A kind of preparation method of high-purity antimony trioxide
A high-purity technology of antimony trioxide, applied in chemical instruments and methods, antimony oxide/antimony hydroxide/antimony oxyacid, inorganic chemistry, etc., can solve the problem that the product particle size cannot meet the requirements of fine fields, trioxide The problem of large particle size of antimony and general product purity can achieve the effect of short time, high purity and simple reagents.
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Embodiment 1
[0036] A preparation method of high-purity antimony trioxide, specifically comprising the following steps:
[0037] (1) Add 1kg of crude antimony ore (1.0%≤Pb≤2.0%) into 3L of 1mol / L hydrochloric acid for impregnation, then pass chlorine gas into the solution, the flow rate of chlorine gas is 300L / h, and react at 70-90°C After 2-4 hours, filter and wash to obtain a mixture of antimony chloride.
[0038] (2) Add 40g of iron powder (reducing agent) to the antimony chloride mixed solution, react at 70-90°C for 2-3 hours, filter and wash to obtain antimony chloride solution.
[0039] (3) Slowly add 4mol / L sodium hydroxide solution to the above antimony chloride solution until the precipitate in the solution no longer increases or the precipitate begins to decrease, that is, stop adding the sodium hydroxide solution and adjust the pH value to 8~ 9. Stir again for 1-3 hours, filter, wash, dry, and then roast in air atmosphere at 600-800°C for 3-5 hours to obtain antimony trioxide. ...
Embodiment 2
[0046] A preparation method of high-purity antimony trioxide, specifically comprising the following steps:
[0047] (1) Add 1kg of crude antimony ore (0.8%≤Pb<1.0%) into 3L of 5mol / L hydrochloric acid for impregnation, then pass chlorine gas into the solution, the flow rate of chlorine gas is 360L / h, and react at 70-90°C After 2-4 hours, filter and wash to obtain a mixture of antimony chloride.
[0048] (2) Add 45g of iron powder (reducing agent) to the antimony chloride mixed solution, react at 70-90°C for 2-3 hours, filter and wash to obtain antimony chloride solution.
[0049] (3) Slowly add 4mol / L sodium hydroxide solution to the above antimony chloride solution until the precipitate in the solution no longer increases or the precipitate begins to decrease, that is, stop adding the sodium hydroxide solution and adjust the pH value to 8~ 9. Stir again for 1-3 hours, filter, wash, dry, and then roast in air atmosphere at 600-800°C for 3-5 hours to obtain antimony trioxide. ...
Embodiment 3
[0056] A preparation method of high-purity antimony trioxide, specifically comprising the following steps:
[0057] (1) Add 1kg of crude antimony ore (0.6%≤Pb<0.8%) into 4L of 5mol / L hydrochloric acid for impregnation, then pass chlorine gas into the solution, the flow rate of chlorine gas is 280L / h, and react at 70-90°C After 2-4 hours, filter and wash to obtain a mixture of antimony chloride.
[0058] (2) Add 51g of iron powder (reducing agent) to the antimony chloride mixed solution, react at 70-90°C for 2-3 hours, filter and wash to obtain antimony chloride solution.
[0059] (3) Slowly add 4mol / L sodium hydroxide solution to the above antimony chloride solution until the precipitate in the solution no longer increases or the precipitate begins to decrease, that is, stop adding the sodium hydroxide solution and adjust the pH value to 8~ 9. Stir again for 1-3 hours, filter, wash, dry, and then roast in air atmosphere at 600-800°C for 3-5 hours to obtain antimony trioxide. ...
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