Patent GB-1089553-A (GB)
Title: A process and an apparatus for the production of ferroselenium in granular form
IPC: B01J2/06
Filed: 1964-09-18
Abstract: Ferroselenium in the form of spherical granules is produced by heating a powdered mixture of 40 to 60% selenium and the rest iron to sintering and reaction temperature say 350 DEG C and thereafter to melting temperature, say 900-1100 DEG C and allowing the molten ferroselenium to fall 3 to 12 metres through a gas which is chemically inert relative to the melt into a liquid inert to ferroselenium e.g. water at say 30 to 90 DEG C.  The product preferably contains approximately 54.7% Se (formula FeSe corresponds to 58.57%Se).  The melting container is made of or is lined with a material inert to the reaction mixture and not wetted by ferroselenium e.g. graphite, carbides and nitrides such as silicon carbide, boron nitride.  The melting may be carried out in an inert gas such as nitrogen or argon.  In Fig.1 graphite crucible 1 with a cylindrical casing has a bottom 2 having a plurality of orifices for draining the melt, and is surrounded by electrical resistance furnace 3 which may be provided with separate heating elements at the top and bottom.  Charging tube 4 is surrounded by a jacket 5 for passing cooling air to prevent melting and sticking of the reactant mixture. Gases and dust from the system are expelled through 7.  Powder mixture is fed to <PICT:1089553/C6-C7/1> charge tube 4 by feed worm 9 from a pocket 10 and a supply container 11.  Shaft 12 is provided with a pipe-socket 13 for introducing an inert gas into the system, and opens into collecting container 14 connected to a lesser collecting container 17 having a drain 18 closed by clamp valve 19. Collecting container 14 may be closed by a cover provided with an opening adapted to the outer diameter of the shaft.  The container system is filled with water until the water level reaches the lower end of the tube 12.  Air is expelled from the shaft and the crucible by introducing nitrogen or argon through 13.  The ferroselenium level is maintained at a desired height in the crucible by adapting the charging of the powder to the drainage from the crucible using known sensing devices.  The granules formed in the water collect in chamber 17 and discharged on to sieve 20 for air drying by closing throttle 16 and opening clamp valve 19. Undersized or over-sized ferroselenium granules may be charged into container 11.ALSO:Ferroselenium in the form of spherical granules is produced by heating a powdered mixture of 40 to 60% selenium and the rest iron to sintering and reaction temperature say 350 DEG  C. and thereafter to melting temperature, say 900-1100 DEG  C. and allowing the molten ferroselenium to fall 3 to 12 metres through a gas which is chemically inert relative to the melt into a liquid inert to ferroselenium e.g. water at say 30 DEG to 90 DEG  C. The product preferably contains approximately 54.7% Se (formula FeSe corresponds to 58.57% Se).  The melting container is made of or is lined with a material inert to the reaction mixture and not wetted by ferroselenium e.g. graphite, carbides and nitrides such as silicon carbide, boron nitride.  The melting may be carried out in an inert gas such as nitrogen or argon.  In Fig. 1 graphite crucible 1 with a cylindrical casing has a bottom 2 having a plurality of orifices for draining the melt, and is surrounded by electrical resistance furnace 3 which may be provided with separate heating elements at the top and bottom.  Charging tube 4 is surrounded by a jacket 5 for passing cooling air to prevent melting and sticking of the reactant mixture.  Gases and dust from the system are expelled through 7.  Powder mixture is fed to charge tube 4 by feed worm 9 from a pocket 10 and a supply container 11.  Shaft 12 <PICT:1089553/C1/1> is provided with a pipe-socket 13 for introducing an inert gas into the system, and opens into collecting container 14 connected to a lesser collecting container 17 having a drain 18 closed by clamp valve 19.  Collecting container 14 may be closed by a cover provided with an opening adapted to the outer diameter of the shaft.  The container system is filled with water until the water level reaches the lower end of the tube 12. Air is expelled from the shaft and the crucible by introducing nitrogen or argon through 13. The ferroselenium level is maintained at a desired height in the crucible by adapting the charging of the powder to the drainage from the crucible using known sensing devices.  The granules formed in the water collect in chamber 17 and discharged on to sieve 20 for air drying by closing throttle 16 and opening clamp valve 19. Undersized or oversized ferroselenium granules may be charged into container 11.