Sample Name: Poly(styrene-b-2-vinyl pyridinetert butylmethacrylate-Butyl methacrylate ran)
bearing ethynyl (acetylenic triple bond) phenyl –
phenyl ethylene at the junction of S-2VP block
Sample #:
P19070-S(acetylene) 2VPtBuMAnBuMAran
H NMR:
Structure:
CH3
CH3
H3 C
CH
CH2
CH
CH2
CH2
C
H2
C
CH
H2
C
C
C
n
n
H
O
C
CH2
X
C
H3 C
N
O
O
C
CH2
O
H 2C
HC
C
H3 C
CH3
CH2
CH3
CH3
Composition: tBuMA: nBuMA 1:1ratio
Mn x 103
PDI
S-b-2VP-b-tBuMAnBuMA
49.0-b-44.0-b-165.0
1.08
HNMR
Tg: oC
101:119:68
S:2VP
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
1H-NMR
n
n
H3 C
CH2
C
H3 C
CH3
C
Si
H3C
Spectrum of the polymer
N
C
C
CH3
C
H3C Si
CH3
C
CH3
CH3
CH3
CH3
H3C
CH3
H2C
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
C
H3 C
H
X
n
n
CH2
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:
0.1850
Method File
PS80K-Jan22-2015-0000.vcm
Column Set
3x PL 1113-6300
Solvent
THF
216.18
73.92
154.07
172.94
59.14
123.25
44.35
92.44
129.71
86.47
29.57
61.63
43.24
14.78
30.81
0.00
0.00
Right Angle Light Scattering (mV)
4.8827
Sample dn/dc (mL/g)
Viscometer - DP(mV)
Refractive Index (mV)
Sample ID: P19070-1
Concentration (mg/mL)
0.00
15.00
17.00
P19070-1_01.vdt:
19.00 21.00
23.00 25.00 27.00 29.00
Retention Volume (mL)
Refractive Index
31.00 33.00
35.00
37.00
40.00
Right Angle Light Scattering
Viscometer - DP
Sample
MW Number
Average (Da)
MW Weight
Average (Da)
MW at Peak
(Da)
Polydispersity Intrinsic
Viscosity
(dL/g)
P19070-1_01.vdt
48,690
51,660
47,718
1.061
0.4793
Concentration (mg/mL)
6.4843
Sample dn/dc (mL/g)
0.1700
Method File
PS80K-Jan22-2015-0000.vcm
Column Set
3x PL 1113-6300
Solvent
THF
306.89
89.47
245.51
67.10
184.14
44.73
122.76
49.47
22.37
61.38
0.00
0.00
148.41
98.94
Visc ometer - DP (mV)
111.83
197.88
Refractive Index (mV)
247.35
Right Angle Light Scattering (mV)
Sample ID: P19070-S2VP
0.00
15.00
17.00 19.00 21.00 23.00 25.00 27.00 29.00 31.00 33.00 35.00 37.00 40.00
Retention Volume (mL)
P19070-2_01.vdt:
Refractive Index
Right Angle Light Scattering
Viscometer - DP
Sample
MW Number MW Weight MW at Peak
Average (Da) Average (Da) (Da)
PolydispersityIntrinsic
Viscosity
(dL/g)
P19070-2_01.vdt
99,454
1.058
105,222
99,478
0.5722
v.A-1