A kind of preparation method of ammonium dithiotungstate
A technology of ammonium dithiotungstate and ammonium sulfide, which is applied in chemical instruments and methods, tungsten compounds, inorganic chemistry, etc., can solve problems such as being unable to adapt to industrial applications, unfavorable for industrialized large-scale production, and harsh operating conditions. , to achieve high industrial application prospects, less waste discharge, and environmental friendliness.
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Embodiment 1
[0022] Add 3.7 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, 1.2 g of yellow needle-like crystals can be obtained, with a yield of 99% (calculated as ammonium metatungstate).
[0023] The elemental analysis data of the thus prepared ammonium dithiotungstate sample are shown in Table 1.
[0024] Table 1 Elemental analysis data of ammonium dithiotungstate sample
[0025] Elemental composition, M%
[0026] The results in Table 1 show that the elemental analysis results of ammonium dithiotungstate...
Embodiment 2
[0028] Add 326.4g 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 122.3g 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 8 hours, then use a Buchner funnel to suction filter, and wash the crystals with cold distilled water (3×100mL) and ethanol (3×100mL) respectively After three times, it was dried at room temperature for 4 hours to obtain 114.9 g of yellow needle-like crystals with a yield of 98% (calculated as sodium tungstate).
[0029] The elemental analysis data of the thus prepared ammonium dithiotungstate sample are shown in Table 2.
[0030] Table 2 Elemental analysis data of ammonium dithiotungstate sample
[0031] Elemental composition, M%
[0032]The results in Table 2 show that the elemental analysis results of ammonium dith...
Embodiment 3
[0034] Add 2967kg of ammonium sulfide solution with a sulfur content of 8% (mass fraction) into a synthetic kettle with mechanical agitation, then add 1000kg of ammonium metatungstate to it, blow nitrogen into it during the reaction, and heat up to 60 with an oil bath. ℃, stirred and reacted for 1 hour, added 572kg of ammonium acetate, allowed to stand for crystallization for 24 hours, then suction filtered, washed the crystals three times with cold distilled water (3×10000mL) and ethanol (3×10000mL), and dried at room temperature for 12 hours , 1161kg of yellow needle-like crystals can be obtained, with a yield of 99% (calculated as ammonium metatungstate).
[0035] The elemental analysis data of the thus prepared ammonium dithiotungstate sample are shown in Table 3.
[0036] Table 3 Elemental analysis data of ammonium dithiotungstate sample
[0037] Elemental composition, M%
[0038] The results in Table 3 show that the elemental analysis results of ammonium dithi...
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