JP4895553B2 - ジスルフィド結合含有ポリプロピレン - Google Patents
ジスルフィド結合含有ポリプロピレン Download PDFInfo
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- JP4895553B2 JP4895553B2 JP2005244615A JP2005244615A JP4895553B2 JP 4895553 B2 JP4895553 B2 JP 4895553B2 JP 2005244615 A JP2005244615 A JP 2005244615A JP 2005244615 A JP2005244615 A JP 2005244615A JP 4895553 B2 JP4895553 B2 JP 4895553B2
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- polypropylene
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Description
本発明において特に好ましい反応は下式に表されるように、具体的にはチオ酢酸をラジカル開始剤とともに使用することにより、チオ酢酸エステル化する方法である。ここで、ラジカル開始剤は特に制限はないが、具体的には2,2′−アゾビスイソブチロニトリル(AIBN)が好ましい。
GPC(ゲル濾過クロマトグラフィー):GPC−8020(東ソー(株)製)FT−IR(赤外線吸収スペクトル):1600−FT−IR(パーキンエルマー社(株)製)、KBr法
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、Mn=11万、Mw/Mn=4.8)を回分式真空熱分解装置(大型装置)で高度制御熱分解することにより合成して両末端にビニリデン基を有するテレケリックiPP−TVDを得た。得られたiPP−TVDは、Mn=1.0x103、Mw/Mn=1.0、ftvd=1.8であった。
実施例1で得られた溶液にKOHの水・エタノール溶液(1:1.5vol/vol、60%)を2.5ml加え、90℃で3時間反応させた。その後、濃塩酸10.1ml加え、90℃で2時間反応させ、脱酢酸反応させた。
上で得られたiPP-SCOCH32gをトルエン20mlに溶解し、水酸化カリウム4g、水4ml、エタノール4mlを加えて空気雰囲気中で90℃で加熱して加水分解を行った。反応混合物を過剰のメタノール中に滴下し、白色の生成物2gを得得た。以下ジスルフィド結合含有ポリプロピレンをiPP-SS-iPP.1とした。
iPP-SS-iPP.1の2gをトルエン20mlに溶解し、エタノール4ml、水4ml、亜鉛粉末4g、濃塩酸20mlを加え90℃で、窒素雰囲気下で加熱して還元を行った。反応混合液を熱ろ過し、過剰のメタノール中に滴下した。生成した沈殿物はろ別回収し、減圧加温乾燥した。以下得られた両末端チオール化オリゴプロピレンをiPP-SHとした。収率は約80%であった。
iPP-SHをトルエン0.5mlに溶解し、30%過酸化水素0.2mlとKOH0.1gを用いて80℃3時間加熱して酸化反応を行った。反応混合物を過剰のメタノール中に滴下し得られた生成物をiPP-SS-iPP.2とした。収率はほぼ定量的であった。GPC曲線、及び分子量特性をそれぞれ図3、表2に示した。
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JP2005244615A JP4895553B2 (ja) | 2005-08-25 | 2005-08-25 | ジスルフィド結合含有ポリプロピレン |
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JP2007056166A JP2007056166A (ja) | 2007-03-08 |
JP4895553B2 true JP4895553B2 (ja) | 2012-03-14 |
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JP2005244615A Expired - Fee Related JP4895553B2 (ja) | 2005-08-25 | 2005-08-25 | ジスルフィド結合含有ポリプロピレン |
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JPS5027516B2 (ja) * | 1972-02-07 | 1975-09-08 | ||
JP3853719B2 (ja) * | 2002-09-19 | 2006-12-06 | 孝志 澤口 | 両末端チオール化オリゴプロピレン |
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