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Thulium: Oxide Reduced with Aluminium in Flowing Argon and the Vapour Condensed (CN 104152695 B)
Pellets of thulium oxide and aluminium are fed into an induction furnace at 1700 °C. The aluminium takes the oxygen and stays behind as slag. Thulium boils off as vapour, and a stream of argon carries it into a water-cooled tank where it condenses to metal.
Result: thulium metal, 99.5 % of the thulium recovered. No vacuum pump is needed: the moving argon sweeps the vapour away as fast as it forms.
Source: Zhang, Dou et al. (Northeastern University), Chinese patent CN 104152695 B (2014), Example 1. Not given: batch size, the form of the aluminium, pellet size, the purity of the thulium. Picture: Wikimedia Commons.
Lanjutan
1 day
Arahan
1
1
Weigh and mix
Weigh and mix
Weigh thulium oxide and aluminium, both over 99.0 % pure, in the molar ratio 1 : 2.2: 10 % more aluminium than the reaction needs (ours: about 15.4 g of aluminium to 100 g of oxide). Mix them evenly.
Bahan untuk langkah ini:
Tulium oksida100 gAlatan diperlukan:
Aluminium
Penimbang2
2
Press into pellets
Press into pellets
Press the mix in a roller press at 100 kg/cm² into lumpy pellets.
Alatan diperlukan:
Mesin tekan penggelek3
3
Reduce in flowing argon
Reduce in flowing argon
Run argon (99.95 %) through a medium-frequency induction furnace (the patent's coil is 220 mm across) at 5 L/min; ours: set the flow with a rotameter. Feed the pellets in continuously and hold them at 1700 °C for 30 min. The thulium leaves as vapour mixed with the argon; draw the slag off continuously.
Alatan diperlukan:
Relau aruhan
Argon
Rotameter4
4
Condense the thulium
Condense the thulium
Let the argon carry the vapour out of the furnace through a sealed pipe straight into a condensing tank cooled by circulating water. The thulium condenses there as metal: 99.5 % recovered. Example 2 of the patent runs at 1500 °C for 60 min with 15 L/min of argon (pellets pressed at 150 kg/cm²) and reports 99.2 %.
Alatan diperlukan:
Kebuk pemeluwapan
AirBahan
1- 100 gPemegang Tempat
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Berbahaya
Erbium, Ytterbium, Thulium and Lutetium Oxides: Xenotime Separated on Ion Exchange Columns with EDTA and HEDTA (Spedding and Powell, US 2,956,858)
oleh Charlie
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Berbahaya
Aluminium by Hall–Héroult Electrolysis: Alumina in Molten Cryolite
oleh Forge
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Argon: Air Led over Calcium Carbide and Calcium Chloride at 800 °C (Fischer and Ringe, Thorpe 1912)
oleh Charlie
Bukan Organik
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Ytterbium: Oxide Reduced by Lanthanum at 1020 °C in Vacuum, Metal Distilled Off (Shindo and Yagi, US 2010/0260640)
oleh Charlie
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