Preparation method of tungstate with hexagonal prism shape
A hexagonal prism-shaped, tungstate technology, applied in chemical instruments and methods, tungsten compounds, inorganic chemistry, etc., can solve problems such as difficulty in producing ultra-fine tungsten powder, unfavorable product performance improvement, and unstable product quality. Low production cost, high yield and good fluidity
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Embodiment 1
[0030] Add 0.15g of oleic acid and water to the ammonium tungstate solution (0.3mol of tungstate obtained after ion exchange) (the tungstate is calculated as WO3, the same below)), add 0.15g of oleic acid and water, stir and mix uniformly to obtain 300ml of initial liquid of A, and then add dilute hydrochloric acid Adjust the pH to 6.0 to form liquid A; dissolve 1.5 mol of hydrazine hydrate in water to obtain 600 ml of liquid B; add liquid A and liquid B to the reaction kettle by co-current feeding method, control the temperature at 90 ℃ to react for 1 hour, and stir Speed 120rpm, then add cold water and cool to room temperature 10℃; separate the reaction product by centrifugal filtration to obtain a tungstate filter cake; wash with water to remove impurities in the tungstate filter cake, and treat the waste water intensively; finally, dry in the air at 80℃ for 8h , To obtain hexagonal prism tungstate powder.
Embodiment 2
[0032] Add 0.16g of oleylamine and water to the crude sodium tungstate solution (0.3mol tungstate) obtained after ion exchange, stir and mix uniformly to obtain 200ml of initial liquid A, then add dilute sulfuric acid to adjust the pH to 5.0 to form liquid A ; Dissolve 2.1mol methylamine in water to obtain 700ml of liquid B; add liquid A and liquid B to the reaction kettle by co-current feeding method, the temperature of the reaction system is maintained at 50 ℃ for 6 hours, stirring speed 200rpm, and then add cold water to cool to 20℃; the reaction product is separated by centrifugal filtration to obtain the tungstate filter cake; the impurities in the tungstate filter cake are removed by washing with water, and the wastewater is concentratedly treated; finally, it is dried in the air at 70℃ for 12 hours to obtain hexagonal prism tungstate powder .
Embodiment 3
[0034] Add 0.1g of oleic acid and water to the ammonium tungstate solution (0.05mol tungstic acid radical) dissolved in ammonia to obtain 100ml of initial liquid A, then add dilute nitric acid to adjust the pH to 6.0 to form A Liquid; Dissolve 0.4mol ethylenediamine in water to obtain 400ml of liquid B; add liquid A and liquid B to the reaction kettle by co-current feeding method, control the temperature at 60℃ for 4h, stir at 60rpm, and then add cold water to cool to 30℃; The reaction product is separated by centrifugal filtration to obtain tungstate filter cake; the impurities in the tungstate filter cake are removed by washing with water, and the waste water is concentratedly treated; finally, it is dried in the air at 60℃ for 6 hours to obtain hexagonal prism tungstate powder .
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