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Synthesis of cyclohexanone formaldehyde resin-methylmethacrylate block-graft copolymers via ATRP

机译:ATRP法合成环己酮甲醛树脂-甲基丙烯酸甲酯嵌段接枝共聚物

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摘要

Well defined block-graft copolymers of cyclohexanone-formaldehyde resin (CFR) and methylmethacrylate (MMA) were prepared via atom transfer radical polymerization (ATRP). In the first step, cyclohexanone formaldehyde resin (CFR) containing hydroxyl groups were modified with 2-bromopropionyl bromide. Resulting multifunctional macroinitiator was used in the ATRP of MMA using copper bromide (CuBr) and N,N,N',N'',N''-pentamethyl-diethylenetriamine (PMDETA) as catalyst system at 90°C. The chemical composition and structure of the copolymers were characterized by nuclear magnetic resonance (~1H-NMR) spectroscopy, Fourier transform infrared (FTIR) spectroscopy, and molecular weight measurement. Molecular weight distributions of the CFR graft copolymers were measured by gel permeation chromatography (GPC). M_n values up to 19,000 associated with narrow molecular weight distributions (polydispersity index (PDI) < 1.6) were obtained with conversions up to 49%. Coating properties of synthesized graft copolymers such as adhesion and gloss values were measured. They exhibited good adhesion properties on Plexiglas substrate. The thermal behaviors of all polymers were conducted using differential scanning calorimetry (DSC) and thermogravimetric analysis (TGA).
机译:通过原子转移自由基聚合(ATRP)制备了定义明确的环己酮-甲醛树脂(CFR)和甲基丙烯酸甲酯(MMA)的嵌段接枝共聚物。在第一步中,将含有羟基的环己酮甲醛树脂(CFR)用2-溴丙酰溴进行改性。将得到的多功能大分子引发剂用于溴化铜(CuBr)和N,N,N',N'',N'',N''-五甲基二亚乙基三胺(PMDETA)作为催化剂体系的MMA催化剂,在90°C下使用。通过核磁共振(〜1H-NMR)光谱,傅立叶变换红外(FTIR)光谱和分子量测量来表征共聚物的化学组成和结构。通过凝胶渗透色谱法(GPC)测量CFR接枝共聚物的分子量分布。获得的M_n值高达19,000,与窄分子量分布(多分散指数(PDI)<1.6)相关,转化率高达49%。测量了合成接枝共聚物的涂层性能,如粘合力和光泽度。它们在有机玻璃基板上显示出良好的粘合性能。使用差示扫描量热法(DSC)和热重分析(TGA)进行所有聚合物的热行为。

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