化硼素及び/又は珪酸マグネシウム塩からなる無機化合物10〜100質量部
(C)繊維の長さ方向に直角な断面の長径をD2、短径をD1とするとき、D2/D1比(扁平率)が1.5〜10の範囲のものであるガラス繊維20〜90質量部
(D)アニオン部分が下記式(1)または式(2)で表され、カチオン部分がアルミニウムイオンまたはカルシウムイオンであるホスフィン酸塩10〜60質量部
- (A)成分が、カルボン酸成分及びアルコール成分のそれぞれ70モル%以上がテレフタル酸及び1,4−ブタンジオールに由来するものであり、且つ共重合成分としてポリテトラメチレンエーテルグリコール、ダイマー酸及びイソフタル酸の何れかに由来する成分を含有しているものであることを特徴とする請求項1記載のポリアルキレンテレフタレート系樹脂組成物。
- 前記(B)成分における珪酸マグネシウム塩が、タルクであることを特徴とする請求項1または2に記載のポリアルキレンテレフタレート系樹脂組成物。
- タルクの嵩比重が0.4以上であることを特徴とする請求項3に記載のポリアルキレンテレフタレート系樹脂組成物。
- 更に、下記(E−1)〜(E−4)からなる群より選ばれる少なくとも1つの(E)難燃剤を含有することを特徴とする請求項1乃至4の何れかに記載のポリアルキレンテレフタレート系樹脂組成物。
(E−1)リン酸エステル0.1〜20質量部
(E−2)アミノ基含有トリアジン類の塩からなる窒素系難燃剤1〜50質量部
(E−3)25℃で固体状態にあるオルガノシロキサン重合体1〜10質量部
(E−4)硼酸金属塩0.1〜4質量部 - 請求項1乃至5のいずれかに記載のポリアルキレンテレフタレート系樹脂組成物を射出成形してなる樹脂成形品。
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