Iron-bath reactors

Figure 1. Two-stage smelting reduction process using an iron-bath reactor. (From Japan Metal Bull., 1988.)...

Zhang, L., and Oeters, F., A Model of Post-Combustion in Iron-Bath Reactors, Part 1 Theoretical Basis, Steel Res., 62 95 (1991a)... 

There are currently three industrially-proven methods for coal gasification, namely fixed-bed gasification (e.g. Lurgi), fluidized bed reactors (e.g. Fritz Winkler (BASF)) and entrained bed processes (e.g. Texaco, Koppers-Toizt, Other processes are being developed, e.g. coal gasification in an iron bath. 

The older literature reports the synthesis of phosphorus-(V) sulfochloride by reaction of phosphorus (V) chloride with phosphorus (V) sulfide in a sealed tube at 120°. Experience has shown that pressures as great as 700 p.s.i. may result under these conditions, indicating that an autoclave or bomb should be used. In the absence of these, the reactor shown in Fig. 8 is suitable. It consists of an oil bath containing a lecture bottle fitted with a pipe plug (iron pipe size, % in.), a thermometer, and a knife type of immersion heater. Although no difficulty has been experienced in the use of this reactor, it is well to keep it behind a barricade during the reaction. 

A reactor was charged with 84 ml of hexane and butadiene (10 g) and then treated sequentially with iron isooctanoate (0.0124 mmol), triisobutylaluminum (0.19 mmol), and ethyl phosphite (0.0295 mmol). The mixture was placed into a 50°C water bath and polymerized for 4 hours. Thereafter an aqueous alcohol solution containing 2,6-di(t-butyl)-4-cresol was added to precipitate the mbber sample. The material was dried, and the product was isolated. 

Fig. 339. Preparation of very fine iron powder with globular particles. a iron carbonyl distillation flask b oil bath c decomposition reactor and furnace d thermocouple f filter.

The sodium reduction of titanium tetrachloride was actually carried out as early as 1939 in Germany, and about 670 kg was produced by the Deutsche Gold and Silber Scheideanstalt, during the 1939-45 war. The process, now obsolete, involved reduction in a molten bath of 50 per cent sodium chloride and 50 per cent potassium chloride at 800°C in an atmos phere of hydrogen. The reactors consisted of expendable welded sheet-iron cylindrical vessels, 50 cm diameter by 70 cm deep and 2 mm thick. These rested loosely in a stout iron crucible, fitted into a gas-fired furnace. A portable stirrer was used to agitate the reactor contents. Approximately 20 kg batches of titanium were reduced by distilling 85 kg of titanium tetrachloride at a controlled rate into a melt of 15 kg sodium chloride and 15 kg of potassium chloride, covered with a layer of 46 kg of molten sodium. The titanium sank to the bottom of the molten salts, and at the end of the reaction was recovered from the crushed solidified melt by leaching with dilute hydrochloric acid, in a ceramic-lined vessel. It was finally washed in water and dried at a moderate temperature. The same plant was also used for the production of zirconium metal by the sodium reduction of potassium fluorozirconate (KaZrF ]. 

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