Chem. J. Chinese Universities ›› 2017, Vol. 38 ›› Issue (9): 1687.doi: 10.7503/cjcu20170037
• Polymer Chemistry • Previous Articles Next Articles
HUANG Haihong*(), ZHANG Baoyu, ZHAO Zhipei
Received:
2017-01-16
Online:
2017-09-10
Published:
2017-08-25
Contact:
HUANG Haihong
E-mail:huanghaihong@hfut.edu.cn
Supported by:
CLC Number:
TrendMD:
HUANG Haihong, ZHANG Baoyu, ZHAO Zhipei. Degradation and Characterization of Recycling Carbon Fiber/Epoxy Resin Composites in Supercritical n-Butanol†[J]. Chem. J. Chinese Universities, 2017, 38(9): 1687.
Fig.1 CF/EP before degradation and products after degradation(A) CF/EP before degradation; (B) solid residue of CF/EP after degradation; (C) liquid residue of CF/EP after degradation.
Code | Process parameter | Level | ||||
---|---|---|---|---|---|---|
-2 | -1 | 0 | 1 | 2 | ||
A | Reaction temperature/℃ | 290 | 300 | 310 | 320 | 330 |
B | Holding time/min | 20 | 30 | 40 | 50 | 60 |
C | cKOH/(mol·L-1) | 0.02 | 0.03 | 0.04 | 0.05 | 0.06 |
D | V(n-Butanol)/mL | 400 | 425 | 450 | 475 | 500 |
Table 1 Process parameters and levels
Code | Process parameter | Level | ||||
---|---|---|---|---|---|---|
-2 | -1 | 0 | 1 | 2 | ||
A | Reaction temperature/℃ | 290 | 300 | 310 | 320 | 330 |
B | Holding time/min | 20 | 30 | 40 | 50 | 60 |
C | cKOH/(mol·L-1) | 0.02 | 0.03 | 0.04 | 0.05 | 0.06 |
D | V(n-Butanol)/mL | 400 | 425 | 450 | 475 | 500 |
Source | Sum of squares | Degree of freedom | F-value | P-value>F-value | Significance |
---|---|---|---|---|---|
Relation | 0.066 | 12 | 19.53 | <0.0001 | Significant |
A | 4.773×10-3 | 1 | 16.87 | 0.0007 | Significant |
B | 0.011 | 1 | 38.60 | <0.0001 | Significant |
C | 5.367×10-3 | 1 | 18.97 | 0.0004 | Significant |
D | 6.055×10-4 | 1 | 2.14 | 0.1608 | Significant |
AC | 1.830×10-3 | 1 | 6.47 | 0.0204 | Significant |
CD | 4.442×10-4 | 1 | 1.57 | 0.2263 | Not significant |
B2 | 3.353×10-3 | 1 | 11.85 | 0.0029 | Significant |
C2 | 1.273×10-3 | 1 | 4.50 | 0.0480 | Significant |
BCD | 1.051×10-3 | 1 | 3.72 | 0.0698 | Not significant |
A2B | 4.726×10-3 | 1 | 16.70 | 0.0007 | Significant |
A2D | 1.287×10-3 | 1 | 4.55 | 0.0470 | Significant |
AB2 | 2.735×10-3 | 1 | 9.66 | 0.0061 | Significant |
Residual | 5.093×10-3 | 18 | |||
Lack of fit | 4.109×10-3 | 12 | 2.09 | 0.1884 | Not significant |
Pure error | 9.843 | 6 |
Table 2 Analysis of variance for established mathematical model
Source | Sum of squares | Degree of freedom | F-value | P-value>F-value | Significance |
---|---|---|---|---|---|
Relation | 0.066 | 12 | 19.53 | <0.0001 | Significant |
A | 4.773×10-3 | 1 | 16.87 | 0.0007 | Significant |
B | 0.011 | 1 | 38.60 | <0.0001 | Significant |
C | 5.367×10-3 | 1 | 18.97 | 0.0004 | Significant |
D | 6.055×10-4 | 1 | 2.14 | 0.1608 | Significant |
AC | 1.830×10-3 | 1 | 6.47 | 0.0204 | Significant |
CD | 4.442×10-4 | 1 | 1.57 | 0.2263 | Not significant |
B2 | 3.353×10-3 | 1 | 11.85 | 0.0029 | Significant |
C2 | 1.273×10-3 | 1 | 4.50 | 0.0480 | Significant |
BCD | 1.051×10-3 | 1 | 3.72 | 0.0698 | Not significant |
A2B | 4.726×10-3 | 1 | 16.70 | 0.0007 | Significant |
A2D | 1.287×10-3 | 1 | 4.55 | 0.0470 | Significant |
AB2 | 2.735×10-3 | 1 | 9.66 | 0.0061 | Significant |
Residual | 5.093×10-3 | 18 | |||
Lack of fit | 4.109×10-3 | 12 | 2.09 | 0.1884 | Not significant |
Pure error | 9.843 | 6 |
No. | Reactor temperature/℃ | Holding time/min | Additive concentration/ (mol·L-1) | V(n-Butanol)/ mL | Actual degradation rate(%) | Theoretical degradation rate(%) | Error (%) |
---|---|---|---|---|---|---|---|
1 | 330 | 40 | 0.04 | 443 | 98.82 | 99.20 | -0.38 |
2 | 300 | 50 | 0.04 | 450 | 91.19 | 88.90 | 2.58 |
3 | 320 | 20 | 0.04 | 500 | 92.98 | 98.34 | -5.45 |
4 | 330 | 60 | 0.03 | 430 | 99.59 | 101.50 | -1.91 |
5 | 310 | 50 | 0.05 | 430 | 97.23 | 96.98 | 0.25 |
6 | 300 | 60 | 0.04 | 500 | 80.12 | 77.94 | -2.18 |
Table 3 Experiments of process parameters to verify the mathematical model
No. | Reactor temperature/℃ | Holding time/min | Additive concentration/ (mol·L-1) | V(n-Butanol)/ mL | Actual degradation rate(%) | Theoretical degradation rate(%) | Error (%) |
---|---|---|---|---|---|---|---|
1 | 330 | 40 | 0.04 | 443 | 98.82 | 99.20 | -0.38 |
2 | 300 | 50 | 0.04 | 450 | 91.19 | 88.90 | 2.58 |
3 | 320 | 20 | 0.04 | 500 | 92.98 | 98.34 | -5.45 |
4 | 330 | 60 | 0.03 | 430 | 99.59 | 101.50 | -1.91 |
5 | 310 | 50 | 0.05 | 430 | 97.23 | 96.98 | 0.25 |
6 | 300 | 60 | 0.04 | 500 | 80.12 | 77.94 | -2.18 |
Fig.2 Effect of different process parameters on degradation rate(A) t=40 min, c=0.04 mol/L; (B) temperature=310 ℃, L= 450 mL; (C) c=0.04 mol/L, L= 450 mL;(D) t=40 min, temperature=310 ℃.
No. | Reaction temperature/℃ | Holding time/ min | c(Additive)/ (mol·L-1) | V(n-Butanol)/ mL | Actual degradation rate(%) | Theoretical degradation rate(%) |
---|---|---|---|---|---|---|
1 | 330 | 60 | 0.0538 | 413 | 100.69 | 100.00 |
2 | 330 | 60 | 0.0538 | 413 | 98.17 | |
3 | 330 | 60 | 0.0538 | 413 | 99.50 | |
4 | 330 | 60 | 0.0538 | 413 | 98.71 | |
5 | 330 | 60 | 0.0538 | 413 | 100.40 | |
6 | 330 | 60 | 0.0538 | 413 | 99.87 |
Table 4 Experiments under the optimal process parameters
No. | Reaction temperature/℃ | Holding time/ min | c(Additive)/ (mol·L-1) | V(n-Butanol)/ mL | Actual degradation rate(%) | Theoretical degradation rate(%) |
---|---|---|---|---|---|---|
1 | 330 | 60 | 0.0538 | 413 | 100.69 | 100.00 |
2 | 330 | 60 | 0.0538 | 413 | 98.17 | |
3 | 330 | 60 | 0.0538 | 413 | 99.50 | |
4 | 330 | 60 | 0.0538 | 413 | 98.71 | |
5 | 330 | 60 | 0.0538 | 413 | 100.40 | |
6 | 330 | 60 | 0.0538 | 413 | 99.87 |
Species | C(%) | O(%) | N(%) | Si(%) | K(%) | O/C |
---|---|---|---|---|---|---|
Original carbon fiber | 77.96 | 20.29 | 1.09 | 0.66 | 0 | 0.260 |
Recycled carbon fiber | 78.46 | 16.70 | 1.86 | 1.71 | 1.27 | 0.213 |
Table 5 Elemental composition of carbon fibers from XPS spectra
Species | C(%) | O(%) | N(%) | Si(%) | K(%) | O/C |
---|---|---|---|---|---|---|
Original carbon fiber | 77.96 | 20.29 | 1.09 | 0.66 | 0 | 0.260 |
Recycled carbon fiber | 78.46 | 16.70 | 1.86 | 1.71 | 1.27 | 0.213 |
Species | Comporition(%) | ||||
---|---|---|---|---|---|
C—C | C—OH | C | COOH | C | |
Original carbon fiber | 67.93 | 29.13 | 1.45 | 0.48 | 0.99 |
Recycled carbon fiber | 33.76 | 44.74 | 18.74 | 1.23 | 1.53 |
Table 6 Oxygen functional groups of carbon fibers from XPS spectra
Species | Comporition(%) | ||||
---|---|---|---|---|---|
C—C | C—OH | C | COOH | C | |
Original carbon fiber | 67.93 | 29.13 | 1.45 | 0.48 | 0.99 |
Recycled carbon fiber | 33.76 | 44.74 | 18.74 | 1.23 | 1.53 |
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