Method for producing high-purity zirconium oxychloride and co-producing silicon tetrachloride through zircon sand boiling chlorination method
A technology of boiling chlorination and pure zirconium oxychloride, which is applied in the direction of zirconium halide, silicon halide compound, halosilane, etc., can solve the problem of high production cost, increased production cost, and product quality that cannot reach high-purity zirconium oxychloride Quality standards and other issues to achieve the effect of low production cost and good product quality
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[0040] Example 1
[0041] Process route see figure 1 , The specific preparation is:
[0042] 1) Chlorination reaction
[0043] Add the raw materials zircon sand, calcined petroleum coke and silicon carbide to the ratio of zircon sand: calcined coke: silicon carbide=1:0.22:0.34 into the mixer to mix the materials, and add them to the front of the furnace after mixing. The silo is continuously fed into the chlorination furnace through a screw conveyor.
[0044] Chlorine gas is introduced into the bottom of the chlorination furnace, the weight of which is zircon sand: chlorine = 1:2.78, so that the chlorine gas enters the reaction section through the sparger to react with the raw materials. The reaction temperature is controlled at 1170°C and the furnace pressure is controlled within 3000 Pa. Determine the slagging time of the chlorination furnace according to the furnace pressure, and control the chlorine flow rate at 0.009m / s, the reaction can proceed quickly, and the chemical reactio...
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[0080] Example 2
[0081] The gas-solid separation of the silicon tetrachloride-containing tail gas into the gas obtained by the quencher cooling treatment in Example 1, the obtained solid is zirconium tetrachloride solid, which enters the purifier for purification, and then enters the hydrolysis tank through the screw conveyor, and adds Pure water, evaporating acid, and washing liquid are hydrolyzed, and the amount of material added is controlled to zirconium tetrachloride
[0082] Solid: pure water: evaporating acid: washing liquid is 0.91:2.35:0.72:1.00 (weight ratio), control the hydrolysis temperature at 40-50℃, the speed of the hydrolysis tank mixer is 100r / min, and the zirconium concentration of the hydrolyzed solution is 100±10g / l, use a pump to send to the chamber filter press to filter out the entrained solids to obtain a purified refined zirconium oxychloride solution. The washing liquid during hydrolysis can be recycled and reused. Among them, the evaporating acid is ...
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[0094] Example 3
[0095] The primary mother liquor prepared in the above example 1 or example 2 is pressurized and evaporated, the primary crystallization mother liquor enters the dual heating external circulation graphite evaporator, the mother liquor is heated by steam, and the secondary steam from the evaporator is used as the heat source to preheat the mother liquor solution , Control the vapor pressure at 0.3MPa~0.7MPa, and the secondary pressure at 0.2MPa—0.3MPa, so that the concentration of hydrochloric acid in the evaporation liquid is 17~19%, and the concentration of zirconium dioxide is 190±10g / l. Crystallization tank, crystallization treatment at 25 ℃ for 20 hours, the crystallized oxychlorination solution is filtered through a belt filter, after filtration, the crystals are washed with 18% hydrochloric acid to obtain zirconium oxychloride, and the filtrate obtained is secondary Mother liquor.
[0096] The obtained zirconium oxychloride crystal is re-dissolved as a see...
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