Preparation and Application of Magnetic Nano-Solid Acid Catalyst Fe3O4-PDA-SO3H
Abstract
:1. Introduction
2. Materials and Methods
2.1. Materials
2.2. Preparation of Fe3O4 Nanoparticles
2.3. Preparation of Fe3O4-PDA Nanoparticles
2.4. Preparation of Fe3O4-PDA-SO3H Nanoparticles
2.5. Characterization
2.6. Determination of Acid Density
2.7. Typical Experimental Produre for Esterification Between LA with Different Alcohols
2.8. Response Surface Optimization
3. Results and Discussion
3.1. Effect of Sulfonation of Chlorosulfonic Acid
3.1.1. Effect of Chlorosulfonic Acid on Magnetic Nanosolid Acid Catalyst
3.1.2. Effect of Sulfonation Time on Solid Acid Density
3.2. Catalyst Characterization
3.2.1. SEM Characterization
3.2.2. XRD Characterization
3.2.3. EDX Characterization
3.2.4. FT-IR Characterization
3.3. Optimum Reaction Conditions for Fe3O4-PDA-SO3H Magnetic Nano-Solid Acid
3.3.1. Effect of Catalyst Dosage on Esterification Reaction
3.3.2. Effect of Reaction Temperature
3.3.3. Effect of Acid: Alcohol Mole Ratio
3.4. Optimization of Esterification Conditions of Solid Acid Catalyst Fe3O4-PDA-SO3H
3.5. Recyclability of Catalyst
3.6. Comparison with other Typical Solid Acids
4. Conclusions
- (1)
- FT-IR and EDX demonstrated successful loading of polydopamine and sulfonic groups. SEM and XRD showed that the catalyst showed a complete and uniform core-shell structure, and the loading of chlorosulfonic acid would not affect the crystal form of Fe3O4.
- (2)
- The optimum reaction conditions for catalytic reaction of Fe3O4-PDA-SO3H were obtained by single factor and response surface optimization. The optimum experimental reaction conditions were the reaction temperature is 90.55 °C, the molar ratio of acid to alcohol is 1:12.94, optimal amount of catalyst is 23.99% of the mass of acetylpropionic acid and the stirring rate is 401 r/min. The conversion of acetylpropionic acid was 95.87% under this condition.
- (3)
- The results of LA with different alcohol esterification can be proved that this solid acid catalyst has highly efficient and good reusability. Compared with the common cation exchange resin Amberlyst 36 and Amberlyst 46, the results showed that the effect was better under the same reaction conditions.
Author Contributions
Funding
Conflicts of Interest
References
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Experimental Factors | Level | |
---|---|---|
Low | High | |
Temperature of reaction (°C) | 80 | 100 |
mole ratio | 1:7 | 1:15 |
Amount of catalyst (wt%) | 10 | 25 |
Speed of revolution (r/min) | 320 | 466 |
Type of Catalyst | Acid Density (mmol/g) | LA Conversion with Ethanol (%) | LA Conversion with n-Butanol (%) | LA Conversion with n-Octanol (%) |
---|---|---|---|---|
Fe3O4-PDA-SO3H | 1.238 | 89.8 | 95.55 | 95.65 |
Amberlyst 36 | 5.4 | 10.59 | 13.14 | 39.53 |
Amberlyst 46 | 3.1 | 52.5 | 35.56 | 71.28 |
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Wang, H.; Lu, Y.; Liu, H.; Yin, Y.; Liang, J. Preparation and Application of Magnetic Nano-Solid Acid Catalyst Fe3O4-PDA-SO3H. Energies 2020, 13, 1484. https://doi.org/10.3390/en13061484
Wang H, Lu Y, Liu H, Yin Y, Liang J. Preparation and Application of Magnetic Nano-Solid Acid Catalyst Fe3O4-PDA-SO3H. Energies. 2020; 13(6):1484. https://doi.org/10.3390/en13061484
Chicago/Turabian StyleWang, Honghai, Yifan Lu, Hongli Liu, Yi Yin, and Jun Liang. 2020. "Preparation and Application of Magnetic Nano-Solid Acid Catalyst Fe3O4-PDA-SO3H" Energies 13, no. 6: 1484. https://doi.org/10.3390/en13061484