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Controlled synthesis and characterization of poly[methyl(3,3,3-trifluoropropyl)siloxane] with selective end groups†
RSC Advances ( IF 3.9 ) Pub Date : 2014-10-24 00:00:00 , DOI: 10.1039/c4ra12268b
Hua-Feng Fei 1, 2, 3, 4, 5 , Wenchun Xie 1, 2, 3, 4 , Qian Wang 1, 2, 3, 4 , Xiyin Gao 1, 2, 3, 4, 5 , Tao Hu 1, 2, 3, 4, 5 , Zhijie Zhang 1, 2, 3, 4 , Zemin Xie 1, 2, 3, 4
Affiliation  

Anionic ring-opening polymerization of 1,3,5-tris(trifluoropropylmethyl)cyclotrisiloxane in the bulk was studied using dilithium diphenylsilanediolate as an initiator (I); and N,N-dimethylformamide (DMF), bis(2-methoxyethyl)ether (Diglyme), and 1,2-dimethoxyethane (DME) as promoters (P). A detailed study on the kinetics of polymerization with different molar ratios of promoter to initiator ([P]/[I]) that were equal to 2.0, 4.0, and 6.0 revealed that the yield of linear polymers was the highest when [P]/[I] = 2.0 for all the promoters, among which DME was the most efficient promoter for suppressing the backbiting reactions. The reaction promoted by DME had a very broad “termination window” with the highest yield of linear polymer and very narrow molar mass distribution. The results of the matrix-assisted laser desorption/ionization time of flight mass spectrometry indicated that the intermolecular redistribution occurred during the process of polymerization. PMTFPS with end groups such as vinyl, hydroxyl, hydrogen and chloromethyl were prepared and characterized by 1H NMR, 29Si NMR and FT-IR. Polymers having vinyl end groups displayed higher thermo stability than those having hydroxyl end groups under nitrogen.

中文翻译:

控制合成和聚表征[甲基(3,3,3-三氟丙基)硅氧烷]具有选择性端基

以二苯基硅烷二醇二锂二锂为引发剂,研究了本体的1,3,5-三(三氟丙基甲基)环三硅氧烷的阴离子开环聚合反应。和NN-二甲基甲酰胺(DMF),双(2-甲氧基乙基)醚(Diglyme)和1,2-二甲氧基乙烷(DME)作为促进剂(P)。对促进剂与引发剂的摩尔比([P] / [I])分别为2.0、4.0和6.0的聚合动力学进行的详细研究表明,当[P] /对于所有启动子,[I] = 2.0,其中DME是抑制回位反应的最有效启动子。DME促进的反应具有非常宽的“终止窗口”,具有最高的线性聚合物收率和非常窄的摩尔质量分布。基质辅助激光解吸/电离飞行时间质谱的结果表明,分子间的重新分布发生在聚合过程中。具有末端基团(例如乙烯基,羟基,1 H NMR, 29 Si NMR和FT-IR。在氮气下,具有乙烯基端基的聚合物显示出比具有羟基端基的聚合物更高的热稳定性。
更新日期:2014-10-24
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