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Tetrahydrofuran from Caustic-Washed Furan Hydrogenated over Nickel on Kieselguhr (Banford and Manes, du Pont, US 2,846,449)
Furan from furfural carries a little carbon dioxide and water that distilling does not remove, and they hold back the hydrogenation. Banford and Manes washed the furan with dilute potash first; then nickel on kieselguhr turned nearly all of it into tetrahydrofuran.
Result: tetrahydrofuran, conversion raised from 85-90 % to 97 %.
Source: Banford and Manes, US 2,846,449 (du Pont, 1958), Example 1. Not given: how the THF is drawn off. Picture drawn by Youblob.
Juu
1 day
Maagizo
1
1
Make the caustic wash
Make the caustic wash
Make 10 % potassium hydroxide in water.
Zana zinazohitajika:
Hidroksidi ya potasiamu
Maji2
2
Wash the furan
Wash the furan
Pass distilled furan up through the caustic in a column packed with porcelain saddles, then let suspended caustic settle out. Ours at small scale: shake in a separatory funnel and draw off the caustic.
Vifaa kwa hatua hii:
Furani1 as requiredZana zinazohitajika:
Funeli ya Kutenganisha3
3
Hydrogenate
Hydrogenate
Heat the washed furan and feed it with hydrogen to a hydrogenator holding active nickel on kieselguhr at 85-100 C and about 500 psi gauge.
Vifaa kwa hatua hii:
Hidrojeni1 as requiredZana zinazohitajika:
Kichocheo cha nikeli juu ya kiselguri
Riakta ya shinikizo
Kipima Shinikizo
Kipimajoto4
4
Check the conversion
Check the conversion
Washed furan gives about 97 % tetrahydrofuran; unwashed only 85-90 %. Raising the feed to 105 C does not help unwashed furan.
Zana Zinazohitajika
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