反応 #350553

反応方程式

pyridine

→

Naphthalene

反応条件

後処理

1. 1
   その他a Mettler softening point of 250° C.
2. 2
   その他was conducted at 100° C.
3. 3
   ろ過followed by filtration with a 0.5 μm membrane
4. 4
   ろ過filter
5. 5
   その他to 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
   その他was conducted at about 70° C.
9. 9
   ろ過followed by filtration with a 0.5 μm membrane
10. 10
    ろ過filter
11. 11
    その他to remove a soluble matter
12. 12
    その他From the insoluble matter, the solvent was removed
13. 13
    その他to obtain a spinning pitch
14. 14
    その他ΔTg of 27° C. and Qi of not more than 1% by weight

実験手順

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.

出典