JP6707736B2 - 樹脂組成物、複合材料及び樹脂組成物の製造方法 - Google Patents
樹脂組成物、複合材料及び樹脂組成物の製造方法 Download PDFInfo
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- JP6707736B2 JP6707736B2 JP2015206427A JP2015206427A JP6707736B2 JP 6707736 B2 JP6707736 B2 JP 6707736B2 JP 2015206427 A JP2015206427 A JP 2015206427A JP 2015206427 A JP2015206427 A JP 2015206427A JP 6707736 B2 JP6707736 B2 JP 6707736B2
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- DSLZVSRJTYRBFB-UHFFFAOYSA-N Galactaric acid Natural products OC(=O)C(O)C(O)C(O)C(O)C(O)=O DSLZVSRJTYRBFB-UHFFFAOYSA-N 0.000 description 1
- IAJILQKETJEXLJ-UHFFFAOYSA-N Galacturonsaeure Natural products O=CC(O)C(O)C(O)C(O)C(O)=O IAJILQKETJEXLJ-UHFFFAOYSA-N 0.000 description 1
- AVXURJPOCDRRFD-UHFFFAOYSA-N Hydroxylamine Chemical compound ON AVXURJPOCDRRFD-UHFFFAOYSA-N 0.000 description 1
- HETCEOQFVDFGSY-UHFFFAOYSA-N Isopropenyl acetate Chemical compound CC(=C)OC(C)=O HETCEOQFVDFGSY-UHFFFAOYSA-N 0.000 description 1
- OFOBLEOULBTSOW-UHFFFAOYSA-N Malonic acid Chemical compound OC(=O)CC(O)=O OFOBLEOULBTSOW-UHFFFAOYSA-N 0.000 description 1
- CTQNGGLPUBDAKN-UHFFFAOYSA-N O-Xylene Chemical compound CC1=CC=CC=C1C CTQNGGLPUBDAKN-UHFFFAOYSA-N 0.000 description 1
- CBENFWSGALASAD-UHFFFAOYSA-N Ozone Chemical compound [O-][O+]=O CBENFWSGALASAD-UHFFFAOYSA-N 0.000 description 1
- FQYUMYWMJTYZTK-UHFFFAOYSA-N Phenyl glycidyl ether Chemical compound C1OC1COC1=CC=CC=C1 FQYUMYWMJTYZTK-UHFFFAOYSA-N 0.000 description 1
- 239000004721 Polyphenylene oxide Substances 0.000 description 1
- 239000004372 Polyvinyl alcohol Substances 0.000 description 1
- 229920001328 Polyvinylidene chloride Polymers 0.000 description 1
- AWMVMTVKBNGEAK-UHFFFAOYSA-N Styrene oxide Chemical compound C1OC1C1=CC=CC=C1 AWMVMTVKBNGEAK-UHFFFAOYSA-N 0.000 description 1
- FEWJPZIEWOKRBE-UHFFFAOYSA-N Tartaric acid Natural products [H+].[H+].[O-]C(=O)C(O)C(O)C([O-])=O FEWJPZIEWOKRBE-UHFFFAOYSA-N 0.000 description 1
- 239000004699 Ultra-high molecular weight polyethylene Substances 0.000 description 1
- 239000011954 Ziegler–Natta catalyst Substances 0.000 description 1
- 239000011354 acetal resin Substances 0.000 description 1
- ZOIORXHNWRGPMV-UHFFFAOYSA-N acetic acid;zinc Chemical compound [Zn].CC(O)=O.CC(O)=O ZOIORXHNWRGPMV-UHFFFAOYSA-N 0.000 description 1
- 239000002253 acid Substances 0.000 description 1
- 230000000996 additive effect Effects 0.000 description 1
- 239000000853 adhesive Substances 0.000 description 1
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- 238000005054 agglomeration Methods 0.000 description 1
- 238000004220 aggregation Methods 0.000 description 1
- IAJILQKETJEXLJ-QTBDOELSSA-N aldehydo-D-glucuronic acid Chemical compound O=C[C@H](O)[C@@H](O)[C@H](O)[C@H](O)C(O)=O IAJILQKETJEXLJ-QTBDOELSSA-N 0.000 description 1
- 150000001338 aliphatic hydrocarbons Chemical class 0.000 description 1
- 125000005907 alkyl ester group Chemical group 0.000 description 1
- BJEPYKJPYRNKOW-UHFFFAOYSA-N alpha-hydroxysuccinic acid Natural products OC(=O)C(O)CC(O)=O BJEPYKJPYRNKOW-UHFFFAOYSA-N 0.000 description 1
- 229920005603 alternating copolymer Polymers 0.000 description 1
- 229910052782 aluminium Inorganic materials 0.000 description 1
- XAGFODPZIPBFFR-UHFFFAOYSA-N aluminium Chemical compound [Al] XAGFODPZIPBFFR-UHFFFAOYSA-N 0.000 description 1
- JFCQEDHGNNZCLN-UHFFFAOYSA-N anhydrous glutaric acid Natural products OC(=O)CCCC(O)=O JFCQEDHGNNZCLN-UHFFFAOYSA-N 0.000 description 1
- 150000004945 aromatic hydrocarbons Chemical class 0.000 description 1
- 229910021383 artificial graphite Inorganic materials 0.000 description 1
- 229960005070 ascorbic acid Drugs 0.000 description 1
- 235000010323 ascorbic acid Nutrition 0.000 description 1
- 239000011668 ascorbic acid Substances 0.000 description 1
- WQZGKKKJIJFFOK-VFUOTHLCSA-N beta-D-glucose Chemical compound OC[C@H]1O[C@@H](O)[C@H](O)[C@@H](O)[C@@H]1O WQZGKKKJIJFFOK-VFUOTHLCSA-N 0.000 description 1
- 239000011230 binding agent Substances 0.000 description 1
- 230000005540 biological transmission Effects 0.000 description 1
- 230000015572 biosynthetic process Effects 0.000 description 1
- 229920001400 block copolymer Polymers 0.000 description 1
- IAQRGUVFOMOMEM-UHFFFAOYSA-N butene Natural products CC=CC IAQRGUVFOMOMEM-UHFFFAOYSA-N 0.000 description 1
- 229940065285 cadmium compound Drugs 0.000 description 1
- 150000001662 cadmium compounds Chemical class 0.000 description 1
- AQCDIIAORKRFCD-UHFFFAOYSA-N cadmium selenide Chemical compound [Cd]=[Se] AQCDIIAORKRFCD-UHFFFAOYSA-N 0.000 description 1
- 239000006229 carbon black Substances 0.000 description 1
- 239000004917 carbon fiber Substances 0.000 description 1
- 229910021393 carbon nanotube Inorganic materials 0.000 description 1
- 239000002041 carbon nanotube Substances 0.000 description 1
- 150000001732 carboxylic acid derivatives Chemical class 0.000 description 1
- 239000012461 cellulose resin Substances 0.000 description 1
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 description 1
- 238000004891 communication Methods 0.000 description 1
- 239000002361 compost Substances 0.000 description 1
- 238000013329 compounding Methods 0.000 description 1
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- 150000005676 cyclic carbonates Chemical class 0.000 description 1
- ZWAJLVLEBYIOTI-UHFFFAOYSA-N cyclohexene oxide Chemical compound C1CCCC2OC21 ZWAJLVLEBYIOTI-UHFFFAOYSA-N 0.000 description 1
- FWFSEYBSWVRWGL-UHFFFAOYSA-N cyclohexene oxide Natural products O=C1CCCC=C1 FWFSEYBSWVRWGL-UHFFFAOYSA-N 0.000 description 1
- 230000018044 dehydration Effects 0.000 description 1
- 238000006297 dehydration reaction Methods 0.000 description 1
- 230000006866 deterioration Effects 0.000 description 1
- 150000004985 diamines Chemical class 0.000 description 1
- 229910003460 diamond Inorganic materials 0.000 description 1
- 239000010432 diamond Substances 0.000 description 1
- AXAZMDOAUQTMOW-UHFFFAOYSA-N dimethylzinc Chemical compound C[Zn]C AXAZMDOAUQTMOW-UHFFFAOYSA-N 0.000 description 1
- 229910001873 dinitrogen Inorganic materials 0.000 description 1
- MKRVHLWAVKJBFN-UHFFFAOYSA-N diphenylzinc Chemical compound C=1C=CC=CC=1[Zn]C1=CC=CC=C1 MKRVHLWAVKJBFN-UHFFFAOYSA-N 0.000 description 1
- 238000001035 drying Methods 0.000 description 1
- 239000003759 ester based solvent Substances 0.000 description 1
- MEGHWIAOTJPCHQ-UHFFFAOYSA-N ethenyl butanoate Chemical compound CCCC(=O)OC=C MEGHWIAOTJPCHQ-UHFFFAOYSA-N 0.000 description 1
- UIWXSTHGICQLQT-UHFFFAOYSA-N ethenyl propanoate Chemical compound CCC(=O)OC=C UIWXSTHGICQLQT-UHFFFAOYSA-N 0.000 description 1
- 239000004210 ether based solvent Substances 0.000 description 1
- SUPCQIBBMFXVTL-UHFFFAOYSA-N ethyl 2-methylprop-2-enoate Chemical compound CCOC(=O)C(C)=C SUPCQIBBMFXVTL-UHFFFAOYSA-N 0.000 description 1
- 229960003750 ethyl chloride Drugs 0.000 description 1
- 239000005038 ethylene vinyl acetate Substances 0.000 description 1
- 229920006225 ethylene-methyl acrylate Polymers 0.000 description 1
- 229920005680 ethylene-methyl methacrylate copolymer Polymers 0.000 description 1
- OGPBJKLSAFTDLK-UHFFFAOYSA-N europium atom Chemical compound [Eu] OGPBJKLSAFTDLK-UHFFFAOYSA-N 0.000 description 1
- 238000011156 evaluation Methods 0.000 description 1
- 230000001747 exhibiting effect Effects 0.000 description 1
- 230000002349 favourable effect Effects 0.000 description 1
- 239000000835 fiber Substances 0.000 description 1
- 239000000706 filtrate Substances 0.000 description 1
- 239000012530 fluid Substances 0.000 description 1
- 239000006260 foam Substances 0.000 description 1
- 229910003472 fullerene Inorganic materials 0.000 description 1
- 235000004515 gallic acid Nutrition 0.000 description 1
- 229940074391 gallic acid Drugs 0.000 description 1
- 239000000174 gluconic acid Substances 0.000 description 1
- 235000012208 gluconic acid Nutrition 0.000 description 1
- 229950006191 gluconic acid Drugs 0.000 description 1
- 229940097043 glucuronic acid Drugs 0.000 description 1
- 238000009499 grossing Methods 0.000 description 1
- 229940093915 gynecological organic acid Drugs 0.000 description 1
- 150000008282 halocarbons Chemical class 0.000 description 1
- FUZZWVXGSFPDMH-UHFFFAOYSA-N hexanoic acid Chemical compound CCCCCC(O)=O FUZZWVXGSFPDMH-UHFFFAOYSA-N 0.000 description 1
- 229920001903 high density polyethylene Polymers 0.000 description 1
- 239000004700 high-density polyethylene Substances 0.000 description 1
- 239000003999 initiator Substances 0.000 description 1
- 238000009413 insulation Methods 0.000 description 1
- 230000001788 irregular Effects 0.000 description 1
- QTBFPMKWQKYFLR-UHFFFAOYSA-N isobutyl chloride Chemical compound CC(C)CCl QTBFPMKWQKYFLR-UHFFFAOYSA-N 0.000 description 1
- ULYZAYCEDJDHCC-UHFFFAOYSA-N isopropyl chloride Chemical compound CC(C)Cl ULYZAYCEDJDHCC-UHFFFAOYSA-N 0.000 description 1
- 239000005453 ketone based solvent Substances 0.000 description 1
- 229920000092 linear low density polyethylene Polymers 0.000 description 1
- 239000004707 linear low-density polyethylene Substances 0.000 description 1
- 229920001684 low density polyethylene Polymers 0.000 description 1
- 239000004702 low-density polyethylene Substances 0.000 description 1
- 239000001630 malic acid Substances 0.000 description 1
- 235000011090 malic acid Nutrition 0.000 description 1
- 229920001179 medium density polyethylene Polymers 0.000 description 1
- 239000004701 medium-density polyethylene Substances 0.000 description 1
- 239000000155 melt Substances 0.000 description 1
- 239000012968 metallocene catalyst Substances 0.000 description 1
- 150000002739 metals Chemical class 0.000 description 1
- 125000002496 methyl group Chemical group [H]C([H])([H])* 0.000 description 1
- 239000000178 monomer Substances 0.000 description 1
- DILRJUIACXKSQE-UHFFFAOYSA-N n',n'-dimethylethane-1,2-diamine Chemical compound CN(C)CCN DILRJUIACXKSQE-UHFFFAOYSA-N 0.000 description 1
- GMEPFKKLXPMOGZ-UHFFFAOYSA-N n,n-bis(methylsulfonyl)formamide Chemical compound CS(=O)(=O)N(C=O)S(C)(=O)=O GMEPFKKLXPMOGZ-UHFFFAOYSA-N 0.000 description 1
- SNMVRZFUUCLYTO-UHFFFAOYSA-N n-propyl chloride Chemical compound CCCCl SNMVRZFUUCLYTO-UHFFFAOYSA-N 0.000 description 1
- 239000002086 nanomaterial Substances 0.000 description 1
- 239000002105 nanoparticle Substances 0.000 description 1
- 229910021382 natural graphite Inorganic materials 0.000 description 1
- 239000012299 nitrogen atmosphere Substances 0.000 description 1
- TVMXDCGIABBOFY-UHFFFAOYSA-N octane Chemical compound CCCCCCCC TVMXDCGIABBOFY-UHFFFAOYSA-N 0.000 description 1
- 150000007524 organic acids Chemical class 0.000 description 1
- 235000005985 organic acids Nutrition 0.000 description 1
- 238000012856 packing Methods 0.000 description 1
- 239000008188 pellet Substances 0.000 description 1
- HVAMZGADVCBITI-UHFFFAOYSA-M pent-4-enoate Chemical compound [O-]C(=O)CCC=C HVAMZGADVCBITI-UHFFFAOYSA-M 0.000 description 1
- YWAKXRMUMFPDSH-UHFFFAOYSA-N pentene Chemical compound CCCC=C YWAKXRMUMFPDSH-UHFFFAOYSA-N 0.000 description 1
- PNJWIWWMYCMZRO-UHFFFAOYSA-N pent‐4‐en‐2‐one Natural products CC(=O)CC=C PNJWIWWMYCMZRO-UHFFFAOYSA-N 0.000 description 1
- 150000002978 peroxides Chemical class 0.000 description 1
- 150000002989 phenols Chemical class 0.000 description 1
- 239000011990 phillips catalyst Substances 0.000 description 1
- 230000000704 physical effect Effects 0.000 description 1
- 238000009832 plasma treatment Methods 0.000 description 1
- 229920003023 plastic Polymers 0.000 description 1
- 239000004033 plastic Substances 0.000 description 1
- 229920001200 poly(ethylene-vinyl acetate) Polymers 0.000 description 1
- 229920006122 polyamide resin Polymers 0.000 description 1
- 229920000768 polyamine Polymers 0.000 description 1
- 229920001083 polybutene Polymers 0.000 description 1
- 229920000515 polycarbonate Polymers 0.000 description 1
- 239000004417 polycarbonate Substances 0.000 description 1
- 229920001225 polyester resin Polymers 0.000 description 1
- 239000004645 polyester resin Substances 0.000 description 1
- 229920000570 polyether Polymers 0.000 description 1
- 229920001721 polyimide Polymers 0.000 description 1
- 239000009719 polyimide resin Substances 0.000 description 1
- 239000011116 polymethylpentene Substances 0.000 description 1
- 229920000306 polymethylpentene Polymers 0.000 description 1
- 229920000098 polyolefin Polymers 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920005990 polystyrene resin Polymers 0.000 description 1
- 229920003225 polyurethane elastomer Polymers 0.000 description 1
- 229920002451 polyvinyl alcohol Polymers 0.000 description 1
- 229920000915 polyvinyl chloride Polymers 0.000 description 1
- 239000004800 polyvinyl chloride Substances 0.000 description 1
- 239000005033 polyvinylidene chloride Substances 0.000 description 1
- 239000000843 powder Substances 0.000 description 1
- 239000002244 precipitate Substances 0.000 description 1
- 150000003141 primary amines Chemical class 0.000 description 1
- 239000011164 primary particle Substances 0.000 description 1
- 230000008569 process Effects 0.000 description 1
- NHARPDSAXCBDDR-UHFFFAOYSA-N propyl 2-methylprop-2-enoate Chemical compound CCCOC(=O)C(C)=C NHARPDSAXCBDDR-UHFFFAOYSA-N 0.000 description 1
- PNXMTCDJUBJHQJ-UHFFFAOYSA-N propyl prop-2-enoate Chemical compound CCCOC(=O)C=C PNXMTCDJUBJHQJ-UHFFFAOYSA-N 0.000 description 1
- RUOJZAUFBMNUDX-UHFFFAOYSA-N propylene carbonate Chemical compound CC1COC(=O)O1 RUOJZAUFBMNUDX-UHFFFAOYSA-N 0.000 description 1
- 238000000197 pyrolysis Methods 0.000 description 1
- 229920005604 random copolymer Polymers 0.000 description 1
- 230000035484 reaction time Effects 0.000 description 1
- 230000009257 reactivity Effects 0.000 description 1
- 230000009467 reduction Effects 0.000 description 1
- 238000007670 refining Methods 0.000 description 1
- 238000010992 reflux Methods 0.000 description 1
- 238000007151 ring opening polymerisation reaction Methods 0.000 description 1
- 239000007787 solid Substances 0.000 description 1
- 239000004071 soot Substances 0.000 description 1
- 230000001502 supplementing effect Effects 0.000 description 1
- 238000004381 surface treatment Methods 0.000 description 1
- 230000002194 synthesizing effect Effects 0.000 description 1
- 235000002906 tartaric acid Nutrition 0.000 description 1
- 239000011975 tartaric acid Substances 0.000 description 1
- VZGDMQKNWNREIO-UHFFFAOYSA-N tetrachloromethane Chemical compound ClC(Cl)(Cl)Cl VZGDMQKNWNREIO-UHFFFAOYSA-N 0.000 description 1
- AACMXYCXYZGNBT-UHFFFAOYSA-N trimethyl(oxiran-2-ylmethoxy)silane Chemical compound C[Si](C)(C)OCC1CO1 AACMXYCXYZGNBT-UHFFFAOYSA-N 0.000 description 1
- 229920000785 ultra high molecular weight polyethylene Polymers 0.000 description 1
- 238000007666 vacuum forming Methods 0.000 description 1
- 229920001567 vinyl ester resin Polymers 0.000 description 1
- 238000005406 washing Methods 0.000 description 1
- 239000008096 xylene Substances 0.000 description 1
- 239000004246 zinc acetate Substances 0.000 description 1
- 239000011787 zinc oxide Substances 0.000 description 1
- HEPBQSXQJMTVFI-UHFFFAOYSA-N zinc;butane Chemical compound [Zn+2].CCC[CH2-].CCC[CH2-] HEPBQSXQJMTVFI-UHFFFAOYSA-N 0.000 description 1
Landscapes
- Compositions Of Macromolecular Compounds (AREA)
- Carbon And Carbon Compounds (AREA)
Description
項1.脂肪族ポリカーボネート樹脂とカーボン材料とを含む樹脂組成物。
項2.前記カーボン材料が発光性ナノカーボンを含む、上記項1に記載の樹脂組成物。
項3.前記発光性ナノカーボンの発光スペクトルの発光強度が最大となる発光波長が、波長320〜460nmの励起光を用いた場合に、400〜525nmの範囲内である、上記項1又は2に記載の樹脂組成物。
項4.前記脂肪族ポリカーボネート樹脂が、アルキレンオキシドと二酸化炭素との共重合体を含む、上記項1〜3のいずれか1項に記載の樹脂組成物。
項5.上記項1〜4のいずれか1項に記載の樹脂組成物が基材樹脂中に含まれてなる、複合材料。
項6.前記基材樹脂が熱可塑性樹脂を含む、上記項5に記載の複合材料。
項7.前記熱可塑性樹脂がポリオレフィン系樹脂を含む、上記項6に記載の複合材料。
項8.前記ポリオレフィン系樹脂がポリプロピレンを含む、上記項7に記載の複合材料。
項9.上記項1〜4のいずれか1項に記載の樹脂組成物の製造方法であって、
炭素源化合物および窒素源化合物を含有する原料水溶液を加熱することにより前記カーボン材料を得るステップ、
アルキレンオキシドと二酸化炭素とを重合反応することにより前記脂肪族ポリカーボネート樹脂を製造するステップ、及び、
前記各々のステップで得られたカーボン材料と前記脂肪族ポリカーボネート樹脂とを混合して前記樹脂組成物を得るステップを具備する、樹脂組成物の製造方法。
脂肪族ポリカーボネート樹脂の種類は特に限定的ではなく、例えば、ポリアルキレンカーボネート樹脂が挙げられる。
(昭和電工株式会社の商品名、Shodex OHPac SB−800シリーズ)
カラム温度:40℃
溶出液:0.03mol/L 臭化リチウム‐N,N−ジメチルホルムアミド溶液
流速:0.65mL/min
樹脂組成物に含まれる脂肪族ポリカーボネート樹脂は、1種類のみであってもよいし、あるいは、2種以上が含まれていてもよい。例えば、樹脂組成物に含まれる脂肪族ポリカーボネート樹脂は、ポリアルキレンカーボネート樹脂のみであってもよいし、あるいは、これと他の脂肪族ポリカーボネート樹脂の混合物であってもよい。
カーボン材料は、少なくとも炭素を含有して構成される。カーボン材料としては、樹脂のフィラーとして使用した場合に、発光性、機械的強度、電気的特性、導電性、光吸収性、電磁波吸収性等の性能を付与できる性質を有していることが好ましい。
アルキレンオキシドと二酸化炭素とを重合反応することにより前記脂肪族ポリカーボネート樹脂を製造するステップB、及び、
前記各々のステップで得られたカーボン材料と前記脂肪族ポリカーボネート樹脂とを混合して前記樹脂組成物を得るステップC。
本実施形態の複合材料は、上述した脂肪族ポリカーボネート樹脂とカーボン材料とを含む樹脂組成物が基材樹脂中に含まれてなる。特に、複合材料にあっては、樹脂組成物を構成する脂肪族ポリカーボネート樹脂が基材樹脂中に分散した状態で存在していることが好ましい。この場合、特にカーボン材料の機能が発現しやすくなる。脂肪族ポリカーボネート樹脂が基材樹脂中に分散して存在するとは、脂肪族ポリカーボネート樹脂のドメインが基材樹脂中において偏在、すなわち、一部分のみに凝集した状態で存在しているのではなく、基材樹脂全体にわたってドメインが分布している状態をいう。
カラム:GPCカラム
(東ソー株式会社の商品名、TSKgel GMHHR−H HT)
カラム温度:140℃
溶出液:1,2−ジクロロベンゼン
流速:1mL/min
とできる。
本実施形態に係る複合材料は、樹脂組成物の脂肪族ポリカーボネート樹脂が基材樹脂に分散した状態で存在し得るので、結果として、脂肪族ポリカーボネート樹脂に分散しているカーボン材料も基材樹脂に分散して存在する。そのため、当該複合材料は、カーボン材料による機能が発現されやすく、優れた性能を有し得る。
攪拌機、窒素ガス導入管、温度計、ディーンスターク管、還流冷却管を備えた0.3L容の四つ口フラスコに、酸化亜鉛7.73g(95mmol)、グルタル酸12.3g(100mmol)、酢酸0.114g(2mmol)およびトルエン76.0gを仕込んだ。次に、反応系内に50mL/minの流量で窒素を流しながら、55℃まで昇温し、同温度で4時間攪拌して反応させた。その後、110℃まで昇温し、さらに同温度で2時間攪拌して共沸脱水させ水分を除去した後、室温まで冷却して、有機亜鉛触媒を含むスラリー液を得た。
攪拌機、ガス導入管、温度計を備えた1L容のオートクレーブの系内をあらかじめ窒素雰囲気に置換した後、製造例1により得られた有機亜鉛触媒を含むスラリー液39.1g(有機亜鉛触媒を45mmol含む)、炭酸ジメチル192.4g、プロピレンオキシド26.1g(450mmol)を仕込んだ。次に、攪拌下、二酸化炭素を加え、反応系内が1.0MPaとなるまで二酸化炭素を充填した。その後、60℃に昇温し、反応により消費される二酸化炭素を補給しながら10時間重合反応を行なった。反応終了後、オートクレーブを冷却して脱圧し、ろ過した後、減圧乾燥してポリプロピレンカーボネート樹脂40gを得た。得られたポリプロピレンカーボネート樹脂の質量平均分子量は、330,000(Mw/Mn=10.02)であった。
カラム:GPCカラム
(昭和電工株式会社の商品名、Shodex OHPac SB−800シリーズ)
カラム温度:40℃
溶出液:0.03mol/L 臭化リチウム‐N,N−ジメチルホルムアミド溶液
流速:0.65mL/min
とした。
0.5mol/Lのクエン酸水溶液10gにエチレンジアミン0.34gを混合し、マイクロ波(700W家庭用電子レンジを使用)により3.5分加熱し、熱分解させた。加熱後に得られた固体を少量の水で溶解し、過剰量のエタノール中に注いだ。これにより生じた沈殿物をろ過により除去し、ろ液を減圧留去して発光性ナノカーボンを0.43g、収率32%で得た。
製造例2で得られたポリプロピレンカーボネート樹脂100質量部を熱ジメチルホルムアミドに溶解させた。そこに製造例3で得られた発光性ナノカーボンの水分散液(発光性ナノカーボン含有量20質量%)12質量部を添加して攪拌した。得られた混合溶液をシャーレに展開し、真空オーブン1000Paの減圧下、40℃雰囲気で18時間乾燥させることにより、炭素材料として発光性ナノカーボンを含む樹脂組成物のフィルムを得た。発光性ナノカーボンは、ポリプロピレンカーボネート樹脂100質量部に対し2.4質量部含有されていた。
実施例1で得られた発光性ナノカーボンを含む樹脂組成物3質量部と、予め光安定剤を除去したイソタクチックポリプロピレン(日本ポリプロ株式会社製、Mw=380,000、Mw/Mn=4.9)97質量部をDSM Xplore社製マイクロコンパウンダーに投入し、180℃、回転数50rpmで5分間混練を行うことで、複合材料を得た。
発光性ナノカーボンを含む樹脂組成物を使用せず、ポリプロピレンのみを用いて実施例2と同様の条件で加工し、厚さ0.1mmのシート状成形体を得た。
発光性ナノカーボンを含む樹脂組成物の代わりに、製造例2で得られたポリプロピレンカーボネート樹脂3質量部に変更したこと以外は、実施例2と同様の条件で加工し、厚さ0.1mmのシート状成形体を得た。
実施例2で使用したポリプロピレンに製造例3で得られた発光性ナノカーボンを混合させたが、両者は均一に混ざらなかった。
実施例および比較例で得られた樹脂組成物のシートについて、吸収スペクトル、一軸引張試験及び暴露試験を、以下の方法により行った。
実施例1で得られた発光性ナノカーボンを含む樹脂組成物から形成したフィルムについて、以下の測定装置を用いて、吸収スペクトルを測定した。
測定装置:日本分光株式会社製「紫外可視分光光度計V−550」
測定波長:190nm〜900nm
JIS K 7161:1994に準拠し、以下の試験片および測定装置を用いて、降伏応力、ネック応力、ネックひずみ、破断応力、破断ひずみおよび弾性率を測定した。また、レジリエンスは応力−ひずみ曲線における、ネックひずみまでの積分値から算出した。降伏応力、ネック応力が大きいほど、強度に優れた硬い材料である。破断応力、破断ひずみが大きいほど、延伸性に優れ、粘り強い材料である。ネックひずみ、レジリエンスが大きいほど靭性に優れた材料である。弾性率が大きいほど、変形しにくい材料である。
試験片:ダンベル型(平行部長さ10mm、平行部幅4mm、厚み0.2mm)
測定機:INSTRON社製引張試験機 MODEL4466
引張速度:20mm/min
測定温度:25℃
JIS K 7350:2008に準拠し、以下の測定装置を用いて測定した。
測定機:東洋精機製作所製「卓上キセノン耐光性試験機 SUNTEST cps plus」
光源:キセノンランプ
照度:550W/cm2
ブラックパネル温度:63℃
照射時間:24時間
Claims (8)
- 脂肪族ポリカーボネート樹脂とカーボン材料とを含み、
前記カーボン材料がカーボンドットを含む発光性ナノカーボンである、樹脂組成物。 - 前記発光性ナノカーボンの発光スペクトルの発光強度が最大となる発光波長が、波長320〜460nmの励起光を用いた場合に、400〜525nmの範囲内である、請求項1に記載の樹脂組成物。
- 前記脂肪族ポリカーボネート樹脂が、アルキレンオキシドと二酸化炭素との共重合体を含む、請求項1又は2に記載の樹脂組成物。
- 請求項1〜3のいずれか1項に記載の樹脂組成物が基材樹脂中に含まれてなる、複合材料。
- 前記基材樹脂が熱可塑性樹脂を含む、請求項4に記載の複合材料。
- 前記熱可塑性樹脂がポリオレフィン系樹脂を含む、請求項5に記載の複合材料。
- 前記ポリオレフィン系樹脂がポリプロピレンを含む、請求項6に記載の複合材料。
- 請求項1〜3のいずれか1項に記載の樹脂組成物の製造方法であって、
炭素源化合物および窒素源化合物を含有する原料水溶液を加熱することにより前記カーボン材料を得るステップ、
アルキレンオキシドと二酸化炭素とを重合反応することにより前記脂肪族ポリカーボネート樹脂を製造するステップ、及び、
前記各々のステップで得られたカーボン材料と前記脂肪族ポリカーボネート樹脂とを混合して前記樹脂組成物を得るステップを具備する、樹脂組成物の製造方法。
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