반응 #350553

반응 방정식

pyridine

→

Naphthalene

반응 조건

후처리

1. 1
   기타a Mettler softening point of 250° C.
2. 2
   기타was conducted at 100° C.
3. 3
   여과followed by filtration with a 0.5 μm membrane
4. 4
   여과filter
5. 5
   기타to remove a pyridine-insoluble matter
6. 6
   workup.ADDITIONThen, a solvent mixture of toluene/hexane=40 volume %/60 volume % (solubility parameter: 7.9)
7. 7
   workup.ADDITIONwas added in an amount of 150 ml to 3 g of the soluble matter, and extraction
8. 8
   기타was conducted at about 70° C.
9. 9
   여과followed by filtration with a 0.5 μm membrane
10. 10
    여과filter
11. 11
    기타to remove a soluble matter
12. 12
    기타From the insoluble matter, the solvent was removed
13. 13
    기타to obtain a spinning pitch
14. 14
    기타ΔTg of 27° C. and Qi of not more than 1% by weight

실험 절차

Naphthalene was polymerized at a temperature of from 200° to 400° C. in the presence of a HF.BF3 catalyst to obtain a pitch which had an optical anisotropy of 100%, a Mettler softening point of 250° C. and an elemental composition as analyzed of C: 94.8 wt % and H: 5.2 wt %. This pitch was finely pulverized. Then, pyridine (solubility parameter: 10.6) was added in an amount of 200 ml to 5 g of this pitch, and extraction was conducted at 100° C., followed by filtration with a 0.5 μm membrane filter to remove a pyridine-insoluble matter. Then, a solvent mixture of toluene/hexane=40 volume %/60 volume % (solubility parameter: 7.9) was added in an amount of 150 ml to 3 g of the soluble matter, and extraction was conducted at about 70° C., followed by filtration with a 0.5 μm membrane filter to remove a soluble matter. From the insoluble matter, the solvent was removed to obtain a spinning pitch. The pitch had ΔTg of 27° C. and Qi of not more than 1% by weight.

출처