The object of the present invention is to provide a kind of method for preparing Tin Oxide, and its operation is simple, and process parameter is easy to control, and cost is low, and the stannous oxide purity that makes is high, can reach more than 99%, crso.02%, product dissolves in formazan The solution was clear after sulfanic acid.
The main technical scheme adopted to realize the object of the present invention is: 1. neutralization reaction: the Tin Oxide of crystallization and sodium carbonate are dissolved into solution, while stirring, sodium carbonate solution is gradually added in the tin protochloride solution on the one hand, and the reaction terminal pH Value is 6～7, and reaction solution has white precipitate to separate out;
② Transformation reaction: immediately heat the neutralized reactant, add sodium hydroxide aqueous solution to the material at the same time, keep it in a boiling state, and the conversion is completed when the white precipitate is transformed into a blue-black precipitate;
③ Washing and drying: After the conversion, the reactant is washed with water to remove cr, until the concentration of cr is less than 0.2%, adding an antioxidant, and after the product is filtered, it is heated and vacuum-dried to obtain stannous oxide.
Concrete technical scheme of the present invention also includes:
During neutralization reaction, the weight percent concentration of Tin Oxide solution is 30%～50%, sodium carbonate solution concentration 18～22%; During conversion reaction, sodium hydroxide solution concentration is 4%～15%, the pH of control reaction solution Value is 10～12, keeps reaction solution boiling 1h.
In the washing and drying process of the present invention, the antioxidant added after washing is cresol sulfonic acid, and the amount added is 2ml antioxidant for every 500g crystallized Tin Oxide, and the drying is at 80°C. C~100. Under C, the time is 2h～3h.
Compared with traditional production methods, the present invention has the following advantages:
1. Adopting one-step neutralization conversion, the production process is simplified, and the direct recovery rate is improved. The direct recovery rate of the traditional production method is about 96%, and the direct recovery rate of the present invention can reach more than 98%. 2, use sodium hydroxide instead to convert, strengthen the pH value during conversion, make the product conversion complete, improve the main content of the product, the main content of the traditional production method is about 98%, and the main content of the product produced by the present invention is greater than 99% %.
3, after the present invention has added antioxidant, the stability of product improves, and after being dissolved in 30% methanesulfonic acid solution, solution is clear.