JPWO2015072514A1 - スチレン系樹脂押出発泡体及びその製造方法 - Google Patents
スチレン系樹脂押出発泡体及びその製造方法 Download PDFInfo
- Publication number
- JPWO2015072514A1 JPWO2015072514A1 JP2015547786A JP2015547786A JPWO2015072514A1 JP WO2015072514 A1 JPWO2015072514 A1 JP WO2015072514A1 JP 2015547786 A JP2015547786 A JP 2015547786A JP 2015547786 A JP2015547786 A JP 2015547786A JP WO2015072514 A1 JPWO2015072514 A1 JP WO2015072514A1
- Authority
- JP
- Japan
- Prior art keywords
- styrene
- flame retardant
- extruded foam
- styrene resin
- resin extruded
- 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.)
- Granted
Links
- 239000006260 foam Substances 0.000 title claims abstract description 151
- 238000004519 manufacturing process Methods 0.000 title claims description 15
- 229920001890 Novodur Polymers 0.000 title abstract description 17
- PPBRXRYQALVLMV-UHFFFAOYSA-N Styrene Chemical compound C=CC1=CC=CC=C1 PPBRXRYQALVLMV-UHFFFAOYSA-N 0.000 claims abstract description 285
- 229920005989 resin Polymers 0.000 claims abstract description 149
- 239000011347 resin Substances 0.000 claims abstract description 149
- RNFJDJUURJAICM-UHFFFAOYSA-N 2,2,4,4,6,6-hexaphenoxy-1,3,5-triaza-2$l^{5},4$l^{5},6$l^{5}-triphosphacyclohexa-1,3,5-triene Chemical compound N=1P(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP(OC=2C=CC=CC=2)(OC=2C=CC=CC=2)=NP=1(OC=1C=CC=CC=1)OC1=CC=CC=C1 RNFJDJUURJAICM-UHFFFAOYSA-N 0.000 claims abstract description 139
- 239000003063 flame retardant Substances 0.000 claims abstract description 132
- 239000000203 mixture Substances 0.000 claims abstract description 80
- 239000003381 stabilizer Substances 0.000 claims abstract description 58
- 229920000642 polymer Polymers 0.000 claims abstract description 36
- MTAZNLWOLGHBHU-UHFFFAOYSA-N butadiene-styrene rubber Chemical class C=CC=C.C=CC1=CC=CC=C1 MTAZNLWOLGHBHU-UHFFFAOYSA-N 0.000 claims abstract description 34
- 239000004088 foaming agent Substances 0.000 claims abstract description 34
- 238000001125 extrusion Methods 0.000 claims abstract description 27
- 238000005187 foaming Methods 0.000 claims abstract description 12
- ISWSIDIOOBJBQZ-UHFFFAOYSA-N Phenol Chemical compound OC1=CC=CC=C1 ISWSIDIOOBJBQZ-UHFFFAOYSA-N 0.000 claims description 21
- LCGLNKUTAGEVQW-UHFFFAOYSA-N Dimethyl ether Chemical compound COC LCGLNKUTAGEVQW-UHFFFAOYSA-N 0.000 claims description 16
- 239000004593 Epoxy Substances 0.000 claims description 16
- 150000001875 compounds Chemical class 0.000 claims description 13
- 150000005846 sugar alcohols Polymers 0.000 claims description 13
- IJGRMHOSHXDMSA-UHFFFAOYSA-N Atomic nitrogen Chemical compound N#N IJGRMHOSHXDMSA-UHFFFAOYSA-N 0.000 claims description 12
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- 230000036961 partial effect Effects 0.000 claims description 12
- XLYOFNOQVPJJNP-UHFFFAOYSA-N water Substances O XLYOFNOQVPJJNP-UHFFFAOYSA-N 0.000 claims description 11
- 229910001868 water Inorganic materials 0.000 claims description 11
- CURLTUGMZLYLDI-UHFFFAOYSA-N Carbon dioxide Chemical compound O=C=O CURLTUGMZLYLDI-UHFFFAOYSA-N 0.000 claims description 10
- 125000004432 carbon atom Chemical group C* 0.000 claims description 10
- OJMIONKXNSYLSR-UHFFFAOYSA-N phosphorous acid Chemical compound OP(O)O OJMIONKXNSYLSR-UHFFFAOYSA-N 0.000 claims description 9
- 229930195734 saturated hydrocarbon Natural products 0.000 claims description 8
- 150000001412 amines Chemical class 0.000 claims description 6
- 238000002485 combustion reaction Methods 0.000 claims description 6
- 229910052757 nitrogen Inorganic materials 0.000 claims description 6
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- 150000001298 alcohols Chemical class 0.000 claims description 5
- QVGXLLKOCUKJST-UHFFFAOYSA-N atomic oxygen Chemical compound [O] QVGXLLKOCUKJST-UHFFFAOYSA-N 0.000 claims description 5
- 239000001569 carbon dioxide Substances 0.000 claims description 5
- 229910002092 carbon dioxide Inorganic materials 0.000 claims description 5
- HRYZWHHZPQKTII-UHFFFAOYSA-N chloroethane Chemical compound CCCl HRYZWHHZPQKTII-UHFFFAOYSA-N 0.000 claims description 5
- 229960003750 ethyl chloride Drugs 0.000 claims description 5
- AUONHKJOIZSQGR-UHFFFAOYSA-N oxophosphane Chemical compound P=O AUONHKJOIZSQGR-UHFFFAOYSA-N 0.000 claims description 5
- 239000001301 oxygen Substances 0.000 claims description 5
- 229910052760 oxygen Inorganic materials 0.000 claims description 5
- HGTUJZTUQFXBIH-UHFFFAOYSA-N (2,3-dimethyl-3-phenylbutan-2-yl)benzene Chemical compound C=1C=CC=CC=1C(C)(C)C(C)(C)C1=CC=CC=C1 HGTUJZTUQFXBIH-UHFFFAOYSA-N 0.000 claims description 4
- NEHMKBQYUWJMIP-NJFSPNSNSA-N chloro(114C)methane Chemical compound [14CH3]Cl NEHMKBQYUWJMIP-NJFSPNSNSA-N 0.000 claims description 4
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- XZZNDPSIHUTMOC-UHFFFAOYSA-N triphenyl phosphate Chemical compound C=1C=CC=CC=1OP(OC=1C=CC=CC=1)(=O)OC1=CC=CC=C1 XZZNDPSIHUTMOC-UHFFFAOYSA-N 0.000 claims description 4
- FIQMHBFVRAXMOP-UHFFFAOYSA-N triphenylphosphane oxide Chemical group C=1C=CC=CC=1P(C=1C=CC=CC=1)(=O)C1=CC=CC=C1 FIQMHBFVRAXMOP-UHFFFAOYSA-N 0.000 claims description 4
- 238000010998 test method Methods 0.000 claims description 3
- BHYQWBKCXBXPKM-UHFFFAOYSA-N tris[3-bromo-2,2-bis(bromomethyl)propyl] phosphate Chemical compound BrCC(CBr)(CBr)COP(=O)(OCC(CBr)(CBr)CBr)OCC(CBr)(CBr)CBr BHYQWBKCXBXPKM-UHFFFAOYSA-N 0.000 claims description 3
- 229940077445 dimethyl ether Drugs 0.000 claims description 2
- MPQXHAGKBWFSNV-UHFFFAOYSA-N oxidophosphanium Chemical class [PH3]=O MPQXHAGKBWFSNV-UHFFFAOYSA-N 0.000 claims description 2
- NNPPMTNAJDCUHE-UHFFFAOYSA-N isobutane Chemical compound CC(C)C NNPPMTNAJDCUHE-UHFFFAOYSA-N 0.000 description 16
- -1 alkyl phosphite Chemical compound 0.000 description 13
- 229920001577 copolymer Polymers 0.000 description 12
- 239000004793 Polystyrene Substances 0.000 description 11
- VYPSYNLAJGMNEJ-UHFFFAOYSA-N Silicium dioxide Chemical compound O=[Si]=O VYPSYNLAJGMNEJ-UHFFFAOYSA-N 0.000 description 11
- 238000004898 kneading Methods 0.000 description 11
- 239000000047 product Substances 0.000 description 11
- 239000000126 substance Substances 0.000 description 11
- DEIGXXQKDWULML-UHFFFAOYSA-N 1,2,5,6,9,10-hexabromocyclododecane Chemical compound BrC1CCC(Br)C(Br)CCC(Br)C(Br)CCC1Br DEIGXXQKDWULML-UHFFFAOYSA-N 0.000 description 10
- 230000000694 effects Effects 0.000 description 10
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- KAKZBPTYRLMSJV-UHFFFAOYSA-N Butadiene Chemical compound C=CC=C KAKZBPTYRLMSJV-UHFFFAOYSA-N 0.000 description 9
- 229910019142 PO4 Inorganic materials 0.000 description 9
- 239000010452 phosphate Substances 0.000 description 9
- 239000000654 additive Substances 0.000 description 7
- 238000011038 discontinuous diafiltration by volume reduction Methods 0.000 description 7
- 238000002156 mixing Methods 0.000 description 7
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- 238000000465 moulding Methods 0.000 description 7
- 230000005855 radiation Effects 0.000 description 7
- 150000003254 radicals Chemical class 0.000 description 7
- OKTJSMMVPCPJKN-UHFFFAOYSA-N Carbon Chemical compound [C] OKTJSMMVPCPJKN-UHFFFAOYSA-N 0.000 description 6
- RTZKZFJDLAIYFH-UHFFFAOYSA-N Diethyl ether Chemical compound CCOCC RTZKZFJDLAIYFH-UHFFFAOYSA-N 0.000 description 6
- 230000000052 comparative effect Effects 0.000 description 6
- 238000000354 decomposition reaction Methods 0.000 description 6
- 238000002844 melting Methods 0.000 description 6
- 229920001519 homopolymer Polymers 0.000 description 5
- 230000008018 melting Effects 0.000 description 5
- 238000012545 processing Methods 0.000 description 5
- 239000004604 Blowing Agent Substances 0.000 description 4
- BAPJBEWLBFYGME-UHFFFAOYSA-N Methyl acrylate Chemical compound COC(=O)C=C BAPJBEWLBFYGME-UHFFFAOYSA-N 0.000 description 4
- ATUOYWHBWRKTHZ-UHFFFAOYSA-N Propane Chemical compound CCC ATUOYWHBWRKTHZ-UHFFFAOYSA-N 0.000 description 4
- WNLRTRBMVRJNCN-UHFFFAOYSA-N adipic acid Chemical compound OC(=O)CCCCC(O)=O WNLRTRBMVRJNCN-UHFFFAOYSA-N 0.000 description 4
- 238000005452 bending Methods 0.000 description 4
- 210000004027 cell Anatomy 0.000 description 4
- 230000006866 deterioration Effects 0.000 description 4
- 239000003822 epoxy resin Substances 0.000 description 4
- 238000010438 heat treatment Methods 0.000 description 4
- 239000003112 inhibitor Substances 0.000 description 4
- 239000000463 material Substances 0.000 description 4
- 239000000155 melt Substances 0.000 description 4
- IJDNQMDRQITEOD-UHFFFAOYSA-N n-butane Chemical compound CCCC IJDNQMDRQITEOD-UHFFFAOYSA-N 0.000 description 4
- 229920000647 polyepoxide Polymers 0.000 description 4
- 230000000087 stabilizing effect Effects 0.000 description 4
- 229920003048 styrene butadiene rubber Polymers 0.000 description 4
- RSJKGSCJYJTIGS-UHFFFAOYSA-N undecane Chemical compound CCCCCCCCCCC RSJKGSCJYJTIGS-UHFFFAOYSA-N 0.000 description 4
- ZWEHNKRNPOVVGH-UHFFFAOYSA-N 2-Butanone Chemical compound CCC(C)=O ZWEHNKRNPOVVGH-UHFFFAOYSA-N 0.000 description 3
- QTBSBXVTEAMEQO-UHFFFAOYSA-N Acetic acid Chemical compound CC(O)=O QTBSBXVTEAMEQO-UHFFFAOYSA-N 0.000 description 3
- WKBOTKDWSSQWDR-UHFFFAOYSA-N Bromine atom Chemical compound [Br] WKBOTKDWSSQWDR-UHFFFAOYSA-N 0.000 description 3
- 241000579895 Chlorostilbon Species 0.000 description 3
- LFQSCWFLJHTTHZ-UHFFFAOYSA-N Ethanol Chemical compound CCO LFQSCWFLJHTTHZ-UHFFFAOYSA-N 0.000 description 3
- YLQBMQCUIZJEEH-UHFFFAOYSA-N Furan Chemical compound C=1C=COC=1 YLQBMQCUIZJEEH-UHFFFAOYSA-N 0.000 description 3
- CERQOIWHTDAKMF-UHFFFAOYSA-N Methacrylic acid Chemical compound CC(=C)C(O)=O CERQOIWHTDAKMF-UHFFFAOYSA-N 0.000 description 3
- OKKJLVBELUTLKV-UHFFFAOYSA-N Methanol Chemical compound OC OKKJLVBELUTLKV-UHFFFAOYSA-N 0.000 description 3
- OFBQJSOFQDEBGM-UHFFFAOYSA-N Pentane Chemical compound CCCCC OFBQJSOFQDEBGM-UHFFFAOYSA-N 0.000 description 3
- OAICVXFJPJFONN-UHFFFAOYSA-N Phosphorus Chemical compound [P] OAICVXFJPJFONN-UHFFFAOYSA-N 0.000 description 3
- BGYHLZZASRKEJE-UHFFFAOYSA-N [3-[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxy]-2,2-bis[3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoyloxymethyl]propyl] 3-(3,5-ditert-butyl-4-hydroxyphenyl)propanoate Chemical compound CC(C)(C)C1=C(O)C(C(C)(C)C)=CC(CCC(=O)OCC(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)(COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)COC(=O)CCC=2C=C(C(O)=C(C=2)C(C)(C)C)C(C)(C)C)=C1 BGYHLZZASRKEJE-UHFFFAOYSA-N 0.000 description 3
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- 239000001361 adipic acid Substances 0.000 description 3
- 229910052782 aluminium Inorganic materials 0.000 description 3
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- GDTBXPJZTBHREO-UHFFFAOYSA-N bromine Substances BrBr GDTBXPJZTBHREO-UHFFFAOYSA-N 0.000 description 3
- 229910052794 bromium Inorganic materials 0.000 description 3
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- 238000006731 degradation reaction Methods 0.000 description 3
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- FDPIMTJIUBPUKL-UHFFFAOYSA-N pentan-3-one Chemical compound CCC(=O)CC FDPIMTJIUBPUKL-UHFFFAOYSA-N 0.000 description 3
- NBIIXXVUZAFLBC-UHFFFAOYSA-K phosphate Chemical compound [O-]P([O-])([O-])=O NBIIXXVUZAFLBC-UHFFFAOYSA-K 0.000 description 3
- 229910052698 phosphorus Inorganic materials 0.000 description 3
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- MYRTYDVEIRVNKP-UHFFFAOYSA-N 1,2-Divinylbenzene Chemical compound C=CC1=CC=CC=C1C=C MYRTYDVEIRVNKP-UHFFFAOYSA-N 0.000 description 2
- SMZOUWXMTYCWNB-UHFFFAOYSA-N 2-(2-methoxy-5-methylphenyl)ethanamine Chemical compound COC1=CC=C(C)C=C1CCN SMZOUWXMTYCWNB-UHFFFAOYSA-N 0.000 description 2
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Abstract
Description
[1]スチレン系樹脂、難燃剤組成物、及び発泡剤を用いて押出発泡して得られるスチレン系樹脂押出発泡体であって、難燃剤組成物が、臭素化スチレンブタジエンポリマー、安定剤、及びスチレン系樹脂を含み、難燃剤組成物総重量100wt%とした場合、臭素化スチレンブタジエンポリマーが30〜80wt%であり、且つ難燃剤組成物が、TGAでの5wt%減少温度が255〜270℃であることを特徴とするスチレン系樹脂押出発泡体、
[2]難燃剤組成物中の安定剤として、エポキシ化合物、フェノール系安定剤、ホスファイト系安定剤、多価アルコール部分エステル、及びヒンダートアミン系安定剤からなる群より少なくとも2種以上選ばれる安定剤を含有することを特徴とする[1]に記載のスチレン系樹脂押出発泡体、
[3]前記スチレン系樹脂の総量100重量部に対して、臭素化スチレンブタジエンポリマーが0.5〜6重量部となるように難燃剤組成物を含有せしめることを特徴とする[1]または[2]記載のスチレン系樹脂押出発泡体、
[4]前記スチレン系樹脂の総量100重量部に対して、ラジカル発生剤を0.05〜0.5重量部含有することを特徴とする、[1]〜[3]のいずれかに記載のスチレン系樹脂押出発泡体、
[5]ラジカル発生剤が、2,3−ジメチル−2,3−ジフェニルブタン、ポリ−1,4−ジイソプロピルベンゼンよりなる群から選ばれる少なくとも1種であることを特徴とする、[4]に記載のスチレン系樹脂押出発泡体、
[6]リン酸エステル、ホスフィンオキシドよりなる群から選ばれる少なくとも1種を含有することを特徴とする、[1]〜[5]のいずれかに記載のスチレン系樹脂押出発泡体、
[7]リン酸エステルが、トリフェニルホスフェート、トリス(トリブロモネオペンチル)ホスフェートよりなる群から選ばれる少なくとも1種であり、ホスフィンオキシドがトリフェニルホスフィンオキシドであることを特徴とする、[6]に記載のスチレン系樹脂押出発泡体、
[8]発泡剤が、炭素数が3〜5である飽和炭化水素から選ばれる少なくとも1種を含むことを特徴とする、[1]〜[7]のいずれかに記載のスチレン系樹脂押出発泡体、
[9]発泡剤として、さらに、水、二酸化炭素、窒素、炭素数が1〜4のアルコール類、ジメチルエーテル、塩化メチル、塩化エチルよりなる群から選ばれる少なくとも1種を含むことを特徴とする、[8]に記載のスチレン系樹脂押出発泡体、
[10]前記スチレン系樹脂押出発泡体が、JIS A9511の燃焼試験方法に合格することを特徴とする[1]〜[9]のいずれかに記載のスチレン系樹脂押出発泡体、
[11]前記スチレン系樹脂押出発泡体の酸素指数が26%以上であることを特徴とする[1]〜[10]のいずれかに記載のスチレン系樹脂押出発泡体、
[12]臭素化スチレンブタジエンポリマーを30〜80wt%並びに安定剤及びスチレン系樹脂を含み、TGAでの5wt%減少温度が255〜270℃である難燃剤組成物を調製し、該難燃剤組成物、スチレン系樹脂及び発泡剤を用いて押出発泡を行うことを特徴とするスチレン系樹脂押出発泡体の製造方法、
に関する。
なお、ペレット化の際には一般的に押出機によって溶融・混練が行われるが、難燃剤などへの影響も含め、樹脂の分子劣化ができる限り抑制される温度、例えば160〜240℃程度が好ましい。また、カット屑中の発泡剤を脱気する為に、ベント口を設けることが望ましい。
3000」として、また、ICL−IP社から商品名「FR−122P」として販売されている。
また、エポキシ化合物の含有量が多くなるにつれ、難燃剤組成物のTGAでの5wt%減少温度が高温側へシフトする傾向にある。尚、他の併用される安定剤との組み合わせにも依るが、上記の配合範囲(スチレン系樹脂押出発泡体に含有される臭素系難燃剤100重量部に対して4〜20重量部)を外れると、難燃剤組成物のTGAでの5wt%減少温度255〜270℃を外れる恐れがあり、結果的に発泡体の性能低下を招く恐れがある。
また、多価アルコール部分エステルの含有量が多くなるにつれ、難燃剤組成物のTGAでの5wt%減少温度が高温側へシフトする傾向にある。尚、他の併用される安定剤との組み合わせにも依るが、上記の配合範囲(スチレン系樹脂押出発泡体に含有される臭素系難燃剤100重量部に対して0〜20重量部)を外れると、難燃剤組成物のTGAでの5wt%減少温度が270℃を超える恐れがあり、結果的に発泡体の難燃性能低下を招く恐れがある。
また、フェノール系安定剤の含有量が多くなるにつれ、難燃剤組成物のTGAでの5wt%減少温度が高温側へシフトする傾向にある。尚、他の併用される安定剤との組み合わせにも依るが、上記の配合範囲(スチレン系樹脂押出発泡体に含有される臭素系難燃剤100重量部に対して4〜20重量部)を外れると、難燃剤組成物のTGAでの5wt%減少温度が270℃を超える恐れがあり、結果的に発泡体の性能低下を招く恐れがある。
また、ホスファイト系安定剤の含有量が多くなるにつれ、難燃剤組成物のTGAでの5wt%減少温度が高温側へシフトする傾向にある。尚、他の併用される安定剤との組み合わせにも依るが、上記の配合範囲(スチレン系樹脂押出発泡体に含有される臭素系難燃剤100重量部に対して2.0重量部以下)を外れると、難燃剤組成物の5wt%減少温度が270℃を超える恐れがあり、結果的に発泡体の難燃性能低下を招く恐れがある。
本発明で用いられるホスフィンオキシドとしては、トリフェニルホスフィンオキシドが好ましい。
これらリン酸エステル及びホスフィンオキシドは単独または2種以上併用しても良い。
本発明では、このように、特定の難燃剤組成物を予め調製し、これとスチレン系樹脂及び発泡剤を用いて発泡体とすることで、熱安定性及び難燃性に優れ且つ優れた外観を有する発泡体の提供を可能にした。
尚、スチレン系樹脂、難燃剤組成物、必要に応じて用いる添加剤を加熱溶融手段に供給する際に、前述の安定剤を更に添加してもよい。これにより、更にリサイクル性に優れたスチレン系樹脂押出発泡体を提供できる。
(A)スチレン系樹脂[PSジャパン(株)製、680]
(B)難燃剤
・臭素化スチレンブタジエンブロックポリマー[ケムチュラ製、EMERALD INNOVATION 3000、臭素含有率65wt%]
(C)エポキシ化合物
・ビスフェノール−A−グリシジルエーテル[ADEKA製、EP−13,エポキシ当量180〜200g/eq.]
・クレゾールノボラック型エポキシ樹脂[ハンツマンジャパン製、ECN−1280,エポキシ当量212〜233g/eq.]
(D)多価アルコール部分エステル
・ジペンタエリスリトール−アジピン酸反応混合物[味の素ファインテクノ製、プレンライザーST210]
(E)フェノール系安定剤
・ペンタエリトリトールテトラキス[3−(3’,5’−ジ−tert−ブチル−4’−ヒドロキシフェニル)プロピオネート] [ケムチュラ製 ANOX20]
(F)ホスファイト系安定剤
・3,9−ビス(2,4−ジ−tert−ブチルフェノキシ)−2,4,8,10−テトラオキサ−3,9−ジホスファスピロ[5.5]ウンデカン [ケムチュラ製 Ultranox626]
(G)ラジカル発生剤
・ポリ−1,4−ジイソプロピルベンゼン [UNITED INITIATORS製、CCPIB]
(H)リン系難燃剤
・トリフェニルホスフィンオキシド[住友商事ケミカル]
(I)発泡剤
・イソブタン[三井化学株式会社製]
・工業ブタン[岩谷産業株式会社製]
・水[水道水]
・ジメチルエーテル[三井化学株式会社製]
(J)その他添加剤
・タルク[林化成製、タルカンパウダーPK−Z]
・ベントナイト[ホージュン製、ベンゲルブライト11K]
・シリカ[エボニックデグサジャパン製、カープレックスBS304F]
酸素フラスコ燃焼法にて、臭素系難燃剤の分解後、イオンクロマトグラフ法にてBr含有量を定量した。
試料重量:7mg
測定装置:TG−DTG60A(島津製作所製)
測定セル:アルミニウム
測定雰囲気:窒素(20ml/min)
温度条件:室温(約25℃)から400℃まで10℃/minの昇温速度で加熱
5wt%減少温度:該試料の150℃における試料の質量を基準として、5%重量が減少する温度。
難燃剤組成物のペレット中に、黒スジ及び黒斑点等の変色が無いものを合格とした。
難燃剤組成物が、ストランドカット法にて円柱状にカットできたものについて合格とした。
発泡体密度は、発泡体密度(g/cm3)=発泡体重量(g)/発泡体体積(cm3)に基づいて求め、単位を(kg/m3)に換算して示した。
得られたサンプルを室内に保管し、製造後7日経過した発泡体について、JIS A9511に準拠して測定した。
○:3秒以内に炎が消えて、残じんがなく、燃焼限界指示線を超えて燃焼しないとの基準を満たす。
×:上記基準を満たさない。
発泡体の酸素指数は、JIS K 7201:1999に準拠する方法で測定した。
押出発泡体について、気泡径0.2mm以下の気泡の発泡体断面積あたりの占有面積比を、以下のようにして求めた。ここで、気泡径0.2mm以下の気泡とは、円相当直径が0.2mm以下の気泡とする。
a)走査型電子顕微鏡[(株)日立製作所製、品番:S−450]にて30倍に拡大して発泡体の縦断面を写真撮影する。
b)撮影した写真の上にOHPシートを置き、その上に厚さ方向の径が7.5mmよりも大きい気泡(実寸法が0.2mmより大きい気泡に相当する)に対応する部分を黒インキで塗りつぶして写しとる(一次処理)。
c)画像処理装置[(株)ピアス製、品番:PIAS−II]に一次処理画像を取り込み、濃色部分と淡色部分を、即ち黒インキで塗られた部分か否かを識別する。
d)濃色部分のうち、直径7.5mm以下の円の面積に相当する部分、即ち、厚さ方向の径は長いが、面積的には直径7.5mm以下の円の面積にしかならない部分を淡色化して、濃色部分の補正を行う。
e)画像解析計算機能中の「FRACTAREA(面積率)」を用い、画像全体に占める気泡径7.5mm以下(濃淡で分割した淡色部分)の面積比を次式により求める。
小気泡占有面積比(%)=(1−濃色部分の面積/画像全体の面積)×100
得られたスチレン系樹脂押出発泡体の気泡径は、ASTM D 3567に準拠する方法で測定した。
発泡体作成後7日経過したスチレン系樹脂押出発泡体の熱伝導率を、JIS A9511に準じて測定した。
幅910mm×長さ1820mmの押出発泡板の片一方のみの表面を目視(n=100サンプル)し、黒い点が目視で1つでも確認された場合を不合格品とし、その発生率を下記の評価基準によって評価した。
〇:不合格品が、2枚未満である。
△:不合格品が、2枚以上、5枚未満である。
×:不合格品が、5枚以上である。
(実施例1)
難燃剤組成物総重量を100wt%とした場合、スチレン系樹脂(ポリスチレン680)42.25wt%、難燃剤として臭素化SBSブロックポリマー(EMERALD INNOVATION 3000)50wt%、安定剤として、エポキシ化合物であるクレゾールノボラック型エポキシ樹脂(ARALDITE ECN−1280)2.5wt%、フェノール系安定剤であるペンタエリトリトールテトラキス[3−(3’,5’−ジ−tert−ブチル−4’−ヒドロキシフェニル)プロピオネート](ANOX20)5.0wt%、ホスファイト系安定剤である3,9−ビス(2,4−ジ−tert−ブチルフェノキシ)−2,4,8,10−テトラオキサ−3,9−ジホスファスピロ[5.5]ウンデカン(Ultranox626)0.25wt%を、予めドライブレンドした。その後、口径46mm、L/D≒30の同方向2軸押出機に、シリンダ設定温度150℃の条件で、吐出量50kg/Hrで供給し、ストランドカット法にて難燃剤組成物を作製した。ダイ出口での樹脂温度は190℃であった。
表1に示すように、難燃剤の比率、安定剤の種類・添加量を変更した以外は、実施例1と同様の操作により、難燃剤組成物を得た。得られた難燃剤組成物の特性を、表1に示す。
(実施例A)
スチレン系樹脂100部(難燃剤組成物中のスチレン系樹脂も含む)に対して、実施例1で得られた難燃剤組成物を6.0重量部(難燃剤として3.0重量部に相当するように調整)、ビスフェノールAグリシジルエーテル(EP−13)0.15部、多価アルコール部分エステル(プレンライザーST210)0.2部、ラジカル発生剤としてポリ−1,4−ジイソプロピルベンゼン/0.1部、ステアリン酸カルシウム/0.1部、タルク0.5部、ベントナイト0.5部およびシリカ0.2部をドライブレンドし、樹脂混合物を得た。
表2、3に示すように、発泡剤の種類・使用量、難燃剤組成物の種類、使用量、難燃助剤の種類・使用量、安定剤の種類・使用量、及び他の配合剤の種類・添加量を変更した以外は、実施例1と同様の操作により、発泡体を得た。尚、( )※1と記載されたスチレン系樹脂の重量部は、難燃剤組成物内に含有されたスチレン系樹脂を含めての数値である。また、( )※2と記載された難燃剤及び安定剤の重量部は、難燃剤組成物内に含有された難燃剤もしくは安定剤を、押出発泡体作成時のスチレン系樹脂を100重量とした時の換算値である。得られた発泡体の特性を、表2、3に示す。
Claims (12)
- スチレン系樹脂、難燃剤組成物、及び発泡剤を用いて押出発泡して得られるスチレン系樹脂押出発泡体であって、
難燃剤組成物が、臭素化スチレンブタジエンポリマー、安定剤、及びスチレン系樹脂を含み、難燃剤組成物総重量100wt%とした場合、臭素化スチレンブタジエンポリマーが30〜80wt%であり、且つ難燃剤組成物が、TGAでの5wt%減少温度が255〜270℃であることを特徴とするスチレン系樹脂押出発泡体。 - 難燃剤組成物中の安定剤として、エポキシ化合物、フェノール系安定剤、ホスファイト系安定剤、多価アルコール部分エステル、及びヒンダートアミン系安定剤からなる群より少なくとも2種以上選ばれる安定剤を含有することを特徴とする請求項1に記載のスチレン系樹脂押出発泡体。
- 前記スチレン系樹脂の総量100重量部に対して、臭素化スチレンブタジエンポリマーが0.5〜6重量部となるように難燃剤組成物を含有せしめることを特徴とする請求項1または2記載のスチレン系樹脂押出発泡体。
- 前記スチレン系樹脂の総量100重量部に対して、ラジカル発生剤を0.05〜0.5重量部含有することを特徴とする、請求項1〜3のいずれかに記載のスチレン系樹脂押出発泡体。
- ラジカル発生剤が、2,3−ジメチル−2,3−ジフェニルブタン、ポリ−1,4−ジイソプロピルベンゼンよりなる群から選ばれる少なくとも1種であることを特徴とする、請求項4に記載のスチレン系樹脂押出発泡体。
- リン酸エステル、ホスフィンオキシドよりなる群から選ばれる少なくとも1種を含有することを特徴とする、請求項1〜5のいずれかに記載のスチレン系樹脂押出発泡体。
- リン酸エステルが、トリフェニルホスフェート、トリス(トリブロモネオペンチル)ホスフェートよりなる群から選ばれる少なくとも1種であり、ホスフィンオキシドがトリフェニルホスフィンオキシドであることを特徴とする、請求項6に記載のスチレン系樹脂押出発泡体。
- 発泡剤が、炭素数が3〜5である飽和炭化水素から選ばれる少なくとも1種を含むことを特徴とする、請求項1〜7のいずれかに記載のスチレン系樹脂押出発泡体。
- 発泡剤として、さらに、水、二酸化炭素、窒素、炭素数が1〜4のアルコール類、ジメチルエーテル、塩化メチル、塩化エチルよりなる群から選ばれる少なくとも1種を含むことを特徴とする、請求項8に記載のスチレン系樹脂押出発泡体。
- 前記スチレン系樹脂押出発泡体が、JIS A9511の燃焼試験方法に合格することを特徴とする請求項1〜9のいずれかに記載のスチレン系樹脂押出発泡体。
- 前記スチレン系樹脂押出発泡体の酸素指数が26%以上であることを特徴とする請求項1〜10のいずれかに記載のスチレン系樹脂押出発泡体。
- 臭素化スチレンブタジエンポリマーを30〜80wt%並びに安定剤及びスチレン系樹脂を含み、TGAでの5wt%減少温度が255〜270℃である難燃剤組成物を調製し、該難燃剤組成物、スチレン系樹脂及び発泡剤を用いて押出発泡を行うことを特徴とするスチレン系樹脂押出発泡体の製造方法。
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