JP4481718B2 - 難燃性熱可塑性樹脂組成物 - Google Patents
難燃性熱可塑性樹脂組成物 Download PDFInfo
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- JP4481718B2 JP4481718B2 JP2004140959A JP2004140959A JP4481718B2 JP 4481718 B2 JP4481718 B2 JP 4481718B2 JP 2004140959 A JP2004140959 A JP 2004140959A JP 2004140959 A JP2004140959 A JP 2004140959A JP 4481718 B2 JP4481718 B2 JP 4481718B2
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- 239000011342 resin composition Substances 0.000 title claims description 93
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- 239000003063 flame retardant Substances 0.000 title claims description 67
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- QQOMQLYQAXGHSU-UHFFFAOYSA-N 2,3,6-Trimethylphenol Chemical compound CC1=CC=C(C)C(O)=C1C QQOMQLYQAXGHSU-UHFFFAOYSA-N 0.000 description 5
- 239000003963 antioxidant agent Substances 0.000 description 5
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- CDDWAYFUFNQLRZ-UHFFFAOYSA-N soyasapogenol A Natural products CC12CCC(O)C(C)(CO)C1CCC1(C)C2CC=C2C3CC(C)(C)C(O)C(O)C3(C)CCC21C CDDWAYFUFNQLRZ-UHFFFAOYSA-N 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 239000004575 stone Substances 0.000 description 1
- 229920001909 styrene-acrylic polymer Polymers 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 239000012756 surface treatment agent Substances 0.000 description 1
- 229920003002 synthetic resin Polymers 0.000 description 1
- 229920001897 terpolymer Polymers 0.000 description 1
- ISIJQEHRDSCQIU-UHFFFAOYSA-N tert-butyl 2,7-diazaspiro[4.5]decane-7-carboxylate Chemical compound C1N(C(=O)OC(C)(C)C)CCCC11CNCC1 ISIJQEHRDSCQIU-UHFFFAOYSA-N 0.000 description 1
- 150000003512 tertiary amines Chemical class 0.000 description 1
- JRMUNVKIHCOMHV-UHFFFAOYSA-M tetrabutylammonium bromide Chemical compound [Br-].CCCC[N+](CCCC)(CCCC)CCCC JRMUNVKIHCOMHV-UHFFFAOYSA-M 0.000 description 1
- RKHXQBLJXBGEKF-UHFFFAOYSA-M tetrabutylphosphanium;bromide Chemical compound [Br-].CCCC[P+](CCCC)(CCCC)CCCC RKHXQBLJXBGEKF-UHFFFAOYSA-M 0.000 description 1
- 229940073455 tetraethylammonium hydroxide Drugs 0.000 description 1
- LRGJRHZIDJQFCL-UHFFFAOYSA-M tetraethylazanium;hydroxide Chemical compound [OH-].CC[N+](CC)(CC)CC LRGJRHZIDJQFCL-UHFFFAOYSA-M 0.000 description 1
- 229920006345 thermoplastic polyamide Polymers 0.000 description 1
- 229920002803 thermoplastic polyurethane Polymers 0.000 description 1
- 150000003609 titanium compounds Chemical class 0.000 description 1
- VZCYOOQTPOCHFL-UHFFFAOYSA-N trans-butenedioic acid Natural products OC(=O)C=CC(O)=O VZCYOOQTPOCHFL-UHFFFAOYSA-N 0.000 description 1
- 238000012546 transfer Methods 0.000 description 1
- STCOOQWBFONSKY-UHFFFAOYSA-N tributyl phosphate Chemical compound CCCCOP(=O)(OCCCC)OCCCC STCOOQWBFONSKY-UHFFFAOYSA-N 0.000 description 1
- DQWPFSLDHJDLRL-UHFFFAOYSA-N triethyl phosphate Chemical compound CCOP(=O)(OCC)OCC DQWPFSLDHJDLRL-UHFFFAOYSA-N 0.000 description 1
- CNUJLMSKURPSHE-UHFFFAOYSA-N trioctadecyl phosphite Chemical compound CCCCCCCCCCCCCCCCCCOP(OCCCCCCCCCCCCCCCCCC)OCCCCCCCCCCCCCCCCCC CNUJLMSKURPSHE-UHFFFAOYSA-N 0.000 description 1
- QOQNJVLFFRMJTQ-UHFFFAOYSA-N trioctyl phosphite Chemical compound CCCCCCCCOP(OCCCCCCCC)OCCCCCCCC QOQNJVLFFRMJTQ-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
- QQBLOZGVRHAYGT-UHFFFAOYSA-N tris-decyl phosphite Chemical compound CCCCCCCCCCOP(OCCCCCCCCCC)OCCCCCCCCCC QQBLOZGVRHAYGT-UHFFFAOYSA-N 0.000 description 1
- 150000003755 zirconium compounds Chemical class 0.000 description 1
- 150000007934 α,β-unsaturated carboxylic acids Chemical class 0.000 description 1
- 239000004711 α-olefin Substances 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Manufacture Of Macromolecular Shaped Articles (AREA)
Description
シャーシに適した樹脂組成物としては従来より数多くが提案されている。
(A)芳香族ポリカーボネート(A−1成分)、スチレン系硬質ポリマー(A−2成分)、およびポリフェニレンエーテル(A−3成分)より選ばれる少なくとも1種の熱可塑性ポリマー(A成分)、
(B)有機リン系難燃剤(B成分)より選ばれる少なくとも1種の難燃剤(B成分)、
(C−1)平均粒子径0.5〜30μmのタルク(C−1成分)、
(C−2)マイカ(C−2成分)、
(D)繊維状充填材(D成分)
30≦c1+c2+d≦65 (1)
0.5≦(c1+c2)/(c1+c2+d)≦0.9 (2)
0.4≦c1/(c1+c2)≦0.8 (3)
0.6≦λ≦1.5 (4)
(ここで、λはJIS R2618に基づく非定常熱線法により測定された樹脂組成物の23℃における熱伝導率(W/m・K)を表す。)
<A成分について>
本発明のA成分は、芳香族ポリカーボネート(A−1成分)、スチレン系硬質ポリマー樹脂(A−2成分)、およびポリフェニレンエーテル(A−3成分)より選ばれる少なくとも1種の熱可塑性ポリマーである。
本発明B成分の有機リン系難燃剤の配合は、樹脂組成物の曲げ弾性率を向上させ低比重化が可能である。より好適な有機リン系難燃剤としては、下記一般式(i)で表される1種または2種以上のホスフェート化合物を挙げることができる。
本発明でC−1成分として使用するタルクとは、層状構造を持った鱗片状の粒子であり、化学組成的には含水珪酸マグネシウムであり、一般的には化学式4SiO2・3MgO・2H2Oで表され、通常SiO2を56〜65重量%、MgOを28〜35重量%、H2O約5重量%程度から構成されている。その他の少量成分としてFe2O3が0.03〜1.2重量%、Al2O3が0.05〜1.5重量%、CaOが0.05〜1.2重量%、K2Oが0.2重量%以下、Na2Oが0.2重量%以下などを含有しており、比重は約2.7である。本発明は、上記の特定粒径のタルクにマイカを併用することにより、適度な剛性、寸法精度、機械的特性、および振動特性を有しつつ、良好な熱伝導性を有する難燃性熱可塑性樹脂組成物を達成する。かように同じ板状無機充填材である特定粒径のタルクとマイカを併用し、良好な難燃性熱可塑性樹脂を達成し得ることは従来知られていなかった。
本発明のC−2成分として使用されるマイカとしては、剛性確保の面から、平均粒径が10〜500μmの粉末状のものが好ましい。マイカとは、アルミニウム、カリウム、マグネシウム、ナトリウム、鉄等を含んだケイ酸塩鉱物の粉砕物である。マイカには白雲母、金雲母、黒雲母、人造雲母等があり、本発明で使用するマイカとしてはいずれのマイカも使用できるが、白雲母は金雲母や黒雲母に比べてそれ自体が剛直であり、剛性の点では白雲母が好適である。また、金雲母、黒雲母は白雲母に比べて主成分中にFeが多く含まれているためそれ自体の色相が黒っぽくなり、種々の着色をする場合にも白雲母は好適である。また白雲母は、人造雲母(天然金雲母のOH基がFに置換されたもの)が高価であるのに対しても有利である。したがって本発明においては種々の点から白雲母が好適である。
本発明の繊維状充填剤は、上述のとおりガラス繊維が特に好ましい。ガラス繊維は、Aガラス、Cガラス、Eガラス等のガラス組成を特に限定するものでなく、場合によりTiO2、SO3、P2O5等の成分を含有するものであってもよい。但しより好ましくは、Eガラス(無アルカリガラス)が芳香族ポリカーボネート樹脂に悪影響を及ぼさない点で好ましい。ガラス繊維は溶融ガラスを種々の方法にて延伸しながら急冷し、所定の繊維状にしたものである。かかる場合の急冷および延伸条件についても特に限定されるものでない。また断面の形状は一般的な真円状の他に、異形断面形状であってもよい。異形断面形状としては、例えば真円状の繊維を平行に重ね合わせた形状などが代表的である。さらに真円状と異形断面形状の混合したガラス繊維であってもよい。またこれらのガラス繊維は、エポキシ樹脂、ウレタン樹脂、アクリル樹脂、オレフィン樹脂、シリコーン樹脂、高級脂肪酸エステルなど(樹脂にはオリゴマー、ワックスなどを含む)により集束処理することができる。かかる集束処理剤の量としては、集束処理されたガラス繊維100重量%中0.05〜10重量%が好ましく、より好ましくは0.1〜5重量%である。またシランカップリング剤、チタネートカップリング剤、およびアルミネートカップリング剤等で表面処理されたものが好ましい。付着量の測定はJIS R3420「ガラス繊維一般試験方法」に準じて測定した値である。即ち、ガラス繊維を110℃×1時間乾燥後、その重量を基準とし600℃×30分間加熱した時の重量%で表したものである。
本発明の難燃性熱可塑性樹脂組成物は、離型剤を含有することが好ましい。これにより更に寸法精度が良好でかつ成形サイクルの短縮化が可能な難燃性熱可塑性樹脂組成物が提供される。ここで離型剤としては、オレフィン系ワックス、シリコーンオイル、フッ素オイル、オルガノポリシロキサン、一価または多価アルコールと高級脂肪酸とのエステル、パラフィンワックス、および蜜蝋などが例示されるが、中でも好適には一価または多価アルコールと高級脂肪酸とのエステル(E成分)である。高級脂肪酸は、好ましくは炭素数20以上(より好ましくは炭素数20〜32、更に好ましくは炭素数26〜32)の脂肪酸を60重量%以上含有する。かかる高級脂肪酸として、モンタン酸を主成分とする高級脂肪酸が好ましく例示される。かかる高級脂肪酸は通常モンタンロウを酸化することにより製造される。一方、一価アルコールとしては、例えばドデカノール、テトラデカノール、ヘキサデカノール、オクタデカノール、エイコサノール、テトラコサノール、セリルアルコール、およびトリアコンタノールなどが例示される。
本発明の難燃性熱可塑性樹脂組成物は、上述のとおり更に臭素系難燃剤を含有することが好ましい。かかる臭素系難燃剤としては、臭素化カーボネートオリゴマー、臭素化エポキシ化合物、臭素化ポリスチレン、臭素化トリアジン化合物、臭素化ジフェニルアルカン系化合物、臭素化インダン系化合物、および臭素化芳香族フタルイミド系化合物などが挙げられ、中でもA成分との相溶性に優れ、その耐熱性および熱安定性が良好であることから臭素化カーボネートオリゴマー、臭素化エポキシ化合物が好ましい。
本発明の難燃性熱可塑性樹脂組成物は、上記A成分、B成分、C−1成分、C−2成分およびD成分の必須成分を特定割合で含むものである。かかる割合について次に説明する。
30≦c1+c2+d≦65 (1)
0.5≦(c1+c2)/(c1+c2+d)≦0.9 (2)
0.4≦c1/(c1+c2)≦0.8 (3)
本発明のA−1成分として用いる芳香族ポリカーボネートは、二価フェノールとカーボネート前駆体とを反応させて得られるものである。反応の方法としては界面重縮合法、溶融エステル交換法、カーボネートプレポリマーの固相エステル交換法、および環状カーボネート化合物の開環重合法などを挙げることができる。
比粘度(ηSP)=(t−t0)/t0
[t0は塩化メチレンの落下秒数、tは試料溶液の落下秒数]
求められた比粘度を次式にて挿入して粘度平均分子量Mを求める。
ηSP/c=[η]+0.45×[η]2c(但し[η]は極限粘度)
[η]=1.23×10−4M0.83
c=0.7
本発明のスチレン系硬質ポリマー(A−2成分)は、芳香族ビニル化合物の重合体または共重合体、またこれらと共重合可能な他のビニル単量体とを共重合して得られる重合体をいう。芳香族ビニル化合物は該ポリマー100重量%中少なくとも30重量%以上含有することが好ましい。
本発明のA−3成分であるポリフェニレンエーテルとは、フェニレンエーテル構造を有する核置換フェノールの重合体または共重合体(以下単にPPE重合体と称する場合がある)である。
本発明の難燃性熱可塑性樹脂組成物は、本発明の目的を損なわない範囲においてC−1成分、C−2成分およびD成分以外の無機充填材を少量含むことも可能である。
本発明の難燃性熱可塑性樹脂組成物は、C−1成分もしくはC−2成分(好ましくはC−1成分およびC−2成分)とA成分とを溶融混練する際、該溶融混練がB成分の共存下でなされることにより製造されたものが好ましい。更にD成分の繊維状充填材は、A成分、B成分、およびC−1成分もしくはC−2成分(好ましくはC−1成分およびC−2成分)とを含有する溶融状態の樹脂組成物中に供給されることが好ましい。
表1〜表4に記載の成分を以下の要領でベント式二軸押出機[日本製鋼所(株)製TEX−30XSST]を用い、溶融混練して樹脂組成物のペレットを得た。原料は最後部の第1供給口(表中“計量器”欄において1−1、1−2および1−3のもの)および押出機途中の第2供給口(表中“計量器”欄において2−1および2−2のもの)より供給した。かかる押出機は、第1供給口から第2供給口の間にニーディングディスクによる混練ゾーンがあり、その直後に開放されたベント口が設けられていた。ベント口の長さはスクリュー径(D)に対して約2Dであった。かかるベント口の後にサイドフィーダーが設置され第2供給口から供給された原料が溶融された樹脂中に供給された。サイドフィーダー以後に更にニーディングディスクによる混練ゾーンおよびそれに続くベント口が設けられていた。かかる部分のベント口の長さは約1.5Dであり、その部分では真空ポンプを使用し3kPaの真空下とした。
(2)成形収縮率:幅50mm×長さ100mm×厚さ4mmの試験片を同一の条件で射出成形により成形し、23℃、50%RH雰囲気にて24時間放置した後、試験片寸法を3次元測定機(ミツトヨ(株)製MICROPAK550)により測定し、成形収縮率を算出した。尚、上記試験片は、幅50mmおよび厚み1.5mmのフィルムゲートを長さ方向の一端に有する金型キャビティを用いて成形されたものである。従って、長さ方向が流れ方向、および幅方向が流れ方向と直角の方向となる。
(3)燃焼性:UL94垂直燃焼試験を実施した(試験片厚み:1.5mm)。
(4)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)製熱伝導測定計 KEMTHERM QTM−D3にて測定した(試験片形状:150mm×75mm×10mm)。
(5)セルフタップ強度:外径8mm×内径2.5mm×深さ10mmの試験片を作成し、呼び径3mm、長さ8mmのBタイトネジ(日東精工(株)製)を用いて1.1N・mの締付けトルクにて締め付け試験をn=5にて行い、ネジバカ、ボス割れの有無について評価した。尚、n=5の試験全てでネジバカ、ボス割れが無かった場合を合格、n=5の試験で1回でもネジバカ、ボス割れが発生した場合を不合格とした。
(A成分)
PC: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)
AS: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)、GPC測定による標準ポリスチレン換算の重量平均分子量:95000、アクリロニトリル成分含有量:28.5重量%、スチレン成分含有量:71.5重量%)
ABS:ABS樹脂(日本エイアンドエル(株)製:サンタック UT−61(商品名))
PPE:ポリフェニレンエーテル樹脂(旭化成(株)製:ザイロン300H(商品名))
PFR−1:レゾルシノールビス(ジキシレニルホスフェート)(旭電化工業(株)製:アデカスタブFP−500(商品名);TGA5%重量減少温度=351.0℃)
PFR−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);TGA5%重量減少温度=335.9℃)
(C−1成分)
タルク−1:圧縮処理されていないタルク((株)勝光山鉱業所製;ビクトリライトSG−A(商品名)、かさ密度:0.52g/cm3、アンドレアゼンピペット法で平均粒子径約15μm)
タルク−2:圧縮処理されたタルク((株)勝光山鉱業所製;ビクトリライトTK−RC(商品名)、かさ密度:0.80g/cm3、アンドレアゼンピペット法で平均粒子径2μm)
(C−2成分)
マイカ−1:集束処理されていないマイカ(林化成(株)製;MC−40(商品名)、白雲母、かさ密度:0.30g/cm3、振動式篩分け法で平均粒子径約250μm、乾式粉砕、pH=6.92(JIS K5101))
マイカ−2:集束処理されていないマイカ(林化成(株)製;MC−250(商品名)、白雲母、かさ密度:0.30g/cm3、マイクロトラックレーザー法で平均粒子径約40μm:乾式粉砕、pH=7.0(JIS K5101))
マイカ−3:集束処理されたマイカ(山口雲母工業所(株)製;ミカレット41PU5(商品名)、白雲母、集束処理剤付着量:約0.8%、かさ密度:0.65g/cm3、マイクロトラックレーザー法で平均粒子径40μm、湿式粉砕)
マイカ−4:集束処理されていないマイカ(山口雲母工業所(株)製;B−82(商品名)、白雲母、かさ密度:0.22g/cm3、マイクロトラックレーザー法で平均粒子径170μm、振動式篩い分け法で平均粒子径90μm、湿式粉砕)
GF:ガラス繊維(日東紡績(株)製;3PE937(商品名)、繊維径:13μm、カット長:3mm、アミノシラン処理−エポキシ/ウレタン系集束ガラス繊維、処理剤付着量:約1.0%、かさ密度:0.80g/cm3)
(E成分)
Wax:モンタン酸エチレングリコールエステル(クラリアントジャパン(株)製;Licolub−WE1(商品名)」
(F成分)
B−FR: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))
添加剤−1:トリメチルホスフェート(大八化学工業(株)製;TMP(商品名))
添加剤−2:テトラキス(2,4−ジ−tert−ブチルフェニル)4,4’−ビフェニレン−ジホスホナイトを主成分とする安定剤(クラリアントジャパン(株)製;サンドスタブP−EPQ PLUS(商品名))
添加剤−3:酸変性ポリオレフィン系ワックス(三菱化学(株)製;ダイヤカルナ30M(商品名))
添加剤−4:カーボンブラックマスター(カーボンブラック40重量%/粘度平均分子量15,000の芳香族ポリカーボネート樹脂60重量%)
添加剤−5:カーボンブラックマスター(越谷化成工業(株)製;ROYALBLACK 904S(商品名)、カーボンブラック40重量%/PS樹脂60重量%)
Claims (9)
- 下記A成分、B成分、C−1成分、C−2成分およびD成分の合計を100重量%としたときA成分は20〜65重量%、B成分は1〜20重量%であり、C−1成分はc1重量%、C−2成分はc2重量%およびD成分はd重量%であって、該c1、c2およびdは下記式(1)〜(3)の条件を満足する難燃性熱可塑性樹脂組成物。
(A)芳香族ポリカーボネート(A−1成分)、スチレン系硬質ポリマー(A−2成分)、およびポリフェニレンエーテル(A−3成分)より選ばれる少なくとも1種の熱可塑性ポリマー(A成分)、
(B)有機リン系難燃剤(B成分)より選ばれる少なくとも1種の難燃剤(B成分)、
(C−1)平均粒子径0.5〜30μmのタルク(C−1成分)、
(C−2)平均粒子径10〜500μmのマイカ(C−2成分)、
(D)繊維状充填材(D成分)
30≦c1+c2+d≦65 (1)
0.5≦(c1+c2)/(c1+c2+d)≦0.9 (2)
0.4≦c1/(c1+c2)≦0.8 (3) - 更に一価または多価アルコールと高級脂肪酸とのエステル(E成分)をA成分、B成分、C−1成分、C−2成分およびD成分の合計100重量部あたり、0.01〜2重量部含んでなる請求項1に記載の難燃性熱可塑性樹脂組成物。
- 上記難燃性熱可塑性樹脂組成物は、UL規格94−Vに準拠する1.5mm厚みの試験片の燃焼試験において、燃焼ランクとしてV−1以上を満足するものである請求項1または請求項2のいずれかに記載の難燃性熱可塑性樹脂組成物。
- 更に臭素系難燃剤(F成分)をA成分、B成分、C−1成分、C−2成分およびD成分の合計100重量部あたり、0.1〜20重量部含んでなる請求項1〜請求項3のいずれか1項に記載の難燃性熱可塑性樹脂組成物。
- 上記繊維状充填材(D成分)がガラス繊維である請求項1〜請求項4のいずれか1項に記載の難燃性熱可塑性樹脂組成物。
- A成分は、その100重量%中A−1成分および/またはA−3成分50〜99重量%とA−2成分1〜50重量%からなる請求項1〜請求項5のいずれか1項に記載の難燃性熱可塑性樹脂組成物。
- 上記難燃性熱可塑性樹脂組成物は、下記式(4)を満足する請求項1〜請求項6のいずれか1項に記載の難燃性熱可塑性樹脂組成物。
0.6≦λ≦1.5 (4)
(ここで、λはJIS R2618に基づく非定常熱線法(プローブ法)により測定された樹脂組成物の23℃における熱伝導率(W/m・K)を表す。) - 請求項1〜請求項7のいずれか1項に記載の難燃性熱可塑性樹脂組成物より形成された成形品。
- 請求項1〜請求項7のいずれか1項に記載の難燃性熱可塑性樹脂組成物より形成された重量800〜3,000gのシャーシ成形品。
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