Method for preparing metallic titanium powder by reducing titanium dioxide with magnesium
A technology of titanium dioxide and metal titanium powder is applied in the field of metal material preparation by vacuum metal thermal reduction, which can solve the problems of high cost and long process, and achieve the effects of less impurities, short process and no environmental pollution.
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Embodiment 1
[0013] Embodiment 1: Weigh 5g of pigment-grade titanium dioxide, 5g of analytically pure calcium chloride, 30g of magnesium metal with a purity ≥ 95.7%, and mix the former two; place the magnesium metal at the bottom of a self-made reaction crucible, and place the prepared mixture in the middle Molybdenum transparent plate, sealed, put the crucible into a vacuum furnace, heat up to 900°C at 10°C / min, control the pressure in the furnace at 15-20Pa, keep it at the reaction temperature for 12h; take out the reduced product after cooling to room temperature ; and then leached with 4.48wt% dilute hydrochloric acid for 6 hours, washed repeatedly with distilled water until the pH value was 6.5 to 7, filtered and then dried in a vacuum oven, the temperature was set at 80 ° C, and the time was 12 hours; after drying, metal Titanium powder, the XRD spectrum of the obtained titanium powder is shown in Figure 2.
Embodiment 2
[0014] Embodiment 2: Take by weighing 25g of pigment-grade titanium dioxide, 5g of analytically pure calcium chloride, and 20g of magnesium metal with a purity ≥ 95.7%, mix the former two and make a block material of ￠10×5 under a pressure of 3MPa; The metal is placed at the bottom of the self-made reaction crucible, and the bulk material is placed on the molybdenum transparent plate in the middle, sealed, and the crucible is placed in a vacuum furnace; the temperature is raised to 1000 °C at 10 °C / min, and the pressure in the furnace is stable at 8-20 Pa. Insulate at reaction temperature for 8 hours, take out the reduction product after cooling to room temperature; then leaching with 4.48wt% dilute hydrochloric acid for 8 hours, wash with distilled water repeatedly until the pH value is 6.5-7, filter and then dry in a vacuum oven at a temperature of 90℃, the time is 10h; after drying, metal titanium powder can be obtained.
Embodiment 3
[0015] Embodiment 3: Take by weighing 50g of pigment-grade titanium dioxide, 5g of analytically pure calcium chloride, and 90g of magnesium metal with a purity ≥ 95.7%, mix the former two and make a block of ￠20×10 under a pressure of 3MPa; The metal is placed at the bottom of the self-made reaction crucible, and the bulk material is placed on the molybdenum transparent plate in the middle, sealed, and the crucible is placed in a vacuum furnace; the temperature is raised to 1200 °C at 5 °C / min, and the pressure in the furnace is controlled at 10-14Pa. Insulate at reaction temperature for 8h, take out the reduced product after cooling to room temperature; then leaching with 4.48wt% dilute hydrochloric acid for 8h, wash with distilled water repeatedly until the pH value is 6.5~7, filter and place in a vacuum drying oven to dry, the temperature setting Set at 100°C for 5 hours; after drying, metal titanium powder can be obtained.
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