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ÀWỌN OHUN WÍWỌ̀
Dodecafluoroheptanol: Tetrafluoroethylene Joined to Methanol (Joyce 1951)
Heated with methanol and a little peroxide, tetrafluoroethylene adds on to the methanol in short chains: H(CF2CF2)nCH2OH, with n from 1 to 12. Steam carries off the short ones; distilling the liquid part sorts them by boiling point. The cut at 169–170 °C, three units long, is the start of a fluorine soap used to make PTFE dispersions.
Source: R. M. Joyce (du Pont), US 2,559,628 (1951), Example IV. The steam-distillation and fractionating apparatus is ours. Picture drawn by Youblob.
Ilọsíwájú
2 days
Ìlànà
1
1
Charge the reactor
Charge the reactor
Put 150 parts of methanol and 2 parts of tert-butyl octyl peroxide in a high-pressure reactor. Close it, cool it, and let in 110 parts of tetrafluoroethylene through a valve. Parts are by weight.
Àwọn ohun èlò fún ìgbésẹ̀ yìí:
Methanol150 parts
Tẹ́trafluoroétílénì110 partsÀwọn irinṣẹ́ tí a nílò:
tert-Butyl octyl peroxide
Ìkòkò ìṣesí ìfúnpá
Àgbá gáàsì tí a fi ìfúnpá kún
Òǹwọ̀n ìdọ́gba2
2
Heat at 170 °C for 10 hours
Heat at 170 °C for 10 hours
Agitate and heat at 170 °C for 10 hours. The pressure rises on its own to about 90 atmospheres.
Àwọn irinṣẹ́ tí a nílò:
Ìkòkò ìṣesí ìfúnpá
Ẹ̀rọ Ìwọ̀n Ìtẹ̀
Ẹ̀rọ Ìwọ̀n Ooru3
3
Steam-distil the product
Steam-distil the product
Steam-distil the product. What comes over is part liquid and part solid; separate the two. Ours: steam from a boiler through the flask, a condenser, and a separatory funnel for the liquid.
Àwọn irinṣẹ́ tí a nílò:
Bọ́ìlà èéfín omi
Ìgò Gíláàsì Ìsàn
Ìyípo ẹ̀rọ ìtutù
Fọ́nẹ́ẹ̀lì Ìyàpa4
4
Fractionate; keep the 169–170 °C cut
Fractionate; keep the 169–170 °C cut
Fractionally distil the liquid part. It separates into the series H(CF2CF2)nCH2OH; collect the fraction boiling at 169–170 °C, where n = 3 (dodecafluoroheptanol). The patent gives no yield for this cut.
Àwọn irinṣẹ́ tí a nílò:
Ohun ìsun tí ó pínẸ̀rọ Ìwọ̀n Ooru
Ìgò Gílásì OnídìíÀwọn irinṣẹ́ tó nílò
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