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Dodecafluoroheptanol: Tetrafluoroethylene Joined to Methanol (Joyce 1951)
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28. uMfumfu 2026DE
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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.
Osezingeni eliphezulu
2 days

Imiyalelo

1

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.

Izinto zokwakha zalesi sinyathelo:

I-methanolI-methanol150 parts
I-TetrafluoroethyleneI-Tetrafluoroethylene110 parts

Amathuluzi adingekayo:

I-tert-butyl octyl peroxideI-tert-butyl octyl peroxide
I-reactor yengcindeziI-reactor yengcindezi
Isilinda segesi ecindezelweIsilinda segesi ecindezelwe
Isikali sesilinganisoIsikali sesilinganiso
2

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.

Amathuluzi adingekayo:

I-reactor yengcindeziI-reactor yengcindezi
Isilinganiso SengcindeziIsilinganiso Sengcindezi
IthemomithaIthemomitha
3

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.

Amathuluzi adingekayo:

Ibhayela lesitimuIbhayela lesitimu
Ifulakhi Lengilazi LokuhluzaIfulakhi Lengilazi Lokuhluza
Ugoqo lwe-condenserUgoqo lwe-condenser
Ifasitela lokwehlukanisaIfasitela lokwehlukanisa
4

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.

Amathuluzi adingekayo:

Isicwengi esahlukanisayoIsicwengi esahlukanisayo
IthemomithaIthemomitha
Ijeke Lengilazi ElinesivaloIjeke Lengilazi Elinesivalo

Izinto

2

Amathuluzi Adingekayo

12

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