Sample Name: Poly( methylmethacrylate-b-2-hydroxy ethyl methacxrylate) 1H-NMR Spectrum of the block copolymer: Sample #: P5699 P56995699-MMAHEMA Structure: CH3 CH 3 CH 2 C C CH2 n O C C O O CH 3 CH2 n O CH2 OH SEC of the block copolymer: copolymer: Composition: Mn × 103 MMA-b-HEMA 24.0-b-17.0 1.09 Tg for MMA block: 116 oC Synthesis Procedure: Poly(Methyl methacrylate-b-2-hydroxy ethyl methacrylate) block copolymer is synthesized by living anionic polymerization with sequence addition of methyl methacrylate followed by addition of protecting hydroxyl HEMA (trimethyl siloxy ethyl methacrylate monomer). The obtained polymer was precipitation in methnol/acidic to deprotect the hydroxyl group. Characterization: Polymer was analyzed by size exclusion chromatography (SEC) to obtain the molecular weight and polydispersity index (PDI). The final block copolymer composition was calculated from HNMR. Thermal analysis Thermal analysis of the samples was carried out on a TA Q100 differential scanning calorimeter at a heating rate of 10oC/min.The midpoint of the slope change of the heat flow plot of the second heating scan was considered as the glass transition temperature (Tg). -0 8 10 12 14 16 18 20 22 24 26 28 30 V e ( m l) P o ly ( m e th y l m e th a c r y la te ) M n = 2 4 0 0 0 , M w = 2 6 0 0 0 , P I= 1 .0 5 B l o c k C o p o ly m e r P M M A (2 4 0 0 0 ) -b - P H E M A - T M S ( 2 7 0 0 0 ) ,P I= 1 .0 9 V a l u e s fr o m L ig h t S c a tte r in g ( V i s c o te c k T r ip le d e te c to r ) : M w : 5 7 , 0 0 0 d n /d c : 0 .0 8 5 m l /g i n T H F a t 3 5 o C : R g w : 8 .4 9 n m A fte r d e p r o te c tio n o f O H g r o u p : P M M A - b -H E M A : M n 2 4 ,0 0 0 - b - 1 7 ,0 0 0 DSC thermogram for the MMA block: -0.36 -0.38 107.39°C -0.40 Heat Flow (W/g) Tg for HEMA block: Not distinct (Homopolymer: 85oC for 20k) P 5 6 9 9 -M M A H E M A PDI -0.42 115.67°C(T) -0.44 Solubility: Polymer is soluble in DMF. 122.66°C -0.46 -0.48 80 Exo Up 90 100 110 120 Temperature (°C) 130 140 150 Universal V4.2E TA Instruments
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