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Furan from Furfural Vapour and Steam over Zinc-Iron Chromite (Whitman, du Pont, US 2,374,149)
Furfural carries one aldehyde group too many for most uses. Whitman passed its vapour with plenty of steam over a hot mixed zinc-iron chromite; the aldehyde group leaves and furan, a very volatile ring liquid, is caught in cold condensers.
Result: furan boiling at 31-32 C, 85 % of the furfural converted.
Source: Whitman, US 2,374,149 (du Pont, 1945), Example I. Picture drawn by Youblob.
Advanced
1 day
Instructions
1
1
Pack the catalyst
Pack the catalyst
Fill the reactor tube with zinc-iron chromite pellets, 90 zinc : 10 iron, 3/16 inch. Whitman made it from zinc chloride, 398 g ferrous sulfate and 2170 g ammonium chromate, neutralised with 800 cc of 28 % ammonia, dried at 110 C and ignited 4 hours at 400 C.
Tools needed:
Zinc-Iron Chromite Catalyst
Tube Furnace2
2
Reduce in hydrogen
Reduce in hydrogen
Heat the catalyst in a stream of hydrogen at 450 C.
Tools needed:
HydrogenTube Furnace
Thermometer3
3
Pass furfural with steam
Pass furfural with steam
At 425 C feed 1 volume of furfural vapour with 5 volumes of steam, space velocity 500.
Materials for this step:
Furfural1 part by volumeTools needed:
Steam BoilerTube FurnaceThermometer4
4
Condense cold
Condense cold
Lead the gases through a condenser at 0 C and then one at -60 C to hold the furan.
Tools needed:
Condenser Coil
Cold Trap5
5
Strip, dry and fractionate
Strip, dry and fractionate
Strip the furan off below 70 C, dry it over calcium chloride and take the fraction boiling at 31-32 C. Conversion: 85 %.
Tools needed:
Calcium Chloride
Fractionating StillThermometerTools Required
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