Polymerizing-pyrolytic method for preparing mesocarbon microbead in asphaltic base
A mesophase carbon microsphere and pitch-based technology, which is applied in the field of carbon materials, can solve the problems of low yield, uneven shape and size, and low preparation cost of mesophase carbon microspheres, and achieve easy operation, wide application, and particle size The effect of uniform diameter distribution
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[0038] Example 1
[0039] Take coal tar pitch as raw material, formaldehyde as crosslinking agent, and oxalic acid as catalyst. Add them to a three-necked flask at a mass ratio of 100:4:2. The temperature is freely heated before 100°C, and at a rate of 5°C / min after 100°C. Increase temperature, and pass N from the beginning 2 , N 2 The flow rate is 50mL / min, and the reaction is carried out at 130℃ for 2h, and the polymer modified asphalt is obtained in N 2 Treated at 420°C for 2h under protection, and then dissolved in pyridine (the mass ratio of pyridine to pyrolysis product is 60:1) and extracted to be colorless. After vacuum drying, mesocarbon microspheres with a particle size of about 8μm are obtained. The yield was 30.74%. Good sphericity and narrow particle size distribution.
Example Embodiment
[0040] Example 2
[0041] Using coal tar pitch as the raw material, benzaldehyde as the crosslinking agent, and p-toluenesulfonic acid as the catalyst, add them to a three-necked flask at a mass ratio of 100:12:2. / min heating rate, and from the heating start to pass N 2 , N 2 The flow rate is 50mL / min, and the reaction is carried out at 130℃ for 3h, and the polymer modified asphalt is obtained in N 2 Treated at 460℃ for 2h under protection, and then extracted with pyridine (the mass ratio of pyridine to pyrolysis product is 60:1) to be colorless, dried in vacuum to obtain mesocarbon microspheres with a particle size of about 12μm. The rate is 40.62%. The sphericity is good, and the carbon microspheres rarely merge.
Example Embodiment
[0042] Example 3
[0043] Using coal tar pitch as raw material, p-methylbenzaldehyde as crosslinking agent, and oxalic acid as catalyst, add them to a three-necked flask at a mass ratio of 100:8:2. The temperature is freely heated before 100°C, and 5°C after 100°C / min heating rate, and from the heating start to pass N 2 , N 2 The flow rate is 50mL / min, and the reaction is carried out at 140℃ for 2h, and the polymer modified asphalt is obtained in N 2 Treated under protection at 450℃ for 1h, and then extracted with pyridine (the mass ratio of pyridine to pyrolysis product is 60:1) to be colorless, dried in vacuum to obtain mesocarbon microspheres with a particle size of about 10μm. The rate is 35.54%. The sphericity is good, the surface finish is good, and the fusion between the balls rarely occurs.
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