Crystallization method of ammonium paratungstate
A technology of ammonium paratungstate and ammonium paratungstate, applied in the field of ammonium paratungstate crystallization, can solve the problems such as unseen research on ammonium paratungstate crystallization, inability to obtain large particles of ammonium paratungstate, uneven distribution, etc., to achieve coarse particles, controllable particle size, simple and easy process Effect
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Embodiment 1
[0013] Preparation density 1.25g / cm 3 , ammonium tungstate solution with a volume of 1.01 and a pH value of 8.0 was added to a 3l three-necked flask and heated by an electric heating mantle. When boiling reaches a supersaturated state, or when tiny grains appear, or when the density reaches 1.38g / cm 3 20 g of ammonium paratungstate seed crystals with a Fischer particle size of 30 μm were added to the solution. Keep the temperature at 95°C, return to the boiling state after 40 minutes, then add dilute ammonia water (pH value 11) dropwise to adjust the pH value of the ammonium tungstate solution, and keep the pH value of the solution at 8.0. Evaporate until the mother liquor density is 1.08g / cm 3 time, discharge, filter, wash once with dilute ammonia water, wash twice with deionized water, and finally dry at 90°C.
[0014] The produced ammonium paratungstate product has a Fischer particle size > 45 μm, normal distribution, intact crystal form and smooth surface.
Embodiment 2
[0016] Preparation density 1.28g / cm 3 , ammonium tungstate solution with a volume of 1.01 and a pH value of 8.5 was added to a 31 three-necked flask and heated by an electric heating mantle. When boiling reaches a supersaturated state, or when tiny grains appear, or when the density reaches 1.38g / cm 3 10 g of ammonium paratungstate seed crystals with a Fischer particle size of 35 μm were added to the solution. Keep the temperature at 93°C, return to the boiling state after 30 minutes, then add dilute ammonia water (pH value 12) dropwise to adjust the pH value of the ammonium tungstate solution, and keep the pH value of the solution at 8.5. Evaporate until the mother liquor density is 1.10g / cm 3 time, discharge, filter, wash twice with dilute ammonia water, then wash twice with deionized water, and finally dry at 90°C.
[0017] The produced ammonium paratungstate product has a Fischer particle size > 45 μm, normal distribution, intact crystal form and smooth surface.
Embodiment 3
[0019] Industrial production
[0020] (1) Make the density 1.30g / cm 3 , volume 3.5m 3 , the ammonium tungstate solution with a pH value of 9.0 is pumped into the evaporative crystallization kettle;
[0021] (2) Start stirring, slowly open the steam valve, after the solution boils, adjust the steam valve, and evaporate to boiling;
[0022] (3) When it reaches the supersaturated state, or when tiny grains appear, or the density reaches 1.38g / cm 3 , add 15 kg of ammonium paratungstate seed crystals with a particle size of 40 μm, and keep the solution temperature at 90 ° C for 20 min;
[0023] (4) Open the dilute ammonia water pipeline in the head tank, add ammonia water (pH value 13) to the solution, and adjust the pH value of the ammonium tungstate solution to 8.0;
[0024] (5) Evaporate until the density of the mother liquor is 1.09g / cm 3 , discharge, filter, wash 2 times with dilute ammonia water, then wash 3 times with deionized water;
[0025] (6) Dry at 90°C.
[0026...
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