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Dodecafluoroheptanol: Tetrafluoroethylene Joined to Methanol (Joyce 1951)
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28. Oktoba 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.
Juu
2 days

Maagizo

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.

Vifaa kwa hatua hii:

MethanoliMethanoli150 parts
TetrafluoroethiliniTetrafluoroethilini110 parts

Zana zinazohitajika:

tert-Butili oktili peroksiditert-Butili oktili peroksidi
Riakta ya shinikizoRiakta ya shinikizo
Mtungi wa gesi yenye shinikizoMtungi wa gesi yenye shinikizo
Mizani ya mizani-mbiliMizani ya mizani-mbili
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.

Zana zinazohitajika:

Riakta ya shinikizoRiakta ya shinikizo
Kipima ShinikizoKipima Shinikizo
KipimajotoKipimajoto
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.

Zana zinazohitajika:

Boila ya mvukeBoila ya mvuke
Chupa ya Kioo ya KunerekaChupa ya Kioo ya Kunereka
Koili ya kifidishajiKoili ya kifidishaji
Funeli ya KutenganishaFuneli ya Kutenganisha
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.

Zana zinazohitajika:

Chombo cha kunereka kwa sehemuChombo cha kunereka kwa sehemu
KipimajotoKipimajoto
Mitungi ya kioo yenye vifunikoMitungi ya kioo yenye vifuniko

Vifaa

2

Zana Zinazohitajika

12

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