Sample Name: Poly(styrene-b-2-vinyl pyridinetert butylmethacrylate)
bearing ethynyl (acetylenic triple bond) phenyl –
phenyl ethylene at the junction of S-2VP block
Sample #: P19077-S(acetylene) 2VPtBuMA
H NMR:
Structure:
CH3
H3 C
CH
CH2
CH
CH2
CH2
C
H2
C
CH
C
H
X
n
n
CH2
C
H3 C
O
N
C
O
HC
C
H3 C
CH3
CH3
Composition: tBuMA: nBuMA 1:1ratio
Mn x 103
PDI
S-b-2VP-b-tBuMA
54.0-b-48.0-b-218.0
1.15
By HNMR
Tg: oC
101:119:124
S:2VP:tBuMA
Synthesis Procedure:
By anionic Process
H3 C
CH
CH2
Li
CH
H3C
n
CH
CH2
CH
Li
H2 C
C
n
CH2
CH2
H3C
H3 C
C
CH3
C
Si
C
H3C
CH3
CH3
CH3
CH2 CH
m
H3 C
CH
CH2
CH
CH2
C
N
Li
H3 C
n
CH
CH2
CH2
CH
CH2
CH2
C
CH
Li
n
n
H3 C
CH2
C
H3 C
CH3
N
C
C
Si
H3C
C
CH3
CH3
H2C
1H-NMR
C
H3C Si
CH3
C
CH3
H3C
CH3
CH3
CH3
Spectrum of the polymer
C
C
O
O
C
H3 C
CH3
CH3
CH3
H3C
CH
CH2
CH
CH2
CH2
C
H2
C
CH
C
H
X
n
n
CH2
C
H3C
O
N
C
O
C
H3C Si CH
3
C
H3 C
CH3
CH3
C
H3C
CH3
CH3
Deprotection
CH3
H3 C
CH
CH2
CH
CH2
CH2
C
H2
C
CH
C
H
X
n
n
CH2
C
H3 C
O
N
C
O
HC
C
H3C
CH3
CH3
Characterization:
By SEC and HNMR spectroscopy.
DPE-4Br:
The product was characterized by NMR and FTIR.
v.A-1
SEC for the polymer at different stages:
DSC:
Sample: P19077-1
Size: 9.0000 mg
File: P19077.002
DSC
Heat Flow (W/g)
-0.1
97.95°C
101.71°C(H)
0.09672J/(g·°C)
105.45°C
119.58°C
124.32°C(H)
0.1129J/(g·°C)
128.94°C
-0.3
60
Exo Up
110
Temperature (°C)
160
Universal V4.5A TA Instruments
Concentration (mg/mL)
2.0383
Sample dn/dc (mL/g)
0.1140
Method File
PS80K-Jan22-2015-0000.vcm
Column Set
3x PL 1113-6300
Solvent
THF
60.00
40.00
20.00
-0.00
79.57
89.17
300.00
63.65
71.33
240.00
47.74
53.50
31.83
35.67
15.91
17.83
60.00
0.00
0.00
0.00
8.0010.00
P19077-S2VPtBuMA_01.vdt:
12.00 14.00
16.00 18.00 20.00 22.00
Retention Volume (mL)
Refractive Index
24.00 26.00
Viscometer - DP(mV)
Refractive Index (mV)
80.00
Low Angle Light Scattering (mV)
100.00
180.00
120.00
Right Angle Light Scattering (mV)
Sample ID: P19077-S2VPtBuMA
28.00
30.00
Right Angle Light Scattering
Low Angle Light Scattering
Viscometer - DP
Sample
MW Number
Average (Da)
MW Weight
Average (Da)
MW at Peak
(Da)
Polydispersity Intrinsic
Viscosity
(dL/g)
P19077-S2VPtBuMA_01.vdt
321,293
369,446
376,990
1.150
1.6828
v.A-1