PSt-b-PtBA嵌段共聚物的AGET-ATRP法合成
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摘要
采用活性自由基聚合方法,第一步以苯乙烯为单体,引发剂为溴化苄(BzBr),氯化铁为催化剂,三苯基膦为配体,电子活化再生原子转移自由基聚(AGET-ATRP)法合成得到了聚苯乙烯(PSt-Cl)大分子引发剂;第二步用溴化亚铜(CuBr)为催化剂,联吡啶(bpy)作为配体,用原子转移自由基聚合(ATRP)法得到了嵌段共聚物聚苯乙烯-b-聚丙烯酸叔丁酯(PSt-b-PtBA)。产物的表征用凝胶渗透色谱(GPC)、红外、核磁;得到当温度为95℃时,n(tBA)/n(PSt-Cl)/n(CuBr)/n(bpy)=100∶1∶1∶2,反应时间为28h时,PSt-b-PtBA的分子量为11261,分子量分布(PDI)为1.43。
In this paper,living radical polymerization is used.The first step is styrene as monomer,the initiator is benzyl bromide(BzBr),ferric chloride is used as catalyst,triphenylphosphine is a ligand,and electron activation and regeneration atom transfer is free.Polystyrene(PSt-Cl)macroinitiator was synthesized by AGET-ATRP method;the second step was copper bromide(CuBr)as catalyst,bipyridyl(bpy)as ligand,and atom transfer The block copolymer polystyrene-b-poly(tert-butyl acrylate)(PSt-b-PtBA)was obtained by free radical polymerization(ATRP).Characterization of the product by gel permeation chromatography(GPC),infrared,nuclear magnetic;obtained at a temperature of 95℃,n(tBA)/n(PSt-Cl)/n(CuBr)/n(bpy)=100 :1 :1 :2,when the reaction time was 28 h,the molecular weight of PSt-b-PtBA was 11261,and the molecular weight distribution(PDI)was 1.43.
In this paper,living radical polymerization is used.The first step is styrene as monomer,the initiator is benzyl bromide(BzBr),ferric chloride is used as catalyst,triphenylphosphine is a ligand,and electron activation and regeneration atom transfer is free.Polystyrene(PSt-Cl)macroinitiator was synthesized by AGET-ATRP method;the second step was copper bromide(CuBr)as catalyst,bipyridyl(bpy)as ligand,and atom transfer The block copolymer polystyrene-b-poly(tert-butyl acrylate)(PSt-b-PtBA)was obtained by free radical polymerization(ATRP).Characterization of the product by gel permeation chromatography(GPC),infrared,nuclear magnetic;obtained at a temperature of 95℃,n(tBA)/n(PSt-Cl)/n(CuBr)/n(bpy)=100 :1 :1 :2,when the reaction time was 28 h,the molecular weight of PSt-b-PtBA was 11261,and the molecular weight distribution(PDI)was 1.43.
引文
[1]Gokhan A,Muhammet U.K,Yusuf Y.Synthesis of Block Copolymers by Combination of Atom Transfer Radical Polymerization and Visible LightRadicalPhotopolymerizationMethods[J].Macromolecules,2010,43:9198–9201.
[2]王媚,林文静,黄海亮,等.ATRP以及ATRP法制备嵌段共聚物研究进展综述[J].化工技术与开发,2010,9(39):18-22.
[3]WangJS,MatyjaszewskiK.Control1ed“Living”Radical Polymerization.Atom Transfer Radical Polymeriza-tion in the Presence ofTransition-MetalComplexes[J].J AmChemSoc,1995;117:5614-5615.
[4]牟博,雷忠利,杨红,等.PS-b-PNIPAM?Ag复合微粒的制备与表征[J].物理化学学报,2009,25(11):2399-2403.
[2]王媚,林文静,黄海亮,等.ATRP以及ATRP法制备嵌段共聚物研究进展综述[J].化工技术与开发,2010,9(39):18-22.
[3]WangJS,MatyjaszewskiK.Control1ed“Living”Radical Polymerization.Atom Transfer Radical Polymeriza-tion in the Presence ofTransition-MetalComplexes[J].J AmChemSoc,1995;117:5614-5615.
[4]牟博,雷忠利,杨红,等.PS-b-PNIPAM?Ag复合微粒的制备与表征[J].物理化学学报,2009,25(11):2399-2403.