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t-BuOK

JOURNAL OF POLYMER SCIENCE PART A-POLYMER CHEMISTRY · 2019 ·Vol. 57 ·期 10 ·1130-1139 · IF 2.591

Anionic living polymerization of alkyl methacrylate at ambient temperature and its mechanism research

Zheng Li,Jianding Chen,Guijin Zou,Tongyuan Zhang,Dafu Wei,Xiang Xu,Yong Guan,Anna Zheng

In order to break through the bottleneck of anionic polymerization, polar monomers such as methyl methacrylate (MMA), ethyl methacrylate, butyl methacrylate, and hexyl methacrylate are subjected to anionic polymerization at room temperature in tetrahydrofuran (THF) using potassium tert -butoxide ( t -BuOK) as the initiator. The polymerization of alkyl methacrylates is studied by multidetector gel permeation chromatography, proton nuclear magnetic resonance ( 1 H-NMR) and 13 C-NMR spectroscopy, and dynamic laser light scattering. It is found that t -BuOK can initiate the living anionic polymerization of polar alkyl methacrylate, and the polymerization conversion almost reaches up to 100%. t -BuOK exists into two kinds of agglomerates, whose hydrodynamic volumes are 10 and 80 nm, respectively. t -BuOK in THF is similar to emulsion and has a critical active species concentration of about 0.0265 mol L −1 and does not depend on how much t -BuOK is added. After the initiation of the polymerization, the large agglomerates of a loose and less regular structure that have occupied the main part of t -BuOK are greatly reduced, but they do not continue to decrease until they disappear according to the equilibrium theory. Similarly, the active chain after initiation also will not aggregate again. Furthermore, t -BuOK also has an active species with smaller average vibration size between cation and anion pairs, which can only initiate the polymerization of MMA with rather slow rate but cannot initiate other alkyl methacrylates. At last, because t -BuOK can make the dormant species caused by side reactions to be revived, the anionic polymerization of MMA could obtain a high yield. © 2019 Wiley Periodicals, Inc. J. Polym. Sci., Part A: Polym. Chem. 2019 , 57, 1130–1139

CAS / MDL: 1428-95-1

研究领域: 高分子化学 · 材料科学

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RSC Advances · 2017 ·Vol. 7 ·期 85 ·53996-54001 · IF 3.108

Synthesis of poly(n-hexyl methacrylate)-b-poly(methyl methacrylate) via anionic polymerization with t-BuOK as the initiator at ambient temperature

Anna Zheng,Ling Su,Zheng Li,Guijin Zou,Xiang Xu,Yong Guan

To break through the industrial development bottlenecks of anionic polymerization in the field of polar monomers, poly n-hexyl methacrylate (PHMA) was prepared at 0 °C, 30 °C, and 60 °C with potassium tert-butoxide (t-BuOK) as the initiator in tetrahydrofuran (THF) and the conversions were almost complete. Gel permeation chromatography (GPC) analysis of poly n-hexyl methacrylate indicated that t-BuOK existed in numerous states when dissolved in THF, including different types of association and ion-pairs. A series of block copolymers of n-hexyl methacrylate (n-HMA) and methyl methacrylate (MMA), PMMA-b-PHMA (Mn 8200–16 200) and PHMA-b-PMMA (Mn 19 100–9500) were synthesized at 0 °C, and conversions were close to 100%. The results of dynamic mechanical analysis (DMA) indicated that there were two glass transition temperatures, −10 to 0 °C for the PHMA block and 100 to 110 °C for the PMMA block. Furthermore, the competing behaviors of n-HMA and MMA in copolymerization were investigated by one-shot feeding of two types of monomers at 0 °C, 30 °C, and 60 °C. The kinetics curves and 13C-NMR analysis of the copolymers indicated that the polymerization of n-HMA in the copolymerization was significantly dominant over that of MMA at set temperatures. The results in this study provided the possibility to realize anionic polymerization of methacrylate esters on a commercial scale.

CAS / MDL: 142-09-6

研究领域: 高分子化学 · 材料科学

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