Polyester from dimethylketene and acetaldehyde: Direct copolymerization and β‐lactone ring‐opening polymerization

Polyester from dimethylketene and acetaldehyde: Direct copolymerization and β‐lactone ring‐opening polymerization
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二甲基乙烯酮和乙醛聚酯:直接共聚和β-内酯开环聚合

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发表时间:
2011
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通讯作者:
C. Bunel
C. Bunel
中科院分区:
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文献类型:
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作者:
Marc Brestaz;N. Desilles;Guillaume Lê;C. Bunel

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研究了以二甲基乙烯酮和乙醛为原料合成脂肪族聚酯的两种方法。一方面,在-60 °C的甲苯中进行直接阴离子共聚。所得聚合物主要由PE单元组成。另一方面,一个两步法,包括通过[2+2]环加成合成3,3,4-三甲基-2-氧杂环丁烷酮,然后其开环聚合,与各种引发剂和溶剂,导致预期的PE。获得了高达9000 g mol-1的分子量(通过核磁共振(NMR)测量),具有约1.2的窄的多分散性。发现这些聚合物在氮气下在高达274 °C下是稳定的,并且通过差示扫描量热法(DSC)在139 °C附近观察到归因于结晶度的宽且复杂的吸热峰。通过X射线衍射测量的结晶度接近0.45。© 2011 Wiley Periodicals,Inc.聚合物科学杂志A部分:聚合物化学,2011年
Two ways to obtain aliphatic polyesters (PEs) from dimethylketene and acetaldehyde were investigated. On the one hand, a direct anionic copolymerization was carried out in toluene at −60 °C. The resulting polymer was mainly composed of PE units. On the other hand, a two-step process involving the synthesis of 3,3,4-trimethyl-2-oxetanone by [2+2] cycloaddition, followed by its ring-opening polymerization, with various initiators and solvents, led to the expected PE. Molecular weights up to 9000 g mol−1 (measured by nuclear magnetic resonance (NMR)), with narrow polydispersity around 1.2, were obtained. These polymers were found stable up to 274 °C under nitrogen and a broad and complex endothermic peak attributed to crystallinity was observed near 139 °C by differential scanning calorimetry (DSC). The crystallinity, measured by X-ray diffraction, was close to 0.45. © 2011 Wiley Periodicals, Inc. J Polym Sci Part A: Polym Chem, 2011