Chem. J. Chinese Universities ›› 2015, Vol. 36 ›› Issue (7): 1422.doi: 10.7503/cjcu20150174
• Polymer Chemistry • Previous Articles Next Articles
WANG Min, GE Hao, SONG Jianhui, XU Min*()
Received:
2015-03-03
Online:
2015-07-10
Published:
2015-06-05
Contact:
XU Min
E-mail:xumin@phy.ecnu.edu.cn
Supported by:
CLC Number:
TrendMD:
WANG Min, GE Hao, SONG Jianhui, XU Min. Solid-state NMR Study on the Dynamics of Thermo-sensitive Cellulose/Poly(N-isopropylacrylamide) Composite Hydrogel†[J]. Chem. J. Chinese Universities, 2015, 36(7): 1422.
Fig.4 Solid-state 13C CP/MAS NMR spectra of neat PNIPAM(a), neat cellulose(b) and CL/PNIPAM composite polymer(c)The peaks labeled with “*” are sidebands.
Sample | tCDP/μs | η(C5,6) | η(C1'—C6') | n(AGU)/n(NIPAM) |
---|---|---|---|---|
2%C/PNP | 200 | 1.28 | 1.27 | 0.96 |
4%C/PNP | 200 | 1.83 | 1.85 | 0.80 |
6%C/PNP | 100 | 1.72 | 2.23 | 0.73 |
200 | 2.46 | 2.33 | 0.72 | |
8%C/PNP | 200 | 1.40 | 1.37 | 0.69 |
10%C/PNP | 200 | 1.90 | 1.83 | 0.67 |
Table 1 Quantitative results of cellulose/PNIPAM from QCP NMR*
Sample | tCDP/μs | η(C5,6) | η(C1'—C6') | n(AGU)/n(NIPAM) |
---|---|---|---|---|
2%C/PNP | 200 | 1.28 | 1.27 | 0.96 |
4%C/PNP | 200 | 1.83 | 1.85 | 0.80 |
6%C/PNP | 100 | 1.72 | 2.23 | 0.73 |
200 | 2.46 | 2.33 | 0.72 | |
8%C/PNP | 200 | 1.40 | 1.37 | 0.69 |
10%C/PNP | 200 | 1.90 | 1.83 | 0.67 |
Label of peak | δ | Fitting area(%) | Attribution | Label of peak | δ | Fitting area(%) | Attribution |
---|---|---|---|---|---|---|---|
1 | -0.30 | 1.65 | Few impurity | 5 | 3.83 | 7.56 | b |
2 | 1.05 | 46.21 | a | 6 | 4.78 | 5.54 | H2O |
3 | 1.95 | 25.36 | c,d | 7 | 5.65 | 5.77 | CL |
4 | 2.80 | 7.91 | CL |
Table 2 Nonlinear least squares fitting(NLSF)results of static 1H NMR spectra of CL/PNIPAM composite gel*
Label of peak | δ | Fitting area(%) | Attribution | Label of peak | δ | Fitting area(%) | Attribution |
---|---|---|---|---|---|---|---|
1 | -0.30 | 1.65 | Few impurity | 5 | 3.83 | 7.56 | b |
2 | 1.05 | 46.21 | a | 6 | 4.78 | 5.54 | H2O |
3 | 1.95 | 25.36 | c,d | 7 | 5.65 | 5.77 | CL |
4 | 2.80 | 7.91 | CL |
Temperature/K | Δδ | Fitting area(%) | ||
---|---|---|---|---|
Wide peak | Narrow peak | Wide peak | Narrow peak | |
298 | 145.94 | 3.62 | 26.82 | 73.18 |
304 | 142.68 | 3.63 | 27.20 | 72.80 |
306 | 115.08 | 4.60 | 41.65 | 58.35 |
307 | 100.98 | 6.50 | 56.52 | 43.48 |
308 | 93.85 | 6.91 | 63.35 | 36.65 |
310 | 88.46 | 6.60 | 68.28 | 31.72 |
312 | 85.39 | 6.26 | 70.70 | 29.30 |
Table 3 Gauss and Lorentz fitting results of static 1H NMR spectra of CL/PNIPAM gel at different temperature*
Temperature/K | Δδ | Fitting area(%) | ||
---|---|---|---|---|
Wide peak | Narrow peak | Wide peak | Narrow peak | |
298 | 145.94 | 3.62 | 26.82 | 73.18 |
304 | 142.68 | 3.63 | 27.20 | 72.80 |
306 | 115.08 | 4.60 | 41.65 | 58.35 |
307 | 100.98 | 6.50 | 56.52 | 43.48 |
308 | 93.85 | 6.91 | 63.35 | 36.65 |
310 | 88.46 | 6.60 | 68.28 | 31.72 |
312 | 85.39 | 6.26 | 70.70 | 29.30 |
Temperature/K | 298 | 302 | 304 | 305 | 306 | 307 | 308 | 310 |
---|---|---|---|---|---|---|---|---|
Intensity ratio | 4.5 | 4.2 | 4.1 | 4.4 | 5.5 | 4 | 3.8 | 3.8 |
Table 4 Static 1H NMR spectra of CL/PNIPAM gel at different temperatures before and after spin diffusion intensity ratio
Temperature/K | 298 | 302 | 304 | 305 | 306 | 307 | 308 | 310 |
---|---|---|---|---|---|---|---|---|
Intensity ratio | 4.5 | 4.2 | 4.1 | 4.4 | 5.5 | 4 | 3.8 | 3.8 |
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