A kind of preparation method of isotropic high softening point coal tar pitch
A high softening point, isotropic technology, applied in chemical processing of tar pitch/petroleum pitch/natural pitch, and selective extraction of tar pitch/petroleum pitch/natural pitch, etc. The stability of properties is difficult to control, the pitch-based carbon fibers are broken or woolly, and the application effect is affected, so as to achieve the effects of low toluene soluble content, narrow molecular weight distribution, and short reaction time.
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Embodiment 1
[0024] Using medium-temperature coal tar pitch with a softening point of 75°C, a QI content of 5.2%, and an ash content of 1358ppm as a raw material, the medium-temperature coal tar pitch is liquefied at 150°C by a disc centrifuge and then centrifuged at a speed of 8000 rpm , the QI and ash content of the medium temperature coal tar pitch were reduced to 0.2% and 56ppm respectively, and the modified medium temperature coal tar pitch with a softening point of 81°C was obtained.
Embodiment 2
[0026] With 500g [embodiment one] modified medium temperature coal tar pitch, 60g sulfuric acid and 100g iodine pentoxide (I 2 o 5 ) are simultaneously placed in a 5-liter high-pressure reactor, and after sealing, feed 99.999% high-purity nitrogen until the pressure in the kettle reaches 0.5MPa. The temperature in the kettle was raised to 180° C. at a heating rate of 3° C. / min, and the stirring was continued for 3 hours at a rotating speed of 145 r / min to obtain coal tar pitch with a high softening point. The prepared high softening point coal tar pitch was extracted with methanol at 50°C for 2 hours. After drying, the obtained isotropic high softening point coal tar pitch had a softening point of 267°C, a residual carbon rate of 76.4%, and a toluene soluble content of 6.6%. , the toluene insoluble-quinoline soluble content is 89.7%, the quinoline insoluble content is 3.7%, the ash content is 79ppm, and the molecular structure of the prepared high softening point coal tar pit...
Embodiment 3
[0028] With 500g [embodiment one] modified medium temperature coal tar pitch, 60g sulfuric acid and 200g iodine pentoxide (I 2 o 5 ) are simultaneously placed in a 5-liter high-pressure reactor, and after sealing, feed 99.999% high-purity nitrogen until the pressure in the kettle reaches 0.5MPa. The temperature in the kettle was raised to 180° C. at a heating rate of 3° C. / min, and the stirring was continued for 3 hours at a rotating speed of 145 r / min to obtain coal tar pitch with a high softening point. The prepared high softening point coal tar pitch was extracted with methanol at 50°C for 2 hours. After drying, the softening point of the obtained high softening point coal tar pitch was 282°C, the residual carbon rate was 77.5%, the ash content was 74ppm, and the molecular structure was isotropic. Same-sex structure ( figure 2 ) and a narrow molecular weight distribution. Among them, the toluene soluble content is 5.4%, the toluene insoluble-quinoline soluble content is...
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