Colloidal antimony oxide dry powder with low volatility at high temperature and preparation method thereof
A low-volatility, antimony dry powder technology, applied in chemical instruments and methods, inorganic chemistry, antimony compounds, etc., can solve the problems that affect the appearance and use of the product, the finished product has micropores, and the surface is not smooth, and achieves excellent high-temperature heating performance. The effect of high adhesion and large surface area
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Embodiment 1
[0028] Preparation of antimony pentoxide hydrosol: Add 584mL water into a beaker, start stirring, add 0.7g phosphoric acid, then add 146g Sb 2 o 3 Slurry, then dropwise add 131.4gH 2 o 2 (concentration is 27.5wt%), at 30 ℃, react for 90min, get colloidal Sb 2 o 5 615mL, of which: Sb 2 o 5 : 259.2g / L, Sb 2 o 3 : 0.28g / L.
[0029] Preparation of colloidal antimony oxide dry powder with low volatility at high temperature:
[0030] (1) Reduction: At a temperature of 30°C, adjust the pH value of 615mL of antimony pentoxide hydrosol to 7.1 with NaOH, then add 14.6g of hydrazine hydrate for partial reduction, and react at 80°C for 30 minutes to obtain antimony oxide sol 600mL, of which: Sb 2 o 5 : 199.78g / L, Sb 2 o 3 : 59.48g / L;
[0031] (2) Removal of alkali metal ions: Use cation exchange resin at 30°C for 30 minutes to remove Na in the antimony oxide sol obtained in step (2). + , the pH value in the sol after ion exchange is 6.0;
[0032](3) Drying: Spray-dry the a...
Embodiment 2
[0035] Preparation of antimony pentoxide hydrosol: Add 1460mL water into a beaker, start stirring, add 4.4g phosphoric acid, then add 292g Sb 2 o 3 Slurry, then dropwise add 292gH 2 o 2 (concentration is 27.5wt%), at 50 ℃, reacted for 120min to get colloidal Sb 2 o 5 1600mL, of which, Sb 2 o 5 : 199.2g / L, Sb 2 o 3 : 0.27g / L.
[0036] Preparation of colloidal antimony oxide dry powder with low volatility at high temperature:
[0037] (1) Reduction: At a temperature of 40°C, adjust the pH value of 1600mL of antimony pentoxide hydrosol to 7.5 with KOH, then add 35.0g of hydrazine hydrate for partial reduction, and react at 90°C for 50 minutes to obtain antimony oxide sol 1550mL, of which: Sb 2 o 5 : 155.48g / L, Sb 2 o 3 : 45.12g / L;
[0038] (2) Removal of alkali metal ions: use cation exchange resin at 45°C for 40 minutes to remove K in the antimony oxide sol obtained in step (2) + , the pH value in the sol after ion exchange is 6.5;
[0039] (3) Drying: Spray-dry ...
Embodiment 3
[0042] Preparation of antimony pentoxide hydrosol: Add 4664mL water into a beaker, start stirring, add 17.5g phosphoric acid, then add 583g Sb 2 o 3 Slurry, add dropwise 549.7gH 2 o 2 (Concentration is 35wt%), at 90°C, react for 180min to get colloidal Sb 2 o 5 4850mL, of which, Sb 2 o 5 : 131.1g / L, Sb 2 o 3 : 0.25g / L.
[0043] Preparation of colloidal antimony oxide dry powder with low volatility at high temperature:
[0044] (1) Reduction: At a temperature of 50°C, adjust the pH value of 4850mL of antimony pentoxide hydrosol to 8.0 with NaOH, then add 87.5g of hydrazine hydrate for partial reduction, and react at 95°C for 60 minutes to obtain antimony oxide sol 4750mL, of which: Sb 2 o 5 : 102.46g / L, Sb 2 o 3 : 28.49g / L;
[0045] (2) Removal of alkali metal ions: Use cation exchange resin at 55°C for 60 minutes to remove Na in the antimony oxide sol obtained in step (2) + , the pH value in the sol after ion exchange is 7.0;
[0046] (3) Drying: Spray-dry the ...
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