JP6038163B2 - ポリプロピレン系樹脂組成物およびその用途 - Google Patents
ポリプロピレン系樹脂組成物およびその用途 Download PDFInfo
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- JP6038163B2 JP6038163B2 JP2014536857A JP2014536857A JP6038163B2 JP 6038163 B2 JP6038163 B2 JP 6038163B2 JP 2014536857 A JP2014536857 A JP 2014536857A JP 2014536857 A JP2014536857 A JP 2014536857A JP 6038163 B2 JP6038163 B2 JP 6038163B2
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- OTCKOJUMXQWKQG-UHFFFAOYSA-L magnesium bromide Chemical compound [Mg+2].[Br-].[Br-] OTCKOJUMXQWKQG-UHFFFAOYSA-L 0.000 description 1
- 229910001623 magnesium bromide Inorganic materials 0.000 description 1
- ZLNQQNXFFQJAID-UHFFFAOYSA-L magnesium carbonate Chemical compound [Mg+2].[O-]C([O-])=O ZLNQQNXFFQJAID-UHFFFAOYSA-L 0.000 description 1
- 239000001095 magnesium carbonate Substances 0.000 description 1
- 229910000021 magnesium carbonate Inorganic materials 0.000 description 1
- 239000000395 magnesium oxide Substances 0.000 description 1
- CPLXHLVBOLITMK-UHFFFAOYSA-N magnesium oxide Inorganic materials [Mg]=O CPLXHLVBOLITMK-UHFFFAOYSA-N 0.000 description 1
- 235000019359 magnesium stearate Nutrition 0.000 description 1
- YJCTUQFSSZSZPO-UHFFFAOYSA-L magnesium;chloride;phenoxide Chemical compound [Cl-].[Mg+]OC1=CC=CC=C1 YJCTUQFSSZSZPO-UHFFFAOYSA-L 0.000 description 1
- KRTCPMDBLDWJQY-UHFFFAOYSA-M magnesium;ethanolate;chloride Chemical compound [Mg+2].[Cl-].CC[O-] KRTCPMDBLDWJQY-UHFFFAOYSA-M 0.000 description 1
- ZHLDMBMNKCIBQN-UHFFFAOYSA-M magnesium;methanolate;chloride Chemical compound [Cl-].CO[Mg+] ZHLDMBMNKCIBQN-UHFFFAOYSA-M 0.000 description 1
- AXZKOIWUVFPNLO-UHFFFAOYSA-N magnesium;oxygen(2-) Chemical compound [O-2].[Mg+2] AXZKOIWUVFPNLO-UHFFFAOYSA-N 0.000 description 1
- IWYDHOAUDWTVEP-UHFFFAOYSA-N mandelic acid Chemical compound OC(=O)C(O)C1=CC=CC=C1 IWYDHOAUDWTVEP-UHFFFAOYSA-N 0.000 description 1
- 150000002736 metal compounds Chemical class 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- XPDGHGYGTJOTBC-UHFFFAOYSA-N methoxy(methyl)silicon Chemical compound CO[Si]C XPDGHGYGTJOTBC-UHFFFAOYSA-N 0.000 description 1
- 239000003607 modifier Substances 0.000 description 1
- XOSNGXNHDRYFEF-UHFFFAOYSA-N monohexyl phthalate Chemical compound CCCCCCOC(=O)C1=CC=CC=C1C(O)=O XOSNGXNHDRYFEF-UHFFFAOYSA-N 0.000 description 1
- QEALYLRSRQDCRA-UHFFFAOYSA-N myristamide Chemical compound CCCCCCCCCCCCCC(N)=O QEALYLRSRQDCRA-UHFFFAOYSA-N 0.000 description 1
- WQEPLUUGTLDZJY-UHFFFAOYSA-N n-Pentadecanoic acid Natural products CCCCCCCCCCCCCCC(O)=O WQEPLUUGTLDZJY-UHFFFAOYSA-N 0.000 description 1
- STWWIMKSHFDZEK-UHFFFAOYSA-N n-[butoxy(diethoxy)silyl]propan-1-amine Chemical compound CCCCO[Si](OCC)(OCC)NCCC STWWIMKSHFDZEK-UHFFFAOYSA-N 0.000 description 1
- UYKUVUUMSFADKE-UHFFFAOYSA-N n-[diethoxy(propoxy)silyl]ethanamine Chemical compound CCCO[Si](NCC)(OCC)OCC UYKUVUUMSFADKE-UHFFFAOYSA-N 0.000 description 1
- DQZXTSUCHBQLOB-UHFFFAOYSA-N n-[diethoxy(propoxy)silyl]propan-1-amine Chemical compound CCCN[Si](OCC)(OCC)OCCC DQZXTSUCHBQLOB-UHFFFAOYSA-N 0.000 description 1
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 1
- FDYPWIDITZJTAI-UHFFFAOYSA-N n-ethyl-n-trimethoxysilylethanamine Chemical compound CCN(CC)[Si](OC)(OC)OC FDYPWIDITZJTAI-UHFFFAOYSA-N 0.000 description 1
- CBKZJLJZZXOLDS-UHFFFAOYSA-N n-ethyl-n-tripropoxysilylethanamine Chemical compound CCCO[Si](OCCC)(OCCC)N(CC)CC CBKZJLJZZXOLDS-UHFFFAOYSA-N 0.000 description 1
- QLXYCGCVGODGGB-UHFFFAOYSA-N n-methyl-n-triethoxysilylmethanamine Chemical compound CCO[Si](OCC)(OCC)N(C)C QLXYCGCVGODGGB-UHFFFAOYSA-N 0.000 description 1
- QFQJTKJFFSOFJV-UHFFFAOYSA-N n-propyl-n-triethoxysilylpropan-1-amine Chemical compound CCCN(CCC)[Si](OCC)(OCC)OCC QFQJTKJFFSOFJV-UHFFFAOYSA-N 0.000 description 1
- 229910052757 nitrogen Inorganic materials 0.000 description 1
- FJDUDHYHRVPMJZ-UHFFFAOYSA-N nonan-1-amine Chemical compound CCCCCCCCCN FJDUDHYHRVPMJZ-UHFFFAOYSA-N 0.000 description 1
- 239000002667 nucleating agent Substances 0.000 description 1
- XNGIFLGASWRNHJ-UHFFFAOYSA-N o-dicarboxybenzene Natural products OC(=O)C1=CC=CC=C1C(O)=O XNGIFLGASWRNHJ-UHFFFAOYSA-N 0.000 description 1
- ZWLPBLYKEWSWPD-UHFFFAOYSA-N o-toluic acid Chemical class CC1=CC=CC=C1C(O)=O ZWLPBLYKEWSWPD-UHFFFAOYSA-N 0.000 description 1
- IOQPZZOEVPZRBK-UHFFFAOYSA-N octan-1-amine Chemical compound CCCCCCCCN IOQPZZOEVPZRBK-UHFFFAOYSA-N 0.000 description 1
- LTHCSWBWNVGEFE-UHFFFAOYSA-N octanamide Chemical compound CCCCCCCC(N)=O LTHCSWBWNVGEFE-UHFFFAOYSA-N 0.000 description 1
- 229960002446 octanoic acid Drugs 0.000 description 1
- 239000001301 oxygen Substances 0.000 description 1
- 229910052760 oxygen Inorganic materials 0.000 description 1
- 238000010422 painting Methods 0.000 description 1
- 230000000737 periodic effect Effects 0.000 description 1
- 230000002093 peripheral effect Effects 0.000 description 1
- 239000002530 phenolic antioxidant Substances 0.000 description 1
- 125000001997 phenyl group Chemical group [H]C1=C([H])C([H])=C(*)C([H])=C1[H] 0.000 description 1
- 239000011574 phosphorus Substances 0.000 description 1
- 229910052698 phosphorus Inorganic materials 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000012545 processing Methods 0.000 description 1
- SCUZVMOVTVSBLE-UHFFFAOYSA-N prop-2-enenitrile;styrene Chemical compound C=CC#N.C=CC1=CC=CC=C1 SCUZVMOVTVSBLE-UHFFFAOYSA-N 0.000 description 1
- 239000001294 propane Substances 0.000 description 1
- 238000004064 recycling Methods 0.000 description 1
- 238000011160 research Methods 0.000 description 1
- 238000010092 rubber production Methods 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 150000004671 saturated fatty acids Chemical class 0.000 description 1
- 238000006748 scratching Methods 0.000 description 1
- 239000012321 sodium triacetoxyborohydride Substances 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 239000010959 steel Substances 0.000 description 1
- 125000001424 substituent group Chemical group 0.000 description 1
- 239000005720 sucrose Substances 0.000 description 1
- 239000011593 sulfur Substances 0.000 description 1
- 229910052717 sulfur Inorganic materials 0.000 description 1
- 239000000725 suspension Substances 0.000 description 1
- ASEHKQZNVUOPRW-UHFFFAOYSA-N tert-butyl(triethoxy)silane Chemical compound CCO[Si](OCC)(OCC)C(C)(C)C ASEHKQZNVUOPRW-UHFFFAOYSA-N 0.000 description 1
- JHVNMGWNEQGGDU-UHFFFAOYSA-N tert-butyl-diethoxy-methylsilane Chemical compound CCO[Si](C)(C(C)(C)C)OCC JHVNMGWNEQGGDU-UHFFFAOYSA-N 0.000 description 1
- NETBVGNWMHLXRP-UHFFFAOYSA-N tert-butyl-dimethoxy-methylsilane Chemical compound CO[Si](C)(OC)C(C)(C)C NETBVGNWMHLXRP-UHFFFAOYSA-N 0.000 description 1
- 150000003608 titanium Chemical class 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- 230000007704 transition Effects 0.000 description 1
- 229910052723 transition metal Inorganic materials 0.000 description 1
- 150000003624 transition metals Chemical group 0.000 description 1
- PTCWADDVLPYBBZ-UHFFFAOYSA-N tricyclopentylmethoxysilane Chemical compound C1CCCC1C(C1CCCC1)(O[SiH3])C1CCCC1 PTCWADDVLPYBBZ-UHFFFAOYSA-N 0.000 description 1
- JCVQKRGIASEUKR-UHFFFAOYSA-N triethoxy(phenyl)silane Chemical compound CCO[Si](OCC)(OCC)C1=CC=CC=C1 JCVQKRGIASEUKR-UHFFFAOYSA-N 0.000 description 1
- IOPAQHDEQBHWEB-UHFFFAOYSA-N trimethoxy-(2-methylcyclopentyl)silane Chemical compound CO[Si](OC)(OC)C1CCCC1C IOPAQHDEQBHWEB-UHFFFAOYSA-N 0.000 description 1
- 235000021122 unsaturated fatty acids Nutrition 0.000 description 1
- 150000004670 unsaturated fatty acids Chemical class 0.000 description 1
- 230000000007 visual effect Effects 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
Classifications
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- C08L23/00—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers
- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
- C08L23/12—Polypropene
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- B62D—MOTOR VEHICLES; TRAILERS
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- B62D29/00—Superstructures, understructures, or sub-units thereof, characterised by the material thereof
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- C08K3/18—Oxygen-containing compounds, e.g. metal carbonyls
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- C08L23/04—Homopolymers or copolymers of ethene
- C08L23/08—Copolymers of ethene
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- C08L23/02—Compositions of homopolymers or copolymers of unsaturated aliphatic hydrocarbons having only one carbon-to-carbon double bond; Compositions of derivatives of such polymers not modified by chemical after-treatment
- C08L23/10—Homopolymers or copolymers of propene
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- B29C45/00—Injection moulding, i.e. forcing the required volume of moulding material through a nozzle into a closed mould; Apparatus therefor
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Description
(A)(a−1)JIS K 7210に準拠した方法で測定したメルトフローレート(MFR、230℃、21.16N荷重)が10g/10min以上300g/10min以下であって、プロピレンから導かれる構成単位の含量が98mol%以上100mol%以下であり、エチレンと炭素原子数4〜8のα−オレフィンから選ばれる少なくとも1種のα−オレフィンから導かれる構成単位の含量が0mol%以上2mol%以下であるプロピレン系重合体30〜80重量部と、
(a−2)135℃デカリン中で測定した極限粘度[η]が1.5dl/g以上8dl/g以下、エチレンから導かれる構成単位の含量が30mol%以上60mol%以下であるプロピレン・エチレン共重合体0〜30重量部と
からなり、(a−1)と(a−2)の合計が30〜80重量部であるポリプロピレン系樹脂と、
(B)エチレン含有率が65mol%以上90mol%以下である、エチレンと、炭素原子数3〜8のα−オレフィンから選ばれる少なくとも1種のα−オレフィンからなるエチレン・α−オレフィン共重合体20〜50重量部と、
(E)無機充填材0〜40重量部と、
からなり、(a−2)と(B)との合計が20〜50重量部である基材成分(ただし、(A)、(B)、(E)との合計が100重量部である)100重量部に対して、
(C)脂肪酸アミド0.2〜1重量部、および
(D)界面活性剤0.2〜1重量部
を含む。
前記(C)脂肪酸アミドが、炭素原子数8〜25の脂肪酸アミドおよびその2量体より選ばれる1種以上であり、かつ、
前記(D)界面活性剤が、炭素原子数が8〜25であるエステル基を、1つまたは2つ有する化合物であることが好ましい。
<ポリプロピレン系樹脂組成物>
本発明のポリプロピレン系樹脂組成物は、ポリプロピレン系樹脂(A)とエチレン・α−オレフィン共重合体(B)と、必要に応じて(E)無機充填材からなる基材成分と、脂肪酸アミド(C)および界面活性剤(D)を含む。
本発明のポリプロピレン系樹脂組成物を構成する基材成分は、ポリプロピレン系樹脂(A)と、エチレン・α−オレフィン共重合体(B)と、必要に応じて(E)無機充填材からなる。
ポリプロピレン系樹脂(A)は、(a−1)プロピレン系重合体を必須成分とし、必要に応じて(a−2)プロピレン・エチレン共重合体を含む。
本発明に係る(a−1)成分のプロピレン系重合体は、プロピレンの単独重合体またはプロピレンと少量のα−オレフィンとの共重合体である。ここでα−オレフィンとは、エチレンと炭素原子数4〜8のα−オレフィンから選ばれる少なくとも1種のα−オレフィンであり、好ましくはエチレンである。
ポリプロピレン系樹脂(A)には、上述したプロピレン系重合体(a−1)に加え、必要に応じて、(a−2)プロピレン・エチレン共重合体が含まれてもよい。
本発明に係るポリプロピレン系樹脂(A)は、(a−1)プロピレン系重合体を必須成分とし、必要に応じて(a−2)プロピレン・エチレン共重合体を含む。
ポリプロピレン系樹脂(A)を構成する、プロピレン系重合体(a−1)および必要に応じてプロピレン・エチレン共重合体(a−2)は、上述の通り、公知のオレフィン重合用触媒の存在下に、重合あるいは共重合を行って調製することができる。オレフィン重合用触媒としては、具体的には、たとえば、固体状チタン触媒成分(I)と、有機金属化合物触媒成分(II)とを含む触媒を用いることができる。
[固体状チタン触媒成分(I)]
固体状チタン触媒成分(I)は、チタン、マグネシウム、ハロゲン及び必要に応じて電子供与体を含む。この固体状チタン触媒成分(I)としては、公知の固体状チタン触媒成分を制限無く用いることができる。
(式中、Rは炭化水素基であり、Xはハロゲン原子であり、gは0≦g≦4である。)
より具体的には、TiCl4、TiBr4等のテトラハロゲン化チタン;Ti(OCH3)Cl3、Ti(OC2H5)Cl3、Ti(O−n−C4H9)Cl3、Ti(OC2H5)Br3、Ti(O−isoC4H9)Br3等のトリハロゲン化アルコキシチタン;Ti(OCH3)2Cl2、Ti(OC2H5)2Cl2等のジハロゲン化アルコキシチタン;Ti(OCH3)3Cl、Ti(O−n−C4H9)3Cl、Ti(OC2H5)3Br等のモノハロゲン化アルコキシチタン;Ti(OCH3)4、Ti(OC2H5)4、Ti(OC4H9)4、Ti(O−2−エチルヘキシル)4等のテトラアルコキシチタン等を挙げることができる。
任意のR11〜R36、好ましくはR11及びR12は共同してベンゼン環以外の環を形成していてもよい。
有機金属化合物触媒成分(II)としては、第13族金属を含む化合物、たとえば、有機アルミニウム化合物、第1族金属とアルミニウムとの錯アルキル化物、第2族金属の有機金属化合物等を用いることができる。
(式中、R及びR’は炭化水素基であり、nは0<n<4の整数である。)
上記式で示される有機ケイ素化合物としては、具体的には、ジイソプロピルジメトキシシラン、t−ブチルメチルジメトキシシラン、t−ブチルメチルジエトキシシラン、t−アミルメチルジエトキシシラン、ジシクロヘキシルジメトキシシラン、シクロヘキシルメチルジメトキシシラン、シクロヘキシルメチルジエトキシシラン、ビニルトリメトキシシラン、ビニルトリエトキシシラン、t−ブチルトリエトキシシラン、フェニルトリエトキシシラン、シクロヘキシルトリメトキシシラン、シクロペンチルトリメトキシシラン、2−メチルシクロペンチルトリメトキシシラン、シクロペンチルトリエトキシシラン、ジシクロペンチルジメトキシシラン、ジシクロペンチルジエトキシシラン、トリシクロペンチルメトキシシラン、ジシクロペンチルメチルメトキシシラン、ジシクロペンチルエチルメトキシシラン、シクロペンチルジメチルエトキシシラン等が用いられる。
式中、Raは、炭素数1〜6の炭化水素基であり、Raとしては、炭素数1〜6の不飽和あるいは飽和脂肪族炭化水素基等が挙げられ、特に好ましくは炭素数2〜6の炭化水素基が挙げられる。具体例としてはメチル基、エチル基、n−プロピル基、iso−プロピル基、n−ブチル基、iso−ブチル基、sec−ブチル基、n−ペンチル基、iso−ペンチル基、シクロペンチル基、n−ヘキシル基、シクロヘキシル基等が挙げられ、これらの中でもエチル基が特に好ましい。
式中、RNは、環状アミノ基であり、この環状アミノ基として、例えば、パーヒドロキノリノ基、パーヒドロイソキノリノ基、1,2,3,4−テトラヒドロキノリノ基、1,2,3,4−テトラヒドロイソキノリノ基、オクタメチレンイミノ基等が挙げられる。
このように、不活性炭化水素媒体を用いる場合、予備重合はバッチ式で行うことが好ましい。
この場合には、予備重合を連続的に行うのが好ましい。
プロピレン重合体成分を製造する工程として好ましいのは、バルク重合や懸濁重合等の液相重合あるいは気相重合法である。
分子量を調整するために必要な水素量は、使用する製造プロセスの種類、重合温度、圧力によって異なるため、適宜調整すればよい。
本発明のポリプロピレン系樹脂組成物を構成する、エチレン・α−オレフィン共重合体(B)は、エチレンと炭素数3〜8のα−オレフィンとの共重合体である。
本発明のポリプロピレン系樹脂組成物を構成する基材成分には、無機充填材(E)が含まれていてもよい。
本発明のポリプロピレン系樹脂組成物を構成する基材成分は、上述したプロピレン系重合体(a−1)および必要に応じてプロピレン・エチレン共重合体(a−2)からなるポリプロピレン系樹脂(A)と、エチレン・α−オレフィン共重合体(B)と、必要に応じて(E)無機充填材からなる。このような基材成分は、(a−1)、(a−2)、(B)、(E)の合計100重量部中に、(a−1)を30〜80重量部、(a−2)を0〜30重量部、(B)を20〜50重量部、(E)を0〜40重量部含有するものであり、好ましくは、(a−1)を30〜75重量部、(a−2)を0〜25重量部、(B)を20〜40重量部、(E)を0〜40重量部含有する。
本発明のポリプロピレン系樹脂組成物を構成する脂肪酸アミド(C)は、滑剤あるいは帯電防止剤として作用する脂肪酸アミドであることが好ましい。本発明で用いられる脂肪酸アミドは、飽和脂肪酸アミドであっても、不飽和脂肪酸アミドであってもよく、好ましくは、炭素原子数8〜25の脂肪酸アミドおよびその2量体であり、より好ましくは炭素原子数8〜25の脂肪酸アミド、さらに好ましくは炭素原子数15〜25の脂肪酸アミドである。
本発明のポリプロピレン系樹脂組成物を構成する界面活性剤(D)は、ポリプロピレン系樹脂組成物中において、帯電防止剤としての作用を有するものであることが好ましい。
本発明のポリプロピレン系樹脂組成物には、必要に応じて、耐熱安定剤、耐候安定剤、耐光安定剤、老化防止剤、酸化防止剤、脂肪酸金属塩、軟化剤、分散剤、充填剤、着色剤、顔料などのその他の添加剤(F)が、本発明の目的を損なわない範囲で配合されていてもよい。
本発明のポリプロピレン系樹脂組成物は、(a−1)プロピレン系重合体と必要に応じて(a−2)プロピレン・エチレン共重合体とからなるポリプロピレン系樹脂(A)と、エチレン・α−オレフィン共重合体(B)と、必要に応じて無機充填材(E)からなる基材成分と、脂肪酸アミド(C)および界面活性剤(D)を含む。これらの含有量は、それぞれ以下のとおりである。
本発明の成形体は、上記本発明のポリプロピレン系樹脂組成物からなる。
JIS K 7210に準拠し、230℃、21.16N荷重の条件でメルトフローレート(MFR)を測定した。
まず、試料を5g精秤し、1,000ミリリットルのナス型フラスコに入れ、さらにBHT(ジブチルヒドロキシトルエン、フェノール系酸化防止剤)1gを添加した後、回転子及びn−デカン700ミリリットルを投入した。
フーリエ変換赤外線分光法(FT−IR)により測定した。
デカリン溶媒を用いて、135℃で測定した。サンプル約20mgをデカリン15mlに溶解し、135℃のオイルバス中で比粘度ηspを測定した。このデカリン溶液にデカリン溶媒を5ml追加して希釈後、同様にして比粘度ηspを測定した。この希釈操作をさらに2回繰り返し、濃度(C)を0に外挿した時のηsp/Cの値を極限粘度([η]:〔dl/g〕)として求めた。
・ゴム摩擦による傷付き試験(Scuff足蹴り試験)
樹脂組成物を金型に射出成形して製造し、表面にシボを有する成形体を、成形後1週間以上経過した状態で、試験前に23℃恒温状態で2時間以上静置して状態調節したものを、テストピースとして用いた。テストピースの形状は、縦120cm、横80cm、高さ0.3cmであった。
1.テストピース(1)を装置の台座(3)上に固定する。
2.デジタルデップスゲ−ジを振り子上部にセットし、ゲージの先端を振り子上部へ当て、ゲージの目盛りが0mmになることを確認する。
3.パンタグラフ(4)のレバーを回転させ、台座を上昇させゲージの目盛りが0.3mmになるよう合せる。
4.摩擦物(ゴム試験片)(2)を装着した振り子先端を所定の高さ((5)、傷付き試験面より20cm)の高さまで引き上げる。
5.振り子を放し、テストピース(1)の試験面へゴムを擦る。
6.試験面(6)の傷つき性を目視で判断する。
(1)固体状チタン触媒成分の調製
無水塩化マグネシウム952g、デカン4420mlおよび2−エチルヘキシルアルコール3906gを、130℃で2時間加熱して均一溶液とした。この溶液中に無水フタル酸213gを添加し、130℃にてさらに1時間攪拌混合を行って無水フタル酸を溶解させた。
固体状チタン触媒成分87.5g、トリエチルアルミニウム99.8mL、ジエチルアミノトリエトキシシラン28.4ml、ヘプタン12.5Lを内容量20Lの攪拌機付きオートクレーブに挿入し、内温15〜20℃に保ちプロピレンを875g挿入し、100分間攪拌しながら反応させた。重合終了後、固体成分を沈降させ、上澄み液の除去およびヘプタンによる洗浄を2回行った。得られた前重合触媒を精製ヘプタンに再懸濁して、固体触媒成分濃度で0.7g/Lとなるよう、ヘプタンにより調整を行った。
内容量1000Lの攪拌機付きベッセル重合器に、プロピレンを131kg/時間、触媒スラリーを遷移金属触媒成分として0.70g/時間、トリエチルアルミニウム19.6mL/時間、ジエチルアミノトリエトキシシラン4.2mL/時間を連続的に供給し、水素を気相部の水素濃度が5.3mol%になるように供給した。重合温度75℃、圧力3.5MPa/Gで重合を行った。
製造例1の固体状チタン触媒成分の調製(1)で得た固体状チタン触媒成分を用い、前重合触媒の製造(2)および本重合(3)を以下のようにして行った。
固体触媒成分86.0g、トリエチルアルミニウム39.2mL、2−イソブチル−2−イソプロピル−1,3−ジメトキシプロパン11.0ml、ヘプタン4.6Lを内容量20Lの攪拌機付きオートクレーブに挿入し、内温10〜15℃に保ちプロピレンを860g挿入し、180分間攪拌しながら反応させた。重合終了後、固体成分を沈降させ、上澄み液の除去およびヘプタンによる洗浄を2回行った。得られた前重合触媒を精製ヘプタンに再懸濁して、固体触媒成分濃度で1.0g/Lとなるよう、ヘプタンにより調整を行った。
内容量58Lのジャケット付循環式管状重合器にプロピレンを40kg/時間、水素を204NL/時間、(2)で製造した触媒スラリーを固体触媒成分として0.66g/時間、トリエチルアルミニウム2.5ml/時間、ジシクロペンチルジメトキシシラン1.4ml/時間を連続的に供給し、気相の存在しない満液の状態にて重合した。管状重合器の温度は69.5℃であり、圧力は3.5MPa/Gであった。
製造例1の固体状チタン触媒成分の調製(1)および前重合触媒の製造(2)により得た、前重合触媒(触媒スラリー)を用いて、本重合(3)を以下のようにして行った。
内容量58Lのジャケット付循環式管状重合器にプロピレンを45kg/時間、水素を182NL/時間、(2)で製造した触媒スラリーを固体触媒成分として0.41g/時間、トリエチルアルミニウム2.7ml/時間、ジエチルアミノトリエトキシシラン1.1ml/時間を連続的に供給し、気相の存在しない満液の状態にて重合した。管状重合器の温度は70℃であり、圧力は3.4MPa/Gであった。
・エチレン・α−オレフィン共重合体B−1:α−オレフィン(オクテン)量が38.6重量%であり、MFRが2g/10分であるエチレン・オクテンランダム共重合体、製品名:EG8100、ダウケミカル社製
・エチレン・α−オレフィン共重合体B−2:α−オレフィン(ブテン)量が27.3重量%であり、MFRが2g/10分であるエチレン・ブテンランダム共重合体、製品名:A1070S、三井化学(株)社製
・脂肪酸アミドC−1:エルカ酸アミド、製品名:ニュートロン‐S、日本製化(株)社製
・脂肪酸アミドC−2:オレイン酸アミド、製品名:ニュートロン‐P、日本製化(株)社製
・界面活性剤D−1:グリセロールモノステアレート、製品名:エレクトロストリッパーTS−5、花王(株)社製
・無機充填材E−1:タルク、平均粒径(レーザー回折)5μm、製品名:ハイフィラー5000PJ、浅田製粉(株)社製
[実施例1]
製造例1で得たプロピレン系重合体A−1、エチレン・α−オレフィン共重合体B−1、脂肪酸アミドC−1、界面活性剤D−1の各成分を、表2に示す量(重量部)で用いるとともに、その他の添加剤として、酸化防止剤としてIrganox1010(BASF(株))0.1重量部およびIrgafos168(BASF(株))0.1重量部、耐光剤としてLA−52((株)ADEKA製)0.1重量部、滑剤としてステアリン酸カルシウム((株)日本油脂)0.1重量部、核剤としてアデカスタブNA−11((株)ADEKA製)0.1重量部、および黒色顔料としてMB PPCM 888Y−232((株)東京インキ製)3重量部を用い、これらを順次配合してタンブラーでドライブレンドした。
A〜E成分の各成分および配合量(すなわち、その他の添加剤以外の各成分および配合量。重量部)を、表2または表3に示す通りとしたことのほかは、実施例1と同様にしてポリプロピレン系樹脂組成物ペレットを製造し、射出成形にてテストピースを製造し、ゴム摩擦による傷付き試験(Scuff足蹴り試験)を行った。結果を表2または3に併せて示す。
(2)摩擦物(ゴム試験片)
(3)台座
(4)パンタグラフ
(5)振り子の高さ(20cm)
(6)試験面
Claims (5)
- (A)(a−1)JIS K 7210に準拠した方法で測定したメルトフローレート(MFR、230℃、21.16N荷重)が10g/10min以上300g/10min以下であって、プロピレンから導かれる構成単位の含量が98mol%以上100mol%以下であり、エチレンと炭素原子数4〜8のα−オレフィンから選ばれる少なくとも1種のα−オレフィンから導かれる構成単位の含量が0mol%以上2mol%以下であるプロピレン系重合体30〜80重量部と、
(a−2)135℃デカリン中で測定した極限粘度[η]が1.5dl/g以上8dl/g以下、エチレンから導かれる構成単位の含量が30mol%以上60mol%以下であるプロピレン・エチレン共重合体0〜30重量部と
からなり、(a−1)と(a−2)の合計が30〜80重量部であるポリプロピレン系樹脂と、
(B)エチレン含有率が65mol%以上90mol%以下である、エチレンと、炭素原子数3〜8のα−オレフィンから選ばれる少なくとも1種のα−オレフィンからなるエチレン・α−オレフィン共重合体20〜50重量部と、
(E)無機充填材0〜40重量部と
からなり、(a−2)と(B)との合計が20〜50重量部である基材成分(ただし、(A)、(B)、(E)の合計が100重量部である)100重量部に対して、
(C)オレイン酸アミド、ステアリン酸アミド、エルカ酸アミド、ベヘニン酸アミド、およびエルカ酸アミドの2量体よりなる群から選ばれる脂肪酸アミド0.2〜1重量部、および
(D)界面活性剤0.2〜1重量部
を含み、
前記(D)界面活性剤が、炭素原子数が8〜25であるエステル基を、1つまたは2つ有する化合物である、ポリプロピレン系樹脂組成物。 - 請求項1に記載のポリプロピレン系樹脂組成物からなる成形体。
- 前記成形体が射出成形体である請求項2に記載の成形体。
- 前記成形体が自動車内外装部材である請求項2に記載の成形体。
- 前記自動車内外装部材が、自動車ドア部材またはピラー部材である、請求項4に記載の成形体。
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BR112015005907A2 (pt) | 2017-07-04 |
MX2015003366A (es) | 2015-06-05 |
US20150274948A1 (en) | 2015-10-01 |
WO2014046086A1 (ja) | 2014-03-27 |
CN104640923B (zh) | 2017-08-22 |
US10619039B2 (en) | 2020-04-14 |
JPWO2014046086A1 (ja) | 2016-08-18 |
BR112015005907B1 (pt) | 2021-03-30 |
CN104640923A (zh) | 2015-05-20 |
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