Method for preparing high-purity rhenium(VII) oxide through gas reduction
A rhenium heptaoxide, gas technology, applied in chemical instruments and methods, rhenium compounds, inorganic chemistry and other directions, can solve problems such as affecting the performance of materials, and achieve the effects of short process, high reaction yield and high product purity
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Embodiment 1
[0016] (1) Take 10g of crude ammonium rhenate (the mass percentage of ammonium rhenate is 99%) and place it in a quartz boat, place it horizontally in the center of the quartz tube of the tubular heating furnace, place refractory plugs on both sides of the quartz tube; Replace the air in the quartz tube; the ventilation flow rate is 3000ml / min, and the ventilation time is 30 minutes;
[0017] (2) Heat up to 150 o C, while continuously feeding CO gas, reacted for 2 h; continued to heat up to 350 °C for 5 h, and then naturally cooled to 100 °C.
[0018] (3) Introduce oxygen into the quartz tube cooled to 100°C to replace the CO gas in the tube, the ventilation flow rate is 3000ml / min, and the aeration time is 30 minutes; then raise the temperature to 150°C, and continue to feed oxygen for 2 hours to react, and continue to heat up to React at 350 °C for 1 h, then cool to room temperature naturally. Light yellow rhenium heptoxide is generated in the condenser connected with the ...
Embodiment 2
[0020] (1) Take 10g of crude ammonium rhenate (the mass percentage of ammonium rhenate is 99%) and place it in a quartz boat, place it horizontally in the center of the quartz tube of the tubular heating furnace, place refractory plugs on both sides of the quartz tube, and feed NH 3 Replace the air in the quartz tube; the ventilation flow rate is 3500 ml / min, and the ventilation time is 40 minutes;
[0021] (2) Heat up to 250 o C, while continuously feeding NH 3 , reacted for 1.5 h; continued to heat up to 400 °C for 3 h, then naturally cooled to 100 °C;
[0022] (3) Introduce oxygen into the quartz tube cooled to 100 °C to replace the gas in the tube, the ventilation flow rate is 3500 ml / min, and the ventilation time is 40 min; then the temperature is raised to 150 °C, and the oxygen reaction is continued for 1.5 h at the same time; continue to heat up React at 400°C for 2h, and cool to room temperature naturally. There is light yellow rhenium heptoxide generated in the co...
Embodiment 3
[0024] (1) Take 10g of crude ammonium rhenate (the mass percentage of ammonium rhenate is 99%) and place it in a quartz boat, place it horizontally in the center of the quartz tube of the tubular heating furnace, place refractory plugs on both sides of the quartz tube, and inject NO Replace the air in the quartz tube: the ventilation flow rate is 4000 ml / min, and the ventilation time is 40 minutes;
[0025] (2) Heat up to 150 o C, continue to feed NO gas at the same time, react for 2.5 h; continue to heat up to 450 °C for 4 h, and naturally cool to 100 °C;
[0026] (3) Introduce oxygen into the quartz tube cooled to 100 °C to replace the gas in the tube: the ventilation flow rate is 4000 ml / min, and the ventilation time is 40 min; then the temperature is raised to 200 °C, and the oxygen reaction is continued for 2.5 h at the same time, and the temperature is continued to React at 450°C for 3h, and cool to room temperature naturally. There is light yellow rhenium heptoxide ge...
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