Preparation method of high-purity antimony trioxide
An antimony trioxide, high-purity technology, applied in chemical instruments and methods, antimony oxide/antimony hydroxide/antimony oxyacid, inorganic chemistry, etc. The large particle size of antimony and the large amount of leaching agent can achieve the effects of short time, improved 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 solution for impregnation, then pass chlorine gas into the solution, the flow rate of chlorine gas is 300L / h, at 70~90℃ React for 2 to 4 hours, filter and wash to obtain a mixed solution 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-mentioned 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 obta...
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 solution for impregnation, then pass chlorine gas into the solution, the flow rate of chlorine gas is 360L / h, and the React for 2 to 4 hours, filter and wash to obtain a mixed solution 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-mentioned 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...
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 solution for impregnation, then pass chlorine gas into the solution, the flow rate of chlorine gas is 280L / h, at 70-90°C React for 2 to 4 hours, filter and wash to obtain a mixed solution 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-mentioned 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 obt...
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Abstract
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