Fan-工作總結(jié)2012.7.11課件

新型熱塑性彈性體的制備與結(jié)構(gòu)調(diào)控（2011CB606004）中期匯報(bào)范星河

1)新型單體及三嵌段聚合物的設(shè)計(jì)與合成目標(biāo)單體分子結(jié)構(gòu)如下圖所示bpacbcdbda通過核磁共振、質(zhì)譜及元素分析等表征手段，確認(rèn)了所有中間體及目標(biāo)分子的化學(xué)結(jié)構(gòu)。Anal.Calcd.FoundC79.97%80.00%H6.71%6.80%氮氧自由基聚合及本體性質(zhì)表征NMPSamplesT(oC)Mn(g/mol)PDIPbp-11304,1001.36Pbp-21305,3001.37Pbp-31308,6001.33Pbp-413011,1001.29Pbp-513016,4001.31Pbp-613048,7001.23GPCProfiles樣品名5%熱失重溫度(oC）Pbp-1354Pbp-2367Pbp-3380Pbp-4349Pbp-5369Pbp-6348TGAProfiles樣品名玻璃化轉(zhuǎn)變溫度Tg

(oC）Pbp-1173Pbp-2185Pbp-3191Pbp-4207Pbp-5208Pbp-6217DSCProfiles隨著分子量的增大，玻璃化轉(zhuǎn)變溫度逐漸升高Pbp-1HeatingCoolingPbp-2HeatingCoolingPbp-5HeatingCoolingd-spacing:1.23nm六方柱狀相ROMP-CT聚合合成熱塑性彈性體目標(biāo)聚合物合成路線圖ROMP-CT聚合合成熱塑性彈性體aabbccddeeffgghhiiCTA1HNMRofCTA13CNMRofCTACTA[M+H]+聚合方法：Schlenk技術(shù)兩步投料or封管溶劑：二氯甲烷反應(yīng)溫度：40oCSamplesSolventT(oC)Monomer/CTAMn,GPC(g/mol)PDIMethodPB-119kDCM40600/1119.2k1.65封管PB-110kDCM40300/1110.2k1.68兩步投料PB-63kDCM40500/162.7k1.66兩步投料Cis-:70%Cis-Trans-PB-119k溶劑：氯苯反應(yīng)溫度：130oCSampleSolventT(oC)Monomer/macroinitiatorMn,GPC(g/mol)PDIPbp-PB-Pbpchlorobenzene130100/182.2k1.99流體力學(xué)半徑變小Overberger,C.G.;Frazier,C.;Mandelman,J.;Smith,H.F.,JournaloftheAmericanChemicalSociety1953,

75(14),3326-3330.2）對(duì)庚烷苯乙烯單體及三嵌段聚合物設(shè)計(jì)與合成Macroinitiatormonomer:initiatorMw(*103)PDIMI1210:1221.15MI2410:1421.22MI3680:1671.27MI2MI1MI3三嵌段聚合物合成TriblockM2:MI1Mn(*103)(GPC)PDIM2content(1H-NMR)

Tri122:1331.3653.5%Pbp52-PSt90-Pbp52Tri111:1511.3964.7%Pbp82-PSt90-Pbp82Tri211:2