Preparation method of ammonium tetrathiotungstate
A kind of ammonium tetrathiotungstate and its preparation method are applied in the fields of tungsten compounds, chemical instruments and methods, inorganic chemistry, etc., which can solve the problems of not being well adapted to industrial applications, not too high yield, and short reaction time, etc. problems, to achieve the effect of high industrial application prospects, simple process conditions, and less waste discharge
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Embodiment 1
[0023] Add 8.9 g of ammonium sulfide solution with a sulfur content of 8% (mass fraction) into a single-necked round-bottomed flask equipped with a magnet, then add 1 g of ammonium metatungstate to it, vacuumize during the reaction, and stir at room temperature for 5 After 1 hour, add 0.1 g of ammonium chloride, let it stand for crystallization for 0.5 hour, then use a Buchner funnel to suction filter, wash the crystals three times with cold distilled water (3×10 mL) and ethanol (3×10 mL), and dry at room temperature for 2 After 1 hour, 1.3 g of yellow needle-like crystals can be obtained, with a yield of 99% (calculated as ammonium metatungstate).
[0024] The elemental analysis data of the thus prepared ammonium tetrathiotungstate sample are shown in Table 1.
[0025] Table 1 Elemental analysis data of ammonium tetrathiotungstate sample
[0026] Elemental composition, M%
[0027] The results in Table 1 show that the elemental analysis results of ammonium tetrathio...
Embodiment 2
[0029] Add 1186.9 g of ammonium sulfide solution with a sulfur content of 8% (mass fraction) into a single-necked round-bottomed flask equipped with a magnet, then add 122.3 g of sodium tungstate to it, blow in argon during the reaction, and heat up After stirring for 0.5 hours to 100°C, add 427g of ammonium bisulfate, let it stand for crystallization for 24 hours, then filter it with a Buchner funnel, and wash the crystals with cold distilled water (3×100mL) and ethanol (3×100mL) After three times, it was dried at room temperature for 8 hours to obtain 126.6 g of yellow needle-like crystals with a yield of 98% (calculated as sodium tungstate).
[0030] The elemental analysis data of the thus prepared ammonium tetrathiotungstate sample are shown in Table 2.
[0031] Table 2 Elemental analysis data of ammonium tetrathiotungstate sample
[0032] Elemental composition, M%
[0033] The results in Table 2 show that the elemental analysis results of ammonium tetrathiotung...
Embodiment 3
[0035]Add 5935 kg of ammonium sulfide solution with a sulfur content of 8% (mass fraction) into a synthetic kettle with mechanical agitation, then add 1000 kg of ammonium metatungstate to it, blow nitrogen into it during the reaction, and heat up to 60 with an oil bath. ℃, after stirring and reacting for 1 hour, add 572 kg of ammonium acetate, let it stand for crystallization for 2 hours, then filter it with suction, wash the crystals three times with cold distilled water (3×10000mL) and ethanol (3×10000mL), and dry at room temperature for 12 hours , 1279kg of yellow needle-like crystals can be obtained, with a yield of 99% (calculated as ammonium metatungstate).
[0036] The elemental analysis data of the thus prepared ammonium tetrathiotungstate sample are shown in Table 3.
[0037] Table 3 Elemental analysis data of ammonium tetrathiotungstate sample
[0038] Elemental composition, M%
[0039] The results in Table 3 show that the elemental analysis results of amm...
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