JPWO2017169494A1 - 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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- JPWO2017169494A1 JPWO2017169494A1 JP2018508843A JP2018508843A JPWO2017169494A1 JP WO2017169494 A1 JPWO2017169494 A1 JP WO2017169494A1 JP 2018508843 A JP2018508843 A JP 2018508843A JP 2018508843 A JP2018508843 A JP 2018508843A JP WO2017169494 A1 JPWO2017169494 A1 JP WO2017169494A1
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- AYEKOFBPNLCAJY-UHFFFAOYSA-O thiamine pyrophosphate Chemical compound CC1=C(CCOP(O)(=O)OP(O)(O)=O)SC=[N+]1CC1=CN=C(C)N=C1N AYEKOFBPNLCAJY-UHFFFAOYSA-O 0.000 description 1
- 125000003396 thiol group Chemical group [H]S* 0.000 description 1
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- WTLBZVNBAKMVDP-UHFFFAOYSA-N tris(2-butoxyethyl) phosphate Chemical compound CCCCOCCOP(=O)(OCCOCCCC)OCCOCCCC WTLBZVNBAKMVDP-UHFFFAOYSA-N 0.000 description 1
- LIPMRGQQBZJCTM-UHFFFAOYSA-N tris(2-propan-2-ylphenyl) phosphate Chemical compound CC(C)C1=CC=CC=C1OP(=O)(OC=1C(=CC=CC=1)C(C)C)OC1=CC=CC=C1C(C)C LIPMRGQQBZJCTM-UHFFFAOYSA-N 0.000 description 1
- 239000006097 ultraviolet radiation absorber Substances 0.000 description 1
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- 125000000391 vinyl group Chemical group [H]C([*])=C([H])[H] 0.000 description 1
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- 150000003739 xylenols Chemical class 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- PZRXQXJGIQEYOG-UHFFFAOYSA-N zinc;oxido(oxo)borane Chemical compound [Zn+2].[O-]B=O.[O-]B=O PZRXQXJGIQEYOG-UHFFFAOYSA-N 0.000 description 1
- BHTBHKFULNTCHQ-UHFFFAOYSA-H zinc;tin(4+);hexahydroxide Chemical compound [OH-].[OH-].[OH-].[OH-].[OH-].[OH-].[Zn+2].[Sn+4] BHTBHKFULNTCHQ-UHFFFAOYSA-H 0.000 description 1
- GFQYVLUOOAAOGM-UHFFFAOYSA-N zirconium(iv) silicate Chemical compound [Zr+4].[O-][Si]([O-])([O-])[O-] GFQYVLUOOAAOGM-UHFFFAOYSA-N 0.000 description 1
- IHPKGUQCSIINRJ-UHFFFAOYSA-N β-ocimene Natural products CC(C)=CCC=C(C)C=C IHPKGUQCSIINRJ-UHFFFAOYSA-N 0.000 description 1
Classifications
-
- C—CHEMISTRY; METALLURGY
- C08—ORGANIC MACROMOLECULAR COMPOUNDS; THEIR PREPARATION OR CHEMICAL WORKING-UP; COMPOSITIONS BASED THEREON
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Abstract
Description
1.下記成分(A)〜(C)を含む樹脂組成物。
(A)熱可塑性樹脂 35〜96質量%
(B)難燃剤及び難燃助剤からなる群より選ばれる1種以上である難燃化成分 3〜60質量%
(C)平均繊維径3〜200nmのナノセルロース 0.5〜20質量%
2.前記(A)熱可塑性樹脂が、ポリオレフィン系樹脂及びポリスチレン系樹脂からなる群より選ばれる1種以上である、1に記載の樹脂組成物。
3.前記(A)熱可塑性樹脂がポリプロピレンである、1又は2に記載の樹脂組成物。
4.前記(A)熱可塑性樹脂がブロックポリプロピレンである、1〜3のいずれかに記載の樹脂組成物。
5.前記(A)熱可塑性樹脂のASTM規格D1238によるメルトフローレートが4〜30g/10分である、1〜4のいずれかに記載の樹脂組成物。
6.前記(B)難燃化成分が、難燃剤及び難燃助剤を含む、1〜5のいずれかに記載の樹脂組成物。
7.前記(B)難燃化成分がリン系難燃剤である、1〜5のいずれかに記載の樹脂組成物。
8.前記(B)難燃化成分の融点が250℃以上である、1〜7のいずれかに記載の樹脂組成物。
9.さらに(D)テルペン系樹脂を0.5〜20質量%含む、1〜8のいずれかに記載の樹脂組成物。
10.1〜9のいずれかに記載の樹脂組成物を成形してなる成形体。
本発明の一態様である樹脂組成物は、下記成分(A)〜(C)を含むものである。
(A)熱可塑性樹脂 35〜96質量%
(B)難燃剤及び難燃助剤からなる群より選ばれる1種以上である難燃化成分 3〜60質量%
(C)平均繊維径3〜200nmのナノセルロース 0.5〜20質量%
また、ナノセルロースを使用することにより、低比重にして高剛性とすることができ、かつ、接着性、塗装性等の向上を図ることができる。
また、本明細書において、好ましいとされている規定は任意に採用することができる。即ち、好ましいとされている一の規定を、好ましいとされている他の一又は複数の規定と組み合わせて採用することができる。好ましいもの同士の組み合わせはより好ましいと言える。
以下、本発明の一態様である樹脂組成物に含まれる各成分について説明する。
成分(A)の熱可塑性樹脂としては、例えば、ポリオレフィン系樹脂、ポリスチレン系樹脂、ポリエステル樹脂、ポリアミド樹脂、ポリカーボネート樹脂等が挙げられる。
成分(A)の熱可塑性樹脂は、上記の樹脂のうち1種のみを含んでいてもよく、又は、上記の樹脂のうち1種以上を組み合わせて含んでいてもよい。
尚、本発明において、「ポリオレフィン系樹脂」、「ポリプロピレン系樹脂」、「ポリエチレン系樹脂」とは、それぞれ、樹脂を構成する主成分が、ポリオレフィン、ポリプロピレン、又はポリエチレンであり、他の成分を含んでもよい樹脂をいう。
尚、メルトフローレートは、ASTM規格D1238により測定できる。
成分(B)の難燃化成分は、難燃剤及び難燃助剤からなる群より選択される1種以上である。
ハロゲンを含まないリン系難燃剤としては、ハロゲン非含有有機リン系難燃剤がある。有機リン系難燃剤としては、リン原子を有し、ハロゲンを含まない有機化合物であれば特に制限なく用いることができる。例えば、リン酸エステル化合物、リン酸アミン塩、ポリリン酸アンモニウム等が挙げられる。中でも、リン原子に直接結合するエステル性酸素原子を1つ以上有するリン酸エステル化合物が好ましく用いられる。有機リン系難燃剤以外のハロゲン非含有リン系難燃剤としては、赤リン等がある。
式(IV)において、有機基とは、置換又は未置換のアルキル基、置換又は未置換のシクロアルキル基、置換又は未置換のアリール基等である。置換されている場合の置換基としては、アルキル基、アルコキシ基、アリール基、アリールオキシ基、アリールチオ基等が挙げられ、さらに、これらの置換基を組み合わせた基であるアリールアルコキシアルキル基等、又はこれらの置換基を酸素原子、窒素原子、イオウ原子等により結合して組み合わせたアリールスルホニルアリール基等であってもよい。
シリコーン系難燃剤としては、官能基含有シリコーン化合物、例えば、官能基を有する(ポリ)オルガノシロキサン類が好ましい。具体的には、式R5 aR6 bSiO(4−a−b)/2〔R5は官能基含有基、R6は炭素数1〜12の炭化水素基、0<a≦3、0≦b<3、0<a+b≦3〕で表される基本構造を有する重合体、又は共重合体が好ましい。官能基としては、アルコキシ基、アリールオキシ基、ポリオキシアルキレン基、水酸基、カルボキシル基、シアノール基、アミノ基、メルカプト基、エポキシ基等が挙げられる。官能基含有シリコーン化合物は、異なる官能基を有していてもよく、複数の異なる官能基含有シリコーン化合物を併用してもよい。官能基含有シリコーン化合物は、その官能基(R5)/炭化水素基(R6)の比が、通常0.1〜3であり、好ましくは0.3〜2である。
(CnF2n+1SO3)mM (2)
(式中、nは1〜10の整数を示し、Mはリチウム、ナトリウム、カリウム、セシウム等のアリカリ金属、又はマグネシウム、カルシウム、ストロンチウム、バリウム等のアルカリ土類金属を示し、mはMの原子価を示す。)
これらの化合物としては、例えば、特公昭47−40445号公報に記載されているものがこれに該当する。
本発明の一態様である樹脂組成物において、成分(B)の難燃化成分がリン系難燃剤であることが好ましい。
融点が250℃以上である難燃化成分としては、例えば、水酸化金属塩、ポリリン酸アンモニウム、ポリリン酸塩、ピロリン酸ピペラジン、エチレンビス(ペンタブロモフェニル)等が挙げられる。
尚、「融点がZ℃以上である」とは、難燃化成分が、Z℃以上の温度で溶融するか、又は、Z℃未満の温度では溶融せず、Z℃以上の温度で分解することをいうものとする。
成分(C)のナノセルロースは、平均繊維径が3〜200nmであるセルロースである。
本発明の一態様である樹脂組成物は、さらに(D)テルペン系樹脂を0.5〜20質量%含むことが好ましい。これにより、成分(C)のナノセルロースの樹脂組成物中における分散性をより向上させることが可能となり、よって、成分(B)の難燃化成分による難燃効果も向上させることができる。
また、フェノール類としては、フェノール、クレゾール、キシレノール、ビスフェノールA等が挙げられるが、これらに限定されない。
本発明の一態様である樹脂組成物は、任意成分として、紫外線吸収剤、酸化防止剤、光安定剤、滑剤、結晶核剤、軟化剤、帯電防止剤、充填剤、顔料、染料、強化剤、離型剤、可塑剤、流動性改良剤等を任意の量で含んでもよい。但し、この場合、本発明の一態様である樹脂組成物は、任意成分を除いたときに、成分(A)〜(C)又は成分(A)〜(D)を上記説明した特定の量範囲(質量%)で含むものとする。
また、本発明の一態様である樹脂組成物又はペレットを各種成形機により賦形することにより、成形体とすることができる。成型方法は特に限定されず、射出成形、異形押出成形、シート押出成形等、公知の方法を適用できる。
本発明の一態様である成形体は、上記説明した本発明の一態様である樹脂組成物を成形してなるものである。
本発明の一態様である成形体は、難燃性が高く、成形外観に優れる。
尚、限界酸素指数は、材料が燃焼を持続するために必要な最低酸素濃度を示す指数であり、JIS K7201−2に準拠して測定することができる。
表1〜4に示すように、各成分を所定の割合で配合して樹脂組成物を調製した。このとき、得られた樹脂組成物100質量部に対して、酸化防止剤としてイルガノックス1010(BASF社)0.2質量部、アデカスタブ2112(株式会社ADEKA)0.1質量部を配合した。
この組成物を押出機(機種名:PCM−30、株式会社池貝)に供給し、210〜260℃で溶融混練し、ペレット化した。
引張弾性率は、ASTM D638に準拠して測定した。
限界酸素指数(LOI)は、JIS K7201−2に準拠して測定した。
使用した成分(A)のアイゾッド(IZOD)衝撃強度は、ASTM D256に準拠して、肉厚1/8インチ(1/20.3cm)の試験片を用いて23℃で測定した。
表面外観は、寸法8×8×0.3cmの試験片の一方の表面を観察し、0.1mm以上の寸法の凹みが20個未満存在する場合を「OK」とし、20個以上存在する場合を「NG」と評価した。
試験片における材料の分散状態を評価した。試験片を液体窒素中に1分間浸漬し凍結させてから、折り曲げて破断し、その断面を、走査型電子顕微鏡(SEM)を用いて2000倍で観察し、凝集物が見られない場合を「OK」とし、凝集物がみられる場合を「NG」と評価した。
[成分(A)]
・樹脂1:ホモポリプロピレン(E−105GM、MFR(230℃、2.16kg)=0.5g/10min、IZOD衝撃強度=7kJ/m2、株式会社プライムポリマー)
・樹脂2:ブロックポリプロピレン(J−966HP、MFR(230℃、2.16kg)=30g/10min、IZOD衝撃強度=60kJ/m2、株式会社プライムポリマー)
・難燃剤1:ピロリン酸ピペラジン(FP2050、融点なし、株式会社ADEKA)
・難燃剤2:リン酸エステル(PX−200、融点96℃、大八化学工業株式会社)
・難燃剤3:ポリリン酸アンモニウム(TERRAJU C−30、融点なし、ブーデンハイム社)
・難燃剤4:水酸化マグネシウム(キスマ5AC、融点なし、協和化学工業株式会社)
・難燃剤5:ポリホウ酸ナトリウム(融点なし、株式会社SOUFA)
・難燃剤6:エチレンビス(ペンタブロモフェニル)(サイテックス8010、融点350℃、アルベマール社)
・難燃助剤:三酸化アンチモン(PATOX−M、融点なし、日本精鉱株式会社)
尚、「融点なし」は、押出機のシリンダー温度である210〜260℃では溶融又は分解しないことを意味する。
・ナノセルロース A(CNF−10、平均繊維径30nm、中越パルプ工業)
・セルロースファイバー(SW−10、平均繊維径25μm、セライト社)
・ナノセルロース B(KY−100G、平均繊維径100nm、ダイセルファインケム)
[成分(D)]
・テルペンフェノール(YSポリスターT130(水酸基価60)、ヤスハラケミカル株式会社)
しかし、溶融しない難燃剤(難燃剤1、3〜6)をナノセルロースと共に配合した樹脂組成物では、樹脂中への難燃剤の分散性は良好で、樹脂組成物の難燃性は向上した。
また、溶融する難燃剤(難燃剤2)でも、ナノセルロースを配合しない場合は、ポリプロプレンとの親和性が低く混練できなかったが(比較例10)、ナノセルロースを併用することにより、混錬可能となり、難燃性が向上した。
μmオーダーの寸法を有するセルロースファイバーを配合した樹脂組成物では、弾性率は向上するものの、樹脂組成物中への難燃剤の分散性が悪く、難燃性は向上しなかった。
本願のパリ優先の基礎となる日本出願明細書の内容を全てここに援用する。
Claims (10)
- 下記成分(A)〜(C)を含む樹脂組成物。
(A)熱可塑性樹脂 35〜96質量%
(B)難燃剤及び難燃助剤からなる群より選ばれる1種以上である難燃化成分 3〜60質量%
(C)平均繊維径3〜200nmのナノセルロース 0.5〜20質量% - 前記(A)熱可塑性樹脂が、ポリオレフィン系樹脂及びポリスチレン系樹脂からなる群より選ばれる1種以上である、請求項1に記載の樹脂組成物。
- 前記(A)熱可塑性樹脂がポリプロピレンである、請求項1又は2に記載の樹脂組成物。
- 前記(A)熱可塑性樹脂がブロックポリプロピレンである、請求項1〜3のいずれかに記載の樹脂組成物。
- 前記(A)熱可塑性樹脂のASTM規格D1238によるメルトフローレートが4〜30g/10分である、請求項1〜4のいずれかに記載の樹脂組成物。
- 前記(B)難燃化成分が、難燃剤及び難燃助剤を含む、請求項1〜5のいずれかに記載の樹脂組成物。
- 前記(B)難燃化成分がリン系難燃剤である、請求項1〜5のいずれかに記載の樹脂組成物。
- 前記(B)難燃化成分の融点が250℃以上である、請求項1〜7のいずれかに記載の樹脂組成物。
- さらに(D)テルペン系樹脂を0.5〜20質量%含む、請求項1〜8のいずれかに記載の樹脂組成物。
- 請求項1〜9のいずれかに記載の樹脂組成物を成形してなる成形体。
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