Study of a new titanium dual initiator for the synthesis of poly(epsilon-caprolactone)-b-polystyrene block copolymers by the combination of coordination and nitroxide mediated polymerizations

Li XX; Jeanmaire T; Zerroukhi A

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Study of a new titanium dual initiator for the synthesis of poly(epsilon-caprolactone)-b-polystyrene block copolymers by the combination of coordination and nitroxide mediated polymerizations

机译：配位和氮氧化物介导的聚合反应合成聚（ε-己内酯）-b-聚苯乙烯嵌段共聚物的新型钛双引发剂的研究

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Poly epsilon-caprolactone-polystyrene blockcopolymers (PCL-b-PSt) were synthesized using a modified titanium catalyst as the dual initiator. Alcoholysis of Ti(OPr)(4) by 4-hydroxy 2,2,6,6 tetramethyl piperidinyl-loxyl (HO-TEMPO) gave a bifunctional initiator Ti(OTEMPO)(4). Poly epsilon-caprolactone prepolymer end-capped with the nitroxide group was first prepared by ring opening polymerization of epsilon-caprolactone with this initiator at high conversion. The nitroxide-end-capped structure and molar mass (M-n) of the polymers were demonstrated by typical UV absorption band. This analytical technique indicates a near-quantitative nitroxide functionality and a M-n in good agreement with size exclusion chromatography (SEC) ones. This polyester prepolymer was used to further initiate the radical polymerization with styrene and reach the block copolymers (PCL-b-PSt). All the prepolymers and block copolymers were characterized by SEC and NMR spectroscopy. Additionally, the preparation of star polymers bearing two kinds of arms (PCL and PSt) was envisaged and a preliminary result was given. (c) 2007 Wiley Periodicals, Inc.

机译：使用改性钛催化剂作为双引发剂合成了聚ε-己内酯-聚苯乙烯嵌段共聚物（PCL-b-PSt）。 Ti（OPr）（4）被4-羟基2,2,6,6四甲基哌啶基-己基（HO-TEMPO）醇解得到双功能引发剂Ti（OTEMPO）（4）。首先通过使ε-己内酯与该引发剂在高转化率下开环聚合来制备被氮氧基封端的聚ε-己内酯预聚物。通过典型的UV吸收带证明了聚合物的氮氧化物封端结构和摩尔质量（M-n）。该分析技术表明氮氧化物的功能接近定量，并且M-n与尺寸排阻色谱法（SEC）高度吻合。该聚酯预聚物用于进一步引发与苯乙烯的自由基聚合，并达到嵌段共聚物（PCL-b-PSt）。所有预聚物和嵌段共聚物都通过SEC和NMR光谱进行了表征。另外，设想了制备具有两种臂（PCL和PSt）的星形聚合物，并给出了初步结果。（c）2007年Wiley Periodicals，Inc.

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《Journal of Applied Polymer Science》 |2008年第6期|共8页
作者
Li XX; Jeanmaire T; Zerroukhi A;
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正文语种 eng
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ring opening polymerization; block copolymers; nitroxide; dual initiator; RING-OPENING POLYMERIZATION; RELEASE; OXIDE);

机译：开环聚合;嵌段共聚物;氮氧化物;双引发剂;开环聚合;释放;氧化物;

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1. Study of a new titanium dual initiator for the synthesis of poly(epsilon-caprolactone)-b-polystyrene block copolymers by the combination of coordination and nitroxide mediated polymerizations [J] . Li XX, Jeanmaire T, Zerroukhi A Journal of Applied Polymer Science . 2008,第6期

机译：配位和氮氧化物介导的聚合反应合成聚（ε-己内酯）-b-聚苯乙烯嵌段共聚物的新型钛双引发剂的研究
2. Synthesis of Poly(n-butyl acrylate)-b-poly(epsilon-caprolactone) through Combination of SG1 Nitroxide-Mediated Polymerization and Sn(Oct)(2)-Catalyzed Ring-Opening Polymerization: Study of Sequential and One-Step Approaches from a Dual Initiator [J] . Chagneux N, Trimaille T, Rollet M, Macromolecules . 2009,第24期

机译：SG1一氧化氮介导的聚合反应和Sn（Oct）（2）催化的开环聚合反应合成聚丙烯酸正丁酯-ε-己内酯双启动器
3. Synthesis of AB(2) 3- and AB(4) 5-miktoarm star copolymers initiated from dendritic tri- and penta- functional initiators by combination of ring-opening polymerization of epsilon-caprolactone and nitroxide-mediated radical polymerization of styrene [J] . Miura Y, Sakai Y, Yamaoka K Macromolecular chemistry and physics . 2005,第4期

机译：由树状三官能和五官能引发剂引发的ε（ε）-己内酯的开环聚合反应和苯乙烯的氮氧化物介导的自由基聚合反应的合成，合成AB（2）3-和AB（4）5-微星共聚物
4. Study of the Compartmentalization Effect in Nitroxide-Mediated Controlled Free-Radical Emulsion Polymerization with in Situ Formation of Poly(Acrylic Acid)-b- Polystyrene Amphiphilic Block Copolymers [C] . Bernadette Charleux, Guillaume Delaittre PMSE Symposia . 2008

机译：用（丙烯酸）-B-聚苯乙烯两亲嵌段共聚物原位形成氮氧化物介导的自由基乳液聚合中的分区化作用研究
5. Nitroxide mediated polymerization: Microemulsion of n-butyl acrylate and the synthesis of block copolymers. [D] . Li, Wing Sze Jennifer. 2012

机译：一氧化氮介导的聚合反应：丙烯酸正丁酯的微乳液和嵌段共聚物的合成。
6. Synthesis and Self-Assembly of Poly(N-Vinylcaprolactam)-b-Poly(ε-Caprolactone) Block Copolymers via the Combination of RAFT/MADIX and Ring-Opening Polymerizations [O] . Rodolfo M. Moraes, Layde T. Carvalho, Gizelda M. Alves, 2020

机译：RAFT / MADIX和开环聚合反应合成聚（N-乙烯基己内酰胺）-b-聚（ε-己内酯）嵌段共聚物并进行自组装
7. A well-defined block copolymer synthesis via living cationic polymerization and nitroxide-mediated polymerization using carboxylic acid-based alkoxyamines as a dual initiator [O] . Le, Dao, Phan, Trang N. T., Autissier, Laurent, 2016

机译：通过活性阳离子聚合和以羧酸为基础的烷氧基胺为双引发剂的硝基氧介导的聚合反应，可以精确定义嵌段共聚物
8. Polymerization of epsilon-Caprolactone in the Presence of OH- or COOH-GroupsContaining Initiators. Copolymers of Lactide with epsilon-Caprolactone: Synthesis, Characterization and Processing [R] . Karjalainen, T., Hiljanen, M. 1994

机译：在含OH-或COOH-基团的引发剂存在下聚ε-己内酯的聚合。丙交酯与ε-己内酯的共聚物：合成，表征和加工

Study of a new titanium dual initiator for the synthesis of poly(epsilon-caprolactone)-b-polystyrene block copolymers by the combination of coordination and nitroxide mediated polymerizations

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