JP5719730B2 - 熱発泡性樹脂組成物、熱発泡性樹脂シート、発泡体およびその製造方法 - Google Patents
熱発泡性樹脂組成物、熱発泡性樹脂シート、発泡体およびその製造方法 Download PDFInfo
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- JP5719730B2 JP5719730B2 JP2011192113A JP2011192113A JP5719730B2 JP 5719730 B2 JP5719730 B2 JP 5719730B2 JP 2011192113 A JP2011192113 A JP 2011192113A JP 2011192113 A JP2011192113 A JP 2011192113A JP 5719730 B2 JP5719730 B2 JP 5719730B2
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- 125000001449 isopropyl group Chemical group [H]C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 238000010030 laminating Methods 0.000 description 1
- 239000007788 liquid Substances 0.000 description 1
- 239000000314 lubricant Substances 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
- 229910001629 magnesium chloride Inorganic materials 0.000 description 1
- 235000011147 magnesium chloride Nutrition 0.000 description 1
- VTHJTEIRLNZDEV-UHFFFAOYSA-L magnesium dihydroxide Chemical compound [OH-].[OH-].[Mg+2] VTHJTEIRLNZDEV-UHFFFAOYSA-L 0.000 description 1
- 239000000347 magnesium hydroxide Substances 0.000 description 1
- 229910001862 magnesium hydroxide 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
- 229910052943 magnesium sulfate Inorganic materials 0.000 description 1
- 235000019341 magnesium sulphate Nutrition 0.000 description 1
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- 230000005291 magnetic effect Effects 0.000 description 1
- 230000007257 malfunction Effects 0.000 description 1
- 125000002960 margaryl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- 229910052759 nickel Inorganic materials 0.000 description 1
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- 125000001147 pentyl group Chemical group C(CCCC)* 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
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- 239000000049 pigment Substances 0.000 description 1
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- 229920003192 poly(bis maleimide) Polymers 0.000 description 1
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- 239000002861 polymer material Substances 0.000 description 1
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- 229920000306 polymethylpentene Polymers 0.000 description 1
- 229920006324 polyoxymethylene Polymers 0.000 description 1
- 229920006380 polyphenylene oxide Polymers 0.000 description 1
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- 229920000128 polypyrrole Polymers 0.000 description 1
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- 229920001021 polysulfide Polymers 0.000 description 1
- 150000008117 polysulfides Polymers 0.000 description 1
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- 229910000027 potassium carbonate Inorganic materials 0.000 description 1
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- OTYBMLCTZGSZBG-UHFFFAOYSA-L potassium sulfate Chemical compound [K+].[K+].[O-]S([O-])(=O)=O OTYBMLCTZGSZBG-UHFFFAOYSA-L 0.000 description 1
- 229910052939 potassium sulfate Inorganic materials 0.000 description 1
- 235000011151 potassium sulphates Nutrition 0.000 description 1
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- 125000001436 propyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
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- 125000004805 propylene group Chemical group [H]C([H])([H])C([H])([*:1])C([H])([H])[*:2] 0.000 description 1
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- 239000012744 reinforcing agent Substances 0.000 description 1
- 239000012779 reinforcing material Substances 0.000 description 1
- 150000003839 salts Chemical class 0.000 description 1
- 125000002914 sec-butyl group Chemical group [H]C([H])([H])C([H])([H])C([H])(*)C([H])([H])[H] 0.000 description 1
- 239000011669 selenium Substances 0.000 description 1
- 229910052711 selenium Inorganic materials 0.000 description 1
- 239000011359 shock absorbing material Substances 0.000 description 1
- 239000000377 silicon dioxide Substances 0.000 description 1
- 229920002050 silicone resin Polymers 0.000 description 1
- 229910052709 silver Inorganic materials 0.000 description 1
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- WXMKPNITSTVMEF-UHFFFAOYSA-M sodium benzoate Chemical compound [Na+].[O-]C(=O)C1=CC=CC=C1 WXMKPNITSTVMEF-UHFFFAOYSA-M 0.000 description 1
- 239000004299 sodium benzoate Substances 0.000 description 1
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- 229910000029 sodium carbonate Inorganic materials 0.000 description 1
- 239000011780 sodium chloride Substances 0.000 description 1
- 229940080264 sodium dodecylbenzenesulfonate Drugs 0.000 description 1
- 239000004317 sodium nitrate Substances 0.000 description 1
- 235000010344 sodium nitrate Nutrition 0.000 description 1
- ZNCPFRVNHGOPAG-UHFFFAOYSA-L sodium oxalate Chemical compound [Na+].[Na+].[O-]C(=O)C([O-])=O ZNCPFRVNHGOPAG-UHFFFAOYSA-L 0.000 description 1
- CHQMHPLRPQMAMX-UHFFFAOYSA-L sodium persulfate Substances [Na+].[Na+].[O-]S(=O)(=O)OOS([O-])(=O)=O CHQMHPLRPQMAMX-UHFFFAOYSA-L 0.000 description 1
- 229910052938 sodium sulfate Inorganic materials 0.000 description 1
- 235000011152 sodium sulphate Nutrition 0.000 description 1
- 238000004544 sputter deposition Methods 0.000 description 1
- 239000003381 stabilizer Substances 0.000 description 1
- 125000004079 stearyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- QAZLUNIWYYOJPC-UHFFFAOYSA-M sulfenamide Chemical class [Cl-].COC1=C(C)C=[N+]2C3=NC4=CC=C(OC)C=C4N3SCC2=C1C QAZLUNIWYYOJPC-UHFFFAOYSA-M 0.000 description 1
- 150000003464 sulfur compounds Chemical class 0.000 description 1
- 150000003467 sulfuric acid derivatives Chemical class 0.000 description 1
- 238000010557 suspension polymerization reaction Methods 0.000 description 1
- 239000000454 talc Substances 0.000 description 1
- 229910052623 talc Inorganic materials 0.000 description 1
- 150000003505 terpenes Chemical class 0.000 description 1
- 235000007586 terpenes Nutrition 0.000 description 1
- 125000000999 tert-butyl group Chemical group [H]C([H])([H])C(*)(C([H])([H])[H])C([H])([H])[H] 0.000 description 1
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- 229920002725 thermoplastic elastomer Polymers 0.000 description 1
- 229920006259 thermoplastic polyimide Polymers 0.000 description 1
- 239000004416 thermosoftening plastic Substances 0.000 description 1
- 229960002447 thiram Drugs 0.000 description 1
- 239000013008 thixotropic agent Substances 0.000 description 1
- 229910052718 tin Inorganic materials 0.000 description 1
- 239000011135 tin Substances 0.000 description 1
- OGIDPMRJRNCKJF-UHFFFAOYSA-N titanium oxide Inorganic materials [Ti]=O OGIDPMRJRNCKJF-UHFFFAOYSA-N 0.000 description 1
- KHPCPRHQVVSZAH-UHFFFAOYSA-N trans-cinnamyl beta-D-glucopyranoside Natural products OC1C(O)C(O)C(CO)OC1OCC=CC1=CC=CC=C1 KHPCPRHQVVSZAH-UHFFFAOYSA-N 0.000 description 1
- 125000002889 tridecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 125000002948 undecyl group Chemical group [H]C([*])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])C([H])([H])[H] 0.000 description 1
- 229930195735 unsaturated hydrocarbon Natural products 0.000 description 1
- 229920006337 unsaturated polyester resin Polymers 0.000 description 1
- 238000001771 vacuum deposition Methods 0.000 description 1
- 238000004073 vulcanization Methods 0.000 description 1
- 238000005303 weighing Methods 0.000 description 1
- 239000002023 wood Substances 0.000 description 1
- 150000003751 zinc Chemical class 0.000 description 1
- 229910052725 zinc Inorganic materials 0.000 description 1
- 239000011701 zinc Substances 0.000 description 1
- BOXSVZNGTQTENJ-UHFFFAOYSA-L zinc dibutyldithiocarbamate Chemical compound [Zn+2].CCCCN(C([S-])=S)CCCC.CCCCN(C([S-])=S)CCCC BOXSVZNGTQTENJ-UHFFFAOYSA-L 0.000 description 1
- AUMBZPPBWALQRO-UHFFFAOYSA-L zinc;n,n-dibenzylcarbamodithioate Chemical compound [Zn+2].C=1C=CC=CC=1CN(C(=S)[S-])CC1=CC=CC=C1.C=1C=CC=CC=1CN(C(=S)[S-])CC1=CC=CC=C1 AUMBZPPBWALQRO-UHFFFAOYSA-L 0.000 description 1
- BPCLXRJJXQFTJE-UHFFFAOYSA-L zinc;n,n-dibenzylcarbamothioate Chemical compound [Zn+2].C=1C=CC=CC=1CN(C(=S)[O-])CC1=CC=CC=C1.C=1C=CC=CC=1CN(C(=S)[O-])CC1=CC=CC=C1 BPCLXRJJXQFTJE-UHFFFAOYSA-L 0.000 description 1
- KMNUDJAXRXUZQS-UHFFFAOYSA-L zinc;n-ethyl-n-phenylcarbamodithioate Chemical compound [Zn+2].CCN(C([S-])=S)C1=CC=CC=C1.CCN(C([S-])=S)C1=CC=CC=C1 KMNUDJAXRXUZQS-UHFFFAOYSA-L 0.000 description 1
- 229910000859 α-Fe Inorganic materials 0.000 description 1
Images
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- Manufacture Of Porous Articles, And Recovery And Treatment Of Waste Products (AREA)
Description
(発泡性ビーズの調製)
脱イオン水700gに、第三リン酸カルシウム1.5g、α−オレフィンスルホン酸ナトリウム0.0525g、アルキルジフェニルエーテルジスルホン酸ナトリウム0.0175g、酢酸ナトリウム1.1g、および、過硫酸カリウム(10時間半減期温度71℃)0.00025gを、撹拌装置の付いた3Lのオートクレーブに仕込んだ。
モノマー溶液の調製において、スチレンの配合量を429.3gから404.0gに変更し、アクリル酸ブチルの配合量を75.8gから101.0gに変更し、α−メチルスチレンダイマーを添加しなかった以外は、調製例1と同様に処理し、発泡性ビーズBを調製した。
モノマー溶液の調製において、スチレンの配合量を429.3gから454.5gに変更し、アクリル酸ブチルの配合量を75.8gから50.5gに変更し、α−メチルスチレンダイマーを添加しなかった以外は、調製例1と同様に処理し、発泡性ビーズCを調製した。
モノマー溶液の調製において、α−メチルスチレンダイマーを添加しなかった以外は、調製例1と同様に処理し、発泡性ビーズDを調製した。
市販品であるマツモトマイクロスフェアーF−36(熱膨張性マイクロカプセル、松本油脂製薬社製)を、比較調製例1の熱膨張カプセルEとして準備した。
実施例1、2、8〜21および比較例1
各成分を、表2〜表5の配合処方に従って、ミキシングロールにて、50℃で、回転数10min−1、10分間混練して、混練物(熱発泡性樹脂組成物)を調製した。その後、調製した混練物を、50℃、圧力50kg/cm2で、5分間プレスすることにより、厚み5mmの熱発泡性樹脂シートを形成した。
混練温度およびプレス温度を、常温(20℃)に変更した以外は、実施例1と同様に処理することにより、厚み5mmの熱発泡性樹脂シートを形成した。
(発泡性ビーズおよび熱膨張カプセルの評価)
(1) 重量平均分子量
発泡性ビーズA〜Dをテトラヒドロフランにそれぞれ溶解させて、熱膨張性物質を除去するとともに、テトラヒドロフランの0.1質量%溶液を調製し、これを下記に示すゲル・パーミエーション・クロマトグラフにて測定し、ポリスチレンの校正曲線に基づく重量平均分子量を算出した。
カラム:TSK−GEL SuperH−H、2本連結
カラム温度:40℃
流量:0.6mL/分
移動相:テトラヒドロフラン
検出器:示差屈折率検出器(RID)
その結果を表1に示す。
(2) ガラス転移温度
発泡性ビーズA〜Dを180℃でそれぞれ熱プレスすることにより、熱膨張性物質を除去し、アクリル酸ブチル・スチレンコポリマーからなるシートを作製し、そのガラス転移温度を、昇温速度10℃/分で示差走査熱量測定により、JIS K7121−1987に基づいて測定される熱処理後の中間点ガラス転移温度として、測定した。
(3) 揮発分量
発泡性ビーズA〜Dの揮発分量を、190℃で10分間サンプルを加熱する加熱減量法により測定した。
(4) かさ密度
発泡性ビーズA 1質量部を、表1に記載の所定温度の温水400質量部に投入し、10分間撹拌してそれらを発泡させた後、発泡したビーズAを温水から取り出し、水分を一昼夜、自然乾燥により除去し、100mLのメスシリンダー内に、100mLの標線位置まで充填し、その発泡したビーズAを0.1gの値まで秤量することにより、発泡後のかさ密度(g/L)を測定した。
80*2:計算上の値
0.01〜0.016*3:体積分率の粒径分布カーブにおける累積50%の値(D50)
47.5*4:計算上の値
(熱発泡性樹脂シートの評価)
(1) ムーニー粘度
上記した混練物の調製において、発泡性樹脂粒子を配合せずに、それら以外の成分を混練して得られた混練物について、ムーニー粘度(ML1+4、100℃)を測定した。その結果を表2〜表5に示す。
(2) 密度および発泡倍率
上記により得られた厚み5mmの熱発泡性樹脂シートを、直径19mmの円形状に打ち抜いてサンプルを作製し、その後、作製したサンプルを、65℃のオーブンに投入して、30分間加熱することにより、サンプルを発泡させて、発泡体を得た。
(3) 発泡直後の発泡充填性
上記により得られた厚み5mmの熱発泡性樹脂シートを、長さ50mm、幅20mmのサイズに切り取ってサンプル(1)を作製し、その後、作製したサンプル(1)を、図5(a)に示すサイズ(長さ50mm、幅25mm)の試験鋼板(2)の間において、下側の試験鋼板(2)の上面の中央に載置した。
○:発泡充填性が良好であった。
(4) 80℃で100時間保存後の充填性
上記(3)と同様にして得られた発泡体を、80℃で100時間保持し、試験鋼板(2)の間における発泡体(3)の充填性を目視にて下記の基準にて評価した。その結果を表2〜表5に示す。
○:発泡体(3)が試験鋼板(2)の間を充填したまま、隙間ができなかった。
ポリイソブチレンゴム*1:商品名「Oppanol B50」、重量平均分子量(GPC:標準ポリスチレン換算値)340000、密度0.92g/cm3、BASF社製
ポリイソブチレンゴム*2:商品名「Oppanol B12」、重量平均分子量(GPC:標準ポリスチレン換算値)51000、密度0.92g/cm3、BASF社製
シリコーンゴム*3:商品名「KE−550−U」、密度1.21g/cm3、信越シリコーン社製
シリコーンゴム*4:商品名「KE−951−U」、密度1.14g/cm3、信越シリコーン社製
EPDM*5:商品名「EPT9090M」、ジエン含有量14.2%、三井化学社製
EPDM*6:商品名「EPT4045」、ジエン含有量8.0%、三井化学社製
EPDM*7:商品名「EPT1045」、ジエン含有量5.0%、三井化学社製
天然ゴム*8:商品名「INT3RSS Small Bale」、素練ゴム、Teck Bee Hang社製
SBR*9:スチレン・ブタジエンゴム、商品名「タフデン2003」、スチレン含有量25質量%、ムーニー粘度33(ML(1+4)100℃)、旭化成社製
BR*10:ブタジエンゴム、商品名「JSR BR01」、ムーニー粘度45(ML(1+4)100℃)、JSR社製
NBR*11、アクリロニトリル・ブタジエンゴム、商品名「Nipol DN219」、ニトリル含有量33.5質量%、ムーニー粘度27(1+4)100℃)、日本ゼオン社製
エポキシ樹脂*12:商品名「エピコート♯834」、ビスフェノールA型エポキシ樹脂、エポキシ当量230〜270、密度1.18g/cm3、JER社製
エポキシ樹脂*13:商品名「PKHM−301」、ビスフェノールA型エポキシ樹脂、ガラス転移温度45℃、重量平均分子量39000、ガラス転移温度45℃、InChem社製
石油系樹脂*14:商品名「ペトロタック 90HM」、C5脂肪族/C9芳香族共重合石油樹脂、軟化点88℃、東ソー社製
硫黄*15:微粉硫黄、200メッシュ、細井化学工業社製
酸化亜鉛*16:平均粒子径0.24〜0.3μm
2−メルカプトベンゾチアゾール*17:商品名「ノクセラーM」、大内新興化学社製
ジベンジルジチオカルバミン酸亜鉛*18:商品名「ノクセラーZTC」、大内新興化学社製
ジメチルジチオカルバミン酸亜鉛*19:商品名「ノクセラーPZ」、大内新興化学社製
アミン化合物*20:商品名「ノックマスターEGS」、大内新興化学社製
ムーニー粘度*21:100℃のムーニー粘度、自動ムーニー粘度計「AM−1」(東洋精機製作所社製)にて測定
密度*22:JIS Z8807に準拠して測定
発泡倍率*23:体積発泡倍率=発泡前のサンプルの密度/発泡後の発泡体の密度
発泡直後*24:65℃で30分間発泡直後
2 試験鋼板(中空部材)
3 発泡体
4 発熱部材
5 熱発泡性積層体
Claims (12)
- 発泡性樹脂粒子と樹脂組成物とを含有し、
前記発泡性樹脂粒子は、中実の樹脂に発泡剤が含有され、
前記中実の樹脂が、スチレン系モノマーと、(メタ)アクリル酸アルキルエステルとの共重合体であり、
前記(メタ)アクリル酸アルキルエステルの配合割合は、前記(メタ)アクリル酸アルキルエステルおよび前記スチレン系モノマーの総量に対して、5質量%以上、50質量%以下であり、
前記樹脂の重量平均分子量は、ゲル・パーミエーション・クロマトグラフによる標準ポリスチレン換算値で、50万以下、5万以上であり、
前記発泡性樹脂粒子は、70℃の温水に浸漬して発泡させた後のかさ密度が、15〜100g/Lであることを特徴とする、熱発泡性樹脂組成物。 - 90℃以下で発泡することを特徴とする、請求項1に記載の熱発泡性樹脂組成物。
- 65℃で30分加熱して発泡させた発泡体の密度が、0.05〜0.75g/cm3であることを特徴とする、請求項1または2に記載の熱発泡性樹脂組成物。
- 前記発泡性樹脂粒子の配合割合が、前記樹脂組成物100質量部に対して、0.1〜350質量部であることを特徴とする、請求項1〜3のいずれか一項に記載の熱発泡性樹脂組成物。
- 前記樹脂組成物が、ゴム、熱可塑性樹脂および熱硬化性樹脂からなる群から選択される少なくとも1種を含有していることを特徴とする、請求項1〜4のいずれか一項に記載の熱発泡性樹脂組成物。
- 前記ゴム、前記熱可塑性樹脂および/または前記熱硬化性樹脂のガラス転移温度が、50℃以下であることを特徴とする、請求項5に記載の熱発泡性樹脂組成物。
- さらに、架橋剤を含有することを特徴とする、請求項1〜6のいずれか一項に記載の熱発泡性樹脂組成物。
- さらに、架橋促進剤を含有することを特徴とする、請求項7に記載の熱発泡性樹脂組成物。
- 請求項1〜8のいずれか一項に記載の熱発泡性樹脂組成物が、シート状に形成されていることを特徴とする、熱発泡性樹脂シート。
- 請求項1〜8のいずれか一項に記載の熱発泡性樹脂組成物を加熱して発泡させることにより得られることを特徴とする、発泡体。
- 請求項1〜8のいずれか一項に記載の熱発泡性樹脂組成物を加熱して発泡させることを特徴とする、発泡体の製造方法。
- 90℃以下の温度で加熱することを特徴とする、請求項11に記載の発泡体の製造方法。
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