JP2010132850A - 熱可塑性樹脂組成物、それを用いた積層体およびタイヤ - Google Patents
熱可塑性樹脂組成物、それを用いた積層体およびタイヤ Download PDFInfo
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- JP2010132850A JP2010132850A JP2009046905A JP2009046905A JP2010132850A JP 2010132850 A JP2010132850 A JP 2010132850A JP 2009046905 A JP2009046905 A JP 2009046905A JP 2009046905 A JP2009046905 A JP 2009046905A JP 2010132850 A JP2010132850 A JP 2010132850A
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- resin composition
- thermoplastic resin
- polyamide resin
- rubber
- nylon
- Prior art date
- Legal status (The legal status is an assumption and is not a legal conclusion. Google has not performed a legal analysis and makes no representation as to the accuracy of the status listed.)
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- 229920005992 thermoplastic resin Polymers 0.000 title claims abstract description 75
- 239000011342 resin composition Substances 0.000 title claims abstract description 74
- 229920001971 elastomer Polymers 0.000 claims abstract description 85
- 239000005060 rubber Substances 0.000 claims abstract description 81
- 229920006122 polyamide resin Polymers 0.000 claims abstract description 74
- 150000001875 compounds Chemical class 0.000 claims abstract description 31
- 125000003277 amino group Chemical group 0.000 claims abstract description 20
- 125000004018 acid anhydride group Chemical group 0.000 claims abstract description 14
- 239000004593 Epoxy Substances 0.000 claims abstract description 11
- 125000003178 carboxy group Chemical group [H]OC(*)=O 0.000 claims abstract description 11
- 125000003700 epoxy group Chemical group 0.000 claims abstract description 11
- 238000002844 melting Methods 0.000 claims abstract description 9
- 230000008018 melting Effects 0.000 claims abstract description 9
- 238000002156 mixing Methods 0.000 claims abstract description 7
- 239000000203 mixture Substances 0.000 claims description 37
- 229920000219 Ethylene vinyl alcohol Polymers 0.000 claims description 18
- 229920001577 copolymer Polymers 0.000 claims description 16
- 239000004677 Nylon Substances 0.000 claims description 10
- 229920001778 nylon Polymers 0.000 claims description 10
- 229920002725 thermoplastic elastomer Polymers 0.000 claims description 9
- 229920005555 halobutyl Polymers 0.000 claims description 7
- 229920002292 Nylon 6 Polymers 0.000 claims description 6
- 150000001993 dienes Chemical class 0.000 claims description 6
- 229920000089 Cyclic olefin copolymer Polymers 0.000 claims description 5
- 239000004711 α-olefin Substances 0.000 claims description 5
- 229920000642 polymer Polymers 0.000 claims description 4
- JHWNWJKBPDFINM-UHFFFAOYSA-N Laurolactam Chemical compound O=C1CCCCCCCCCCCN1 JHWNWJKBPDFINM-UHFFFAOYSA-N 0.000 claims description 3
- 229920000571 Nylon 11 Polymers 0.000 claims description 3
- 229920000299 Nylon 12 Polymers 0.000 claims description 3
- 229920003189 Nylon 4,6 Polymers 0.000 claims description 3
- 229920000305 Nylon 6,10 Polymers 0.000 claims description 3
- 229920002302 Nylon 6,6 Polymers 0.000 claims description 3
- 229920000572 Nylon 6/12 Polymers 0.000 claims description 3
- 229920003233 aromatic nylon Polymers 0.000 claims description 3
- 238000012986 modification Methods 0.000 claims description 2
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- 238000004519 manufacturing process Methods 0.000 abstract description 4
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- 238000011156 evaluation Methods 0.000 description 19
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- 230000000052 comparative effect Effects 0.000 description 6
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- 239000000126 substance Substances 0.000 description 6
- 239000000654 additive Substances 0.000 description 5
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- 239000003795 chemical substances by application Substances 0.000 description 5
- 238000001125 extrusion Methods 0.000 description 5
- 230000003449 preventive effect Effects 0.000 description 5
- 238000012360 testing method Methods 0.000 description 5
- 238000004073 vulcanization Methods 0.000 description 5
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 4
- 239000000853 adhesive Substances 0.000 description 4
- 230000001070 adhesive effect Effects 0.000 description 4
- 239000000806 elastomer Substances 0.000 description 4
- 229920006225 ethylene-methyl acrylate Polymers 0.000 description 4
- 238000004898 kneading Methods 0.000 description 4
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- 238000002360 preparation method Methods 0.000 description 4
- 239000002994 raw material Substances 0.000 description 4
- XXVUOMFVRJIVLH-UHFFFAOYSA-N 2-(3-methylbutyl)oxirane Chemical compound CC(C)CCC1CO1 XXVUOMFVRJIVLH-UHFFFAOYSA-N 0.000 description 3
- -1 6 7-epoxy-5-decanol Chemical compound 0.000 description 3
- 244000043261 Hevea brasiliensis Species 0.000 description 3
- 229920000459 Nitrile rubber Polymers 0.000 description 3
- 230000015572 biosynthetic process Effects 0.000 description 3
- 239000006229 carbon black Substances 0.000 description 3
- 238000007796 conventional method Methods 0.000 description 3
- 238000000034 method Methods 0.000 description 3
- 229920003052 natural elastomer Polymers 0.000 description 3
- 229920001194 natural rubber Polymers 0.000 description 3
- 230000003014 reinforcing effect Effects 0.000 description 3
- 229920003048 styrene butadiene rubber Polymers 0.000 description 3
- PTOIJBWGCSYXOX-UHFFFAOYSA-N (3-butan-2-yloxiran-2-yl)methanol Chemical compound CCC(C)C1OC1CO PTOIJBWGCSYXOX-UHFFFAOYSA-N 0.000 description 2
- IKASFLJHSHDRIQ-UHFFFAOYSA-N 2,3-di(propan-2-yl)oxirane Chemical compound CC(C)C1OC1C(C)C IKASFLJHSHDRIQ-UHFFFAOYSA-N 0.000 description 2
- YXIOECOAAMLHPG-UHFFFAOYSA-N 2-(2-methylpropyl)oxirane Chemical compound CC(C)CC1CO1 YXIOECOAAMLHPG-UHFFFAOYSA-N 0.000 description 2
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- GQTBMBMBWQJACJ-UHFFFAOYSA-N 2-[(4-butan-2-ylphenoxy)methyl]oxirane Chemical compound C1=CC(C(C)CC)=CC=C1OCC1OC1 GQTBMBMBWQJACJ-UHFFFAOYSA-N 0.000 description 2
- VWDHLRTUFGDYPM-UHFFFAOYSA-N 2-heptan-4-yl-3-methyloxirane Chemical compound CCCC(CCC)C1OC1C VWDHLRTUFGDYPM-UHFFFAOYSA-N 0.000 description 2
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 2
- JOYRKODLDBILNP-UHFFFAOYSA-N Ethyl urethane Chemical compound CCOC(N)=O JOYRKODLDBILNP-UHFFFAOYSA-N 0.000 description 2
- IPRJXAGUEGOFGG-UHFFFAOYSA-N N-butylbenzenesulfonamide Chemical compound CCCCNS(=O)(=O)C1=CC=CC=C1 IPRJXAGUEGOFGG-UHFFFAOYSA-N 0.000 description 2
- FQYUMYWMJTYZTK-UHFFFAOYSA-N Phenyl glycidyl ether Chemical compound C1OC1COC1=CC=CC=C1 FQYUMYWMJTYZTK-UHFFFAOYSA-N 0.000 description 2
- 239000005062 Polybutadiene Substances 0.000 description 2
- 235000021355 Stearic acid Nutrition 0.000 description 2
- NINIDFKCEFEMDL-UHFFFAOYSA-N Sulfur Chemical compound [S] NINIDFKCEFEMDL-UHFFFAOYSA-N 0.000 description 2
- XLOMVQKBTHCTTD-UHFFFAOYSA-N Zinc monoxide Chemical compound [Zn]=O XLOMVQKBTHCTTD-UHFFFAOYSA-N 0.000 description 2
- 230000003712 anti-aging effect Effects 0.000 description 2
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- 238000013329 compounding Methods 0.000 description 2
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- 238000007720 emulsion polymerization reaction Methods 0.000 description 2
- 229920006244 ethylene-ethyl acrylate Polymers 0.000 description 2
- 239000000945 filler Substances 0.000 description 2
- 239000012948 isocyanate Substances 0.000 description 2
- 150000002513 isocyanates Chemical class 0.000 description 2
- 238000000465 moulding Methods 0.000 description 2
- QIQXTHQIDYTFRH-UHFFFAOYSA-N octadecanoic acid Chemical compound CCCCCCCCCCCCCCCCCC(O)=O QIQXTHQIDYTFRH-UHFFFAOYSA-N 0.000 description 2
- OQCDKBAXFALNLD-UHFFFAOYSA-N octadecanoic acid Natural products CCCCCCCC(C)CCCCCCCCC(O)=O OQCDKBAXFALNLD-UHFFFAOYSA-N 0.000 description 2
- 229920002857 polybutadiene Polymers 0.000 description 2
- 239000002861 polymer material Substances 0.000 description 2
- 239000012744 reinforcing agent Substances 0.000 description 2
- 239000000377 silicon dioxide Substances 0.000 description 2
- 239000008117 stearic acid Substances 0.000 description 2
- 229910052717 sulfur Inorganic materials 0.000 description 2
- 239000011593 sulfur Substances 0.000 description 2
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 description 2
- GJEZBVHHZQAEDB-SYDPRGILSA-N (1s,5r)-6-oxabicyclo[3.1.0]hexane Chemical compound C1CC[C@H]2O[C@H]21 GJEZBVHHZQAEDB-SYDPRGILSA-N 0.000 description 1
- WZJFKVHMXBGZBQ-PMACEKPBSA-N (2s)-1-[(5s)-5-benzamido-4-oxo-6-phenylhexanoyl]pyrrolidine-2-carboxylic acid Chemical compound OC(=O)[C@@H]1CCCN1C(=O)CCC(=O)[C@@H](NC(=O)C=1C=CC=CC=1)CC1=CC=CC=C1 WZJFKVHMXBGZBQ-PMACEKPBSA-N 0.000 description 1
- VJHAPKJZBOYGOD-UHFFFAOYSA-N (3-butyloxiran-2-yl)methanol Chemical compound CCCCC1OC1CO VJHAPKJZBOYGOD-UHFFFAOYSA-N 0.000 description 1
- XEVKRTIYWSUXHP-UHFFFAOYSA-N (3-ethyloxiran-2-yl)methanol Chemical compound CCC1OC1CO XEVKRTIYWSUXHP-UHFFFAOYSA-N 0.000 description 1
- MZPZDPXPQAQGJD-UHFFFAOYSA-N (3-heptyloxiran-2-yl)methanol Chemical compound CCCCCCCC1OC1CO MZPZDPXPQAQGJD-UHFFFAOYSA-N 0.000 description 1
- UDSPJJHSJCWGQS-UHFFFAOYSA-N (3-hexyloxiran-2-yl)methanol Chemical compound CCCCCCC1OC1CO UDSPJJHSJCWGQS-UHFFFAOYSA-N 0.000 description 1
- QQHZNUPEBVRUFO-UHFFFAOYSA-N (3-methyloxiran-2-yl)methanol Chemical compound CC1OC1CO QQHZNUPEBVRUFO-UHFFFAOYSA-N 0.000 description 1
- WAZZYUOFCLUJJN-UHFFFAOYSA-N (3-pentan-3-yloxiran-2-yl)methanol Chemical compound CCC(CC)C1OC1CO WAZZYUOFCLUJJN-UHFFFAOYSA-N 0.000 description 1
- PFEZFCUFFWFUKS-UHFFFAOYSA-N (3-pentyloxiran-2-yl)methanol Chemical compound CCCCCC1OC1CO PFEZFCUFFWFUKS-UHFFFAOYSA-N 0.000 description 1
- IGRZECZSICIWJA-UHFFFAOYSA-N (3-propyloxiran-2-yl)methanol Chemical compound CCCC1OC1CO IGRZECZSICIWJA-UHFFFAOYSA-N 0.000 description 1
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- IBDPHWNKHSOBOI-UHFFFAOYSA-N 1-(3-ethyloxiran-2-yl)ethanol Chemical compound CCC1OC1C(C)O IBDPHWNKHSOBOI-UHFFFAOYSA-N 0.000 description 1
- WHKCBQPAXFQSBV-UHFFFAOYSA-N 1-(3-ethyloxiran-2-yl)hexan-1-ol Chemical compound CCCCCC(O)C1OC1CC WHKCBQPAXFQSBV-UHFFFAOYSA-N 0.000 description 1
- AYXTXYQJEHBLFR-UHFFFAOYSA-N 1-(3-ethyloxiran-2-yl)pentan-1-ol Chemical compound CCCCC(O)C1OC1CC AYXTXYQJEHBLFR-UHFFFAOYSA-N 0.000 description 1
- BNMPDFYACKTODG-UHFFFAOYSA-N 1-(3-hexyloxiran-2-yl)ethanol Chemical compound CCCCCCC1OC1C(C)O BNMPDFYACKTODG-UHFFFAOYSA-N 0.000 description 1
- FHIKGRJBSRFOJT-UHFFFAOYSA-N 1-(3-methyloxiran-2-yl)ethanol Chemical compound CC(O)C1OC1C FHIKGRJBSRFOJT-UHFFFAOYSA-N 0.000 description 1
- ZPLXLLINVSRCIY-UHFFFAOYSA-N 1-(3-methyloxiran-2-yl)heptan-1-ol Chemical compound CCCCCCC(O)C1OC1C ZPLXLLINVSRCIY-UHFFFAOYSA-N 0.000 description 1
- NQSSYNHTAYVQIR-UHFFFAOYSA-N 1-(3-methyloxiran-2-yl)hexan-1-ol Chemical compound CCCCCC(O)C1OC1C NQSSYNHTAYVQIR-UHFFFAOYSA-N 0.000 description 1
- SEHZTEMYUSPLDG-UHFFFAOYSA-N 1-(3-methyloxiran-2-yl)pentan-1-ol Chemical compound CCCCC(O)C1OC1C SEHZTEMYUSPLDG-UHFFFAOYSA-N 0.000 description 1
- MADOEHZKQDEEDD-UHFFFAOYSA-N 1-(3-methyloxiran-2-yl)propan-1-ol Chemical compound CCC(O)C1OC1C MADOEHZKQDEEDD-UHFFFAOYSA-N 0.000 description 1
- JIRMQNUHAZAXLE-UHFFFAOYSA-N 1-(3-pentyloxiran-2-yl)propan-1-ol Chemical compound CCCCCC1OC1C(O)CC JIRMQNUHAZAXLE-UHFFFAOYSA-N 0.000 description 1
- LKCZHKBYFPIEID-UHFFFAOYSA-N 1-(3-propan-2-yloxiran-2-yl)ethanol Chemical compound CC(C)C1OC1C(C)O LKCZHKBYFPIEID-UHFFFAOYSA-N 0.000 description 1
- LEJLUUHSOFWJSW-UHFFFAOYSA-N 1-(oxiran-2-yl)ethanol Chemical compound CC(O)C1CO1 LEJLUUHSOFWJSW-UHFFFAOYSA-N 0.000 description 1
- UEQMKUTZHSNXJT-UHFFFAOYSA-N 1-(oxiran-2-yl)heptan-1-ol Chemical compound CCCCCCC(O)C1CO1 UEQMKUTZHSNXJT-UHFFFAOYSA-N 0.000 description 1
- FHHJAZSGOVDVTP-UHFFFAOYSA-N 1-(oxiran-2-yl)hexan-1-ol Chemical compound CCCCCC(O)C1CO1 FHHJAZSGOVDVTP-UHFFFAOYSA-N 0.000 description 1
- GHYVSUWHOOJVGV-UHFFFAOYSA-N 1-(oxiran-2-yl)octan-1-ol Chemical compound CCCCCCCC(O)C1CO1 GHYVSUWHOOJVGV-UHFFFAOYSA-N 0.000 description 1
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- DCURUSMYSILIGA-UHFFFAOYSA-N 2-(2-methylbutyl)oxirane Chemical compound CCC(C)CC1CO1 DCURUSMYSILIGA-UHFFFAOYSA-N 0.000 description 1
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- ILRVDGBLAUXESJ-UHFFFAOYSA-N 2-(2-methylpentyl)oxirane Chemical compound CCCC(C)CC1CO1 ILRVDGBLAUXESJ-UHFFFAOYSA-N 0.000 description 1
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- DLIXVNZBDSURMJ-UHFFFAOYSA-N 2-butan-2-yl-3-methyloxirane Chemical compound CCC(C)C1OC1C DLIXVNZBDSURMJ-UHFFFAOYSA-N 0.000 description 1
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- IKNXPNNMKVOEMV-UHFFFAOYSA-N 2-butyl-3-propyloxirane Chemical compound CCCCC1OC1CCC IKNXPNNMKVOEMV-UHFFFAOYSA-N 0.000 description 1
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- PRYVSVYBXMVHCG-UHFFFAOYSA-N 2-ethyl-3-(2-methylbutyl)oxirane Chemical compound CCC(C)CC1OC1CC PRYVSVYBXMVHCG-UHFFFAOYSA-N 0.000 description 1
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Abstract
【解決手段】ポリアミド樹脂(A)100質量部に対してポリアミド樹脂の末端アミノ基と結合し得る化合物(B)0.05〜5質量部を、ポリアミド樹脂(A)の融点以上で溶融ブレンドさせて得られる変性ポリアミド樹脂(C)と、酸無水物基、エポキシ基、またはカルボキシル基もしくはその誘導体を有する変性ゴム(D)とからなる熱可塑性樹脂組成物である。化合物(B)は、好ましくは単官能エポキシ化合物である。この熱可塑性樹脂組成物は、タイヤ、ホース等の製造に好適に用いられる。
【選択図】なし
Description
本発明は、ポリアミド樹脂の低温耐久性(繰り返し疲労性)を改善するために、ポリアミド樹脂マトリックス中に低温耐久性に優れる変性ゴムを分散充填した熱可塑性樹脂組成物において、変性ゴムを高充填しても流動性を維持し、フィルム製膜が可能であり、かつ低温耐久性に優れる熱可塑性樹脂組成物を提供することを課題とする。
また、本発明において、ポリアミド樹脂(A)は、好ましくは、ナイロン11、ナイロン12、ナイロン6、ナイロン66、ナイロン666、ナイロン612、ナイロン610、ナイロン46、ナイロン66612、および芳香族ナイロンからなる群から選択される少なくとも1種である。
また、本発明において、変性ゴム(D)は、好ましくは、変性ポリアミド樹脂(C)100質量部に対して、50〜150質量部である。
変性ポリアミド樹脂(C)とエチレン−ビニルアルコール共重合体(E)の質量比は、好ましくは、90/10〜10/90であり、変性ゴム(D)は、好ましくは、変性ポリアミド樹脂(C)とエチレン−ビニルアルコール共重合体(E)の合計量100質量部に対して50〜150質量部である。
本発明の積層体は、好ましくは、ゴム組成物シート中のポリマー成分のうち、ハロゲン化ブチルゴムが30〜100質量%である。
また、本発明の熱可塑性樹脂組成物からなるフィルムおよび該フィルムを含む積層体は、タイヤのインナーライナーやホースなど、低温耐久性が要求される用途に用いることができる。
エポキシ基を有する変性ゴムは、たとえば、グリシジルメタクリレートをゴムに共重合させることにより製造することができる。また、エポキシ基を有する変性ゴムは、市販されており、市販品を用いることができる。市販品としては、住友化学株式会社製エポキシ変性エチレンアクリル酸メチル共重合体(エスプレン(登録商標)EMA2752)などがある。
カルボキシル基もしくはその誘導体を有する変性ゴムは、たとえば、エチレンアクリレートをゴムに共重合させることにより製造することができる。また、カルボキシル基もしくはその誘導体を有する変性ゴムは、市販されており、市販品を用いることができる。市販品としては、デュポン株式会社製カルボキシル変性エチレンアクリル酸エチル共重合体(米マックG)などがある。
特に好ましい変性ゴム(D)は、酸無水物基でグラフト変性されたエチレン−α−オレフィン共重合体であり、その例としては、前述の三井化学株式会社製無水マレイン酸変性エチレン−プロピレン共重合体(タフマー(登録商標)MP−0620)がある。
また、ジエン成分を含むゴム組成物には、前記した成分に加えて、カーボンブラックやシリ力などのその他の補強剤(フィラー)、加硫または架橋剤、加硫又は架橋促進剤、可塑剤、各種オイル、老化防止剤などの樹脂およびゴム組成物用に一般に配合されている各種添加剤を配合することができる。これらの添加剤の配合量は本発明の目的に反しない限り、従来の一般的な配合量とすることができる。
ポリアミド樹脂として、次の2種類を用いた。
ナイロン6:宇部興産株式会社製ナイロン6「UBEナイロン」1022B
ナイロン666:宇部興産株式会社製「UBEナイロン」5033B
グリシドール:日油株式会社製エピオール(登録商標)OH
フェニルグリシジルエーテル:日油株式会社製エピオール(登録商標)P
p−sec−ブチルフェニルグリシジルエーテル:日油株式会社製エピオール(登録商標)SB
n−ブチルベンゼンスルホンアミド:大八化学工業株式会社製BM−4
無水マレイン酸変性エチレン−プロピレン共重合体:三井化学株式会社製タフマー(登録商標)MP−0620。以下「MA−EPM」ともいう。
無水マレイン酸変性エチレン−ブテン共重合体:三井化学株式会社製タフマー(登録商標)MH−7020。以下「MA−EBM」ともいう。
無水マレイン酸変性エチレン−オクテン共重合体:エクソンモービルケミカル株式会社製Exxelor(登録商標)VA1803。以下「MA−EOM」ともいう。
無水マレイン酸変性エチレン−アクリル酸エチル共重合体:三井デュポンポリケミカル株式会社製HPR(登録商標)AR201。以下「MA−EEM」ともいう。
エポキシ変性エチレン−アクリル酸メチル共重合体:住友化学株式会社製エスプレン(登録商標)EMA2752。以下「E−EMA」ともいう。
ポリアミド樹脂、単官能エポキシ化合物および可塑剤を、表1に示す質量比率で、2軸混練機(日本製鉄所製TEX44)に投入し、混練機温度230℃で溶融混練し、11種類の変性ポリアミド樹脂MPA−1〜MPA−11を得た。なお、単官能エポキシ化合物を添加せずに、同様の条件で、2種類の未変性ポリアミド樹脂PA−1およびPA−2を得た。
上記のように調製した変性ポリアミド樹脂または未変性ポリアミド樹脂、および無水マレイン酸変性エチレン−プロピレン共重合体を、表2〜表5に示す質量比率で、2軸混練機に投入し、混練機温度220℃で溶融混練し、押出機から連続してストランド状に排出し、水冷後カッターで切断することによりペレット状の熱可塑性樹脂組成物を得た。
さらに、上記のように調製した変性ポリアミド樹脂または未変性ポリアミド樹脂、無水マレイン酸変性エチレン−プロピレン共重合体、およびエチレン−ビニルアルコール共重合体を、表6に示す質量比率で、2軸混練機に投入し、混練機温度220℃で溶融混練し、押出機から連続してストランド状に排出し、水冷後カッターで切断することによりペレット状の熱可塑性樹脂組成物を得た。
得られた熱可塑性樹脂組成物について、溶融粘度、フィルム成形性および−35℃定ひずみ試験(平均破断回数)を次の方法により評価した。
溶融粘度とは、混練加工時の任意の温度、成分の溶融粘度をいい、各ポリマー材料の溶融粘度は、温度、剪断速度および剪断応力の依存性があるため、一般に細管中を流れる溶融状態にある任意の温度、特に混練時の温度領域でのポリマー材料の応力と剪断速度を測定し、下記式より溶融粘度を測定する。
η=剪断応力/剪断速度
本発明においては、東洋精機社製キャピラリーレオメーターキャピログラフ1Cを用いて、250℃、剪断速度250sec−1において、熱可塑性樹脂組成物の溶融粘度(Pa・s)を測定した。溶融粘度が1800Pa・s以下であることが、フィルム成形性の観点から好ましい。
ペレット状の熱可塑性樹脂組成物を、550mm幅T型ダイス付40mmφ単軸押出機(株式会社プラ技研製)を用いて、押出温度C1/C2/C3/C4/ダイ=200/210/230/235/235℃、冷却ロール温度50℃、引き取り速度4m/分の押出条件で、平均厚み150μmのフィルムに成形した。フィルムが成形できたときは○、フィルムが成形できなかったときは×とした。
ペレット状の熱可塑性樹脂組成物を、200mm幅T型ダイス付40mmφ単軸押出機(株式会社プラ技研製)を用いて、押出温度C1/C2/C3/C4/ダイ=200/210/230/235/235℃、冷却ロール温度50℃、引き取り速度0.7m/分の押出条件で、平均厚み1mmのシートに成形した。次いでJIS 3号ダンベルで切断し、−35℃下で40%の繰り返し変形を与えた。5回の測定を行い、破断した回数の平均値を算出し、平均破断回数とする。平均破断回数が10万回以上であるものを合格、10万回未満であるものを不合格とした。
評価結果を表2〜表6に示す。
ゴム組成物を調製するために次の原料を使用した。
ハロゲン化ブチルゴム:LANXESS Rubber社BROMOBUTYL X2
天然ゴム:PT.NUSIRA社製SRI20
乳化重合SBR:日本ゼオン株式会社製NIPOL 1502
GPFカーボンブラック:新日化カーボン株式会社製HTC#G
湿式シリカ:Rhodia社製Zeosil(登録商標)165GR
アロマオイル:昭和シェル石油株式会社製エキストラクト4号S
亜鉛華:正同化学工業株式会社製酸化亜鉛3種
ステアリン酸:日油株式会社製ビーズステアリン酸YR
硫黄:鶴見化学工業株式会社製キンカジルシビフンイオウ150メッシュ
加硫促進剤:大内新興化学工業株式会社製ノクセラーDM
熱可塑性樹脂組成物のフィルム成形性を評価するために用いた方法および条件で、実施例2、3、10および14ならびに比較例11の熱可塑性樹脂組成物を150μmに成形して熱可塑性樹脂組成物フィルムを作製した。一方、上記の未加硫ゴム組成物1〜4を2mmまたは0.5mmに圧延して未加硫ゴム組成物シートを作製した。作製した熱可塑性樹脂組成物フィルムと未加硫ゴム組成物シートを積層して積層体を作製した。作製した積層体について、下記の評価方法で、積層体接着評価、タイヤ走行評価1、タイヤ走行評価2、およびタイヤエア漏れ性能評価を行なった。結果を表8に示す。
150μmに成形した熱可塑性樹脂組成物フィルムおよび2mmに圧延した未加硫ゴム組成物シートを積層した積層体を、180°Cで10分加硫し、JIS2号ダンベルで切断し、次いで、熱可塑性樹脂組成物フィルムの中央部に、幅方向にカット傷を入れたサンプルを作製した。これを70℃下で40%の繰り返し変形を20万回与えた。試験後、カット傷からのフィルムの剥がれを目視で観察し、以下の基準で評価した。
合格:フィルムの剥がれがまったく見られなかったもの、またはカット傷から2mm未満の微小な剥がれが見られるもの、またはゴムの材料破壊であるもの。
不合格:カット傷から2mm以上、10mm以下の剥がれが生じ、界面剥離となっているもの、またはカット傷から大きな剥がれか生じ、界面剥離となっているもの。
150μmに成形した熱可塑性樹脂組成物フィルムおよび0.5mmに圧延した未加硫ゴムシートを積層した積層体をタイヤ用インナーライナー(空気透過防止層用材)として用い、常法によりラジアルタイヤ(195/65R15)を作製した。JATMA規格で規定された標準リムにて140kPaの圧力で空気を封入し、外形1700mmのドラム上を用い、38℃の室温にて、荷重300kN、速度80km/hで距離10000kmを走行させ、走行後の空気透過防止層端部の剥がれ有無を確認した。
合格:まったく剥がれがない場合、または剥がれが2mm未満である場合。
不合格:剥がれが2mm以上である場合。
150μmに成形した熱可塑性樹脂組成物フィルムおよび0.5mmに圧延した未加硫ゴムシ一トを積層した積層体をタイヤ用インナーライナー(空気透過防止層用材)として用い、常法によりラジアルタイヤ(195/65R15)を作製した。JATMA規格で規定された標準リムにて140kPaの圧力で空気を封入し、外形1700mmのドラム上を用い、−20℃の低温下にて、荷重300kN、速度80km/hで距離2000kmを走行させ、走行後の空気透過防止層のクラックの有無を確認した。
合格:10mm未満のクラックが10個未満である場合。
不合格:10mm未満のクラックが10個以上である場合、または10mm以上のクランクが発生した場合。
150μmに成形した熱可塑性樹脂組成物フィルムおよび0.5mmに圧延した未加硫ゴムシートを積層した積層体をタイヤ用インナーライナー(空気透過防止層用材)として用い、常法によりラジアルタイヤ(195/65R15)を作製した。空気圧250kPa、25℃雰囲気下で3か月間内圧変化を測定し、ブチルゴム/天然ゴム80/20量%の標準インナーライナーを使用した同サイズのタイヤと比較し、内圧保持率が同等以上であるものを合格、同等未満であるものを不合格とした。
ゴム組成物4のシートとの積層体を除き、実施例の熱可塑性樹脂組成物のフィルムとゴム組成物のシートとの積層体は、積層体接着評価およびタイヤ走行評価1において合格であった。一方、比較例の熱可塑性樹脂組成物のフィルムとゴム組成物のシートとの積層体は、積層体接着評価およびタイヤ走行評価1においても不合格であった。
Claims (11)
- ポリアミド樹脂(A)100質量部に対してポリアミド樹脂の末端アミノ基と結合し得る化合物(B)0.05〜5質量部を、ポリアミド樹脂(A)の融点以上で溶融ブレンドさせて得られる変性ポリアミド樹脂(C)と、酸無水物基、エポキシ基、またはカルボキシル基もしくはその誘導体を有する変性ゴム(D)とからなる熱可塑性樹脂組成物。
- ポリアミド樹脂の末端アミノ基と結合し得る化合物(B)が単官能エポキシ化合物であることを特徴とする請求項1に記載の熱可塑性樹脂組成物。
- ポリアミド樹脂(A)が、ナイロン11、ナイロン12、ナイロン6、ナイロン66、ナイロン666、ナイロン612、ナイロン610、ナイロン46、ナイロン66612、および芳香族ナイロンからなる群から選択される少なくとも1種であることを特徴とする請求項1または2に記載の熱可塑性樹脂組成物。
- 変性ゴム(D)が、エチレン−α−オレフィン共重合体またはエチレン−不飽和カルボン酸共重合体もしくはその誘導体であることを特徴とする請求項1〜3のいずれか1項に記載の熱可塑性樹脂組成物。
- 変性ゴム(D)が、変性ポリアミド樹脂(C)100質量部に対して、50〜150質量部であることを特徴とする請求項1〜4のいずれか1項に記載の熱可塑性樹脂組成物。
- さらにエチレン−ビニルアルコール共重合体(E)を含む、請求項1〜4のいずれか1項に記載の熱可塑性樹脂組成物。
- 変性ポリアミド樹脂(C)とエチレン−ビニルアルコール共重合体(E)の質量比が90/10〜10/90であり、変性ポリアミド樹脂(C)とエチレン−ビニルアルコール共重合体(E)の合計量100質量部に対して変性ゴム(D)が50〜150質量部であることを特徴とする請求項6に記載の熱可塑性樹脂組成物。
- 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のフィルムを少なくとも1層、およびジエン成分を含むゴム組成物のシートを少なくとも1層含むことを特徴とする積層体。
- ゴム組成物中のポリマー成分のうち、ハロゲン化ブチルゴムが30〜100質量%であることを特徴とする請求項8に記載の積層体。
- 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のフィルムまたは請求項8もしくは9に記載の積層体を含むタイヤ。
- 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のフィルムまたは請求項8もしくは9に記載の積層体を含むホース。
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EP09013322.4A EP2184323B1 (en) | 2008-11-05 | 2009-10-21 | Tire manufactured using a thermoplastic resin composition |
EP10193634.2A EP2287255B1 (en) | 2008-11-05 | 2009-10-21 | Thermoplastic resin composition and laminate and tire manufactured using the same |
US12/610,512 US8344064B2 (en) | 2008-11-05 | 2009-11-02 | Thermoplastic resin composition and laminate and tire manufactured using the same |
CN2009102122125A CN101735600B (zh) | 2008-11-05 | 2009-11-05 | 热塑性树脂组合物以及使用该组合物制成的层合材料和轮胎 |
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CN101735600A (zh) | 2010-06-16 |
JP5247537B2 (ja) | 2013-07-24 |
CN101735600B (zh) | 2013-02-20 |
US8344064B2 (en) | 2013-01-01 |
EP2184323B1 (en) | 2013-05-08 |
EP2287255A3 (en) | 2012-04-04 |
EP2184323A1 (en) | 2010-05-12 |
EP2287255B1 (en) | 2013-07-03 |
EP2287255A2 (en) | 2011-02-23 |
US20100112257A1 (en) | 2010-05-06 |
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