p5699-mmahema - Polymer Source

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