Germanium dioxide dechlorination method
A germanium dioxide and dechlorination technology, applied in directions such as germanium dioxide, can solve the problems of reduced product yield, increased processing cost, increased pure water production, etc., and achieves the effects of simple operation and low cost
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Embodiment 1
[0031] Add 10L of pure water into the hydrolysis kettle, add 96mol of germanium dioxide raw material into the pure water, stir and disperse. Then add 2.9L ammonia water, and stir for 2h after adding. The resulting solution was heated to 40°C, and nitric acid was added to the solution until the free acidity reached 0.5 mol / L, then kept stirring at 40°C for 8 hours, and filtered to obtain a filter cake. Then add 10L of pure water into the hydrolysis kettle, and wash the filter cake several times until the conductivity of the washing solution is less than 50 μS / cm. Put the filter cake in a quartz container and put it into a calciner, heat up to 750°C and calcinate for 24 hours, and then cool down to room temperature to obtain low-chlorine high-purity germanium dioxide. The impurity content is as follows: figure 1 shown.
Embodiment 2
[0033] Add 60L of pure water into the hydrolysis kettle, add 96mol of germanium dioxide raw material into the pure water, stir and disperse. Then add 6.0L ammonia water, and stir for 6h after adding. The obtained solution was heated up to 100° C., sulfuric acid was added to the solution until the free acidity reached 5.0 mol / L, and then stirred and reacted at 100° C. for 1 hour, and filtered to obtain a filter cake. Then add 40L of pure water into the hydrolysis tank, and wash the filter cake several times until the conductivity of the washing liquid is less than 50 μS / cm. Use a quartz container to hold the filter cake and put it into a calciner, heat up to 1050°C and calcinate for 8 hours, and then cool down to room temperature to obtain low-chlorine high-purity germanium dioxide. The impurity content is as follows: figure 1 shown.
Embodiment 3
[0035] Add 30L of pure water into the hydrolysis kettle, add 96mol of germanium dioxide raw material into the pure water, stir and disperse. Then add 4.0L ammonia water, and stir for 4h after adding. The resulting solution was heated up to 55°C, and acetic acid was added to the solution until the free acidity reached 3.0 mol / L, then kept stirring at 55°C for 4 hours, and filtered to obtain a filter cake. Then add 30L of pure water into the hydrolysis tank, and wash the filter cake several times until the conductivity of the washing solution is less than 50 μS / cm. Put the filter cake in a quartz container and put it into a calciner, heat up to 900°C and calcinate for 18 hours, and then cool down to room temperature to obtain low-chlorine high-purity germanium dioxide. The impurity content is as follows: figure 1 shown.
[0036] The method for dechlorinating germanium dioxide of the invention has the advantages of simple and convenient operation and low cost in the production ...
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