Superfine barium titanate powder and preparation method thereof
A technology of fine barium titanate and powder, which is applied in the direction of titanate, alkaline earth metal titanate, chemical instruments and methods, and can solve the problems of large equipment investment, high production cost, and high technical difficulty
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[0030] The invention provides a kind of preparation method of superfine barium titanate powder, comprises the following steps:
[0031] A) TiCl with a concentration of 0.1 to 1.0 mol / L 4 The solution is hydrolyzed to obtain TiO 2 Colloidal solution;
[0032] B) the TiO 2 The colloidal solution is removed and concentrated to obtain a colloidal solution with a mass content of 8% to 28%;
[0033] C) After dissolving the barium source into an alkaline solution with a temperature ≥ 80°C and a pH value ≥ 12, mix it with the colloid solution obtained in step B), react at 100-110°C, and dry the obtained product to obtain super Fine barium titanate powder.
[0034] In the present invention, TiCl with a concentration of 0.1 to 1.0 mol / L is first 4 The solution is hydrolyzed to obtain TiO 2 colloidal solution.
[0035] Specifically, including:
[0036] TiCl with a concentration of 0.1-1.0mol / L 4 The solution is heated to the hydrolysis temperature for hydrolysis to obtain TiO 2...
Embodiment 1
[0085] 1) Take 0.4mol / L TiCl 4 Pour 5L of the solution into a four-neck flat-bottomed flask, heat up to 104°C at a rate of 2°C / min, and hydrolyze at 104°C for 60 minutes, then cool to room temperature at a rate of 2°C / min to obtain TiO 2 Colloidal solution;
[0086] 2) adopt Mitsubishi chemical PA316 anion resin to describe TiO 2 colloidal solution for impurity removal, the anion resin and the TiO 2 The dosage ratio of the colloidal solution is 1395g: 1L. When the pH value of the colloidal solution is 4.02, stop removing chlorine. The concentration of chloride ions in the colloidal solution is 315ppm. Concentrate using Asahi Kasei hollow fiber membranes to obtain a colloidal solution with a mass content of 13.5%. ;
[0087] 3) Prepare 1.5L of 2mol / L sodium hydroxide solution (pH value is 14), heat the electric heating mantle to 90°C, drop in 350g of octahydrate barium hydroxide powder, stir and dissolve, then drop into the colloidal solution obtained in step 2), The molar ...
Embodiment 2
[0100] 1) Take 0.1mol / L TiCl 4 Pour 5L of the solution into a four-neck flat-bottomed flask, heat up to 104°C at a rate of 2°C / min, and hydrolyze at 104°C for 60 minutes, then cool to room temperature at a rate of 2°C / min to obtain TiO 2 Colloidal solution;
[0101] 2) adopt Mitsubishi chemical PA316 anion resin to describe TiO 2 colloidal solution for impurity removal, the anion resin and the TiO 2 The dosage ratio of the colloidal solution is 349g: 1L. When the pH value of the colloidal solution is 4.13, the dechlorination is stopped. The chloride ion concentration of the colloidal solution is 265ppm. Concentrate using the Asahi Kasei hollow fiber membrane to obtain a colloidal solution with a mass content of 16.3%. ;
[0102] 3) Prepare 1.5L of 2mol / L sodium hydroxide solution (pH value is 14), heat the electric heating mantle to 90°C, drop in 350g of octahydrate barium hydroxide powder, stir and dissolve, then drop into the colloidal solution obtained in step 2), The m...
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