Preparation of Titania–Silica Composite Aerogel at Atmospheric Pressure and Its Catalytic Performance in the Synthesis of Poly (Butylene Succinate)
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Preparation of Titania–Silica Composite Aerogels
2.2.1. Pre-Hydrolysis of Tetraethyl Silicate
2.2.2. Preparation of Titania–Silica Composite Alcohol Gels
2.2.3. Preparation of Titania–Silica Composite Aerogels
2.3. Preparation of PBS
2.4. Characterization and Measurement
3. Results and Discussion
3.1. Surface Morphology and Structure of Titania–Silica Composite Aerogels
3.2. Catalytic Activity of Titania–Silica Composite Aerogels for the Polycondensation of PBS
3.3. Reaction Kinetics of PBS Polycondensation Catalyzed by Titania–Silica Aerogel
4. Conclusions
Author Contributions
Funding
Institutional Review Board Statement
Informed Consent Statement
Data Availability Statement
Conflicts of Interest
References
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Samples | SBET (m2/g) | Sext (m2/g) | Vtot (cm3/g) | Pore Size (nm) |
---|---|---|---|---|
TiO2-AG | 332.86 | 275.01 | 0.39 | 7.56 |
TS91 | 524.59 | 350.29 | 0.85 | 8.08 |
TS82 | 536.81 | 495.99 | 0.86 | 8.12 |
TS73 | 524.04 | 484.16 | 0.84 | 7.51 |
TS64 | 441.37 | 411.81 | 0.66 | 7.24 |
TS55 | 402.87 | 377.93 | 0.46 | 7.02 |
Samples | Element Content (atom.%) | |||
---|---|---|---|---|
Ti | Si | C | O | |
TS91 | 13.70 | 2.66 | 44.99 | 38.65 |
TS82 | 12.55 | 4.10 | 43.67 | 39.68 |
TS73 | 12.45 | 6.40 | 31.30 | 49.85 |
TS64 | 11.30 | 10.20 | 25.42 | 53.08 |
TS55 | 11.09 | 12.40 | 23.31 | 53.19 |
Samples | L Acid Content (μmol/g) | B Acid Content (μmol/g) | L Acid Density (μmol/m2) |
---|---|---|---|
TiO2-AG | 221.29 | 6.04 | 0.665 |
TS91 | 370.29 | 20.05 | 0.705 |
TS82 | 301.33 | 16.67 | 0.564 |
TS73 | 299.51 | 8.74 | 0.571 |
TS64 | 208.83 | 9.85 | 0.473 |
TS55 | 164.51 | 13.27 | 0.407 |
Catalyst | Introduction Stage of Catalyst | [η] (dL/g) | Mn (g/mol) | L | a | b | Terminal Carboxyl Content (mol/t) |
---|---|---|---|---|---|---|---|
TiO2-AG | After esterification | 1.14 | 4.03 × 104 | 90.69 | −0.03 | 2.08 | 32.05 |
TS91 | After esterification | 1.74 | 7.72 × 104 | 90.73 | −0.17 | 1.97 | 25.45 |
TS82 | After esterification | 1.64 | 7.05 × 104 | 90.70 | −0.31 | 2.01 | 24.32 |
TS73 | After esterification | 1.61 | 6.85 × 104 | 90.21 | −0.27 | 2.67 | 25.31 |
TS64 | After esterification | 1.35 | 5.22 × 104 | 89.15 | −0.16 | 3.43 | 23.32 |
TS55 | After esterification | 0.93 | 2.94 × 104 | 88.02 | −0.20 | 4.51 | 26.44 |
TBT | After esterification | 1.89 | 8.74 × 104 | 88.14 | −0.29 | 4.61 | 51.68 |
No catalyst | - | 0.63 | 1.62 × 104 | 82.21 | −0.18 | 9.81 | 82.75 |
TS91 | Before esterification | 1.78 | 7.99 × 104 | 91.03 | −0.21 | 1.93 | 24.43 |
TBT | Before esterification | 1.26 | 4.70 × 104 | 88.26 | −0.32 | 4.79 | 62.37 |
Polycondensation Temperature | Linear Regression Equations (TS91) | Linear Regression Equations (TBT) |
---|---|---|
220 °C | Mt = 2923 + 481t; K = 241 | Mt = 2923 + 716t; K = 358 |
225 °C | Mt = 2923 + 656t; K = 328 | Mt = 2923 + 933t; K = 467 |
230 °C | Mt = 2923 + 779t; K = 390 | Mt = 2923 + 1042t; K = 521 |
235 °C | Mt = 2923 + 946t; K = 473 | Mt = 2923 + 1053t; K = 527 |
240 °C | Mt = 2923 + 972t; K = 486 | Mt = 2923 + 1180t; K = 590 |
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Zou, W.; Bian, H.; Guo, J.; Xu, J.; Guo, B. Preparation of Titania–Silica Composite Aerogel at Atmospheric Pressure and Its Catalytic Performance in the Synthesis of Poly (Butylene Succinate). Materials 2023, 16, 3296. https://doi.org/10.3390/ma16093296
Zou W, Bian H, Guo J, Xu J, Guo B. Preparation of Titania–Silica Composite Aerogel at Atmospheric Pressure and Its Catalytic Performance in the Synthesis of Poly (Butylene Succinate). Materials. 2023; 16(9):3296. https://doi.org/10.3390/ma16093296
Chicago/Turabian StyleZou, Wenqi, Hongli Bian, Jinjing Guo, Jun Xu, and Baohua Guo. 2023. "Preparation of Titania–Silica Composite Aerogel at Atmospheric Pressure and Its Catalytic Performance in the Synthesis of Poly (Butylene Succinate)" Materials 16, no. 9: 3296. https://doi.org/10.3390/ma16093296