Synthesis
Put the tellurium dioxide with purity of 99.9% in graphite burner boat and put it in tubular electric furnace with stainless steel stove pipe; in the tubular electric furnace, pass hydrogen at the flow rate of 3L-30 L/min, and then reduce it at 500-550 for 7-9h, and get the purity of 99.9% at the end of the reaction. The metal tellurium powder obtained by hydrogen reduction is loaded into a heat-resistant glass three-necked flask with a volume of 1-5L, and a heat-resistant glass tube is inserted into the bottom of the flask from one side of the flask; firstly, the air in the three-necked flask is driven off with dry nitrogen, and the three-necked flask is heated up to 250 with an electrically heated thermal insulation set, and the air is passed through the flask by a flow rate of 2-200 ml/min, and the purity is 99.9%. The metal tellurium powder starts to be chlorinated and gradually changes into black tellurium dichloride liquid, continue to pass the chlorine gas, the tellurium dichloride gradually changes into liquid tellurium tetrachloride, and the product tellurium tetrachloride still contains some tellurium dichloride; the three-necked flask containing tellurium tetrachloride is heated up to 420 with an electric heating jacket, and the material is distilled out in the other flask with the chlorine gas gas stream, and the material in the other flask is distilled out. material is distilled out, and tetrachlorotellurium with a purity of 99.99% is obtained in another collection flask; the tetrachlorotellurium in the collection flask is moved to a distillation tower, and the interior of the distillation tower is replaced with nitrogen, and is heated with an electric heating jacket to 420C and a condenser is heated to 270C, at which time the tetrachlorotellurium begins to be distilled out; about 10% of the initial distillate is separated, and about 90% of the distillate is subsequently obtained as a pure purity of greater than 99.99% of the Anhydrous tellurium tetrachloride.
