A kind of preparation method of water-soluble zirconia ceramic precursor and its solution
A technology of zirconia ceramics and precursor solutions, which is applied in the field of preparation of water-soluble zirconia ceramic precursors and their solutions, and can solve the problems of difficult control of zirconia crystal growth, poor solubility of precursors, and limitations on the preparation of zirconia ceramics. , to achieve the effect of expanding industrial application prospects, uniform reaction degree, and good water dispersibility
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Embodiment 1
[0040] 1 mol of zirconium n-propoxide was heated to 30° C., 50.00 g (0.5 mol) of acetylacetone was added dropwise, the dropping rate was controlled, the dropwise addition was completed in 2 hours, and the reaction was refluxed for 4 hours. The temperature was lowered to 40° C., and 180.00 g (10.0 mol) of water was continued to be slowly added dropwise for 3 hours. The temperature was lowered to 40° C., 184 g (4.0 mol) of formic acid was added dropwise, and after 1 hour of dropping, the temperature of the system was distilled to 110° C. under atmospheric pressure. The temperature was lowered to room temperature, and the solvent was removed under reduced pressure at 70° C. to obtain a zirconia polymer ceramic precursor (PNZ).
[0041] The prepared PNZ polymer solid was dissolved in water to prepare a solution with a mass fraction of 60%, and the photo is attached figure 1, the measured solution viscosity is 1000mPa.s. At room temperature, this precursor aqueous solution is unif...
Embodiment 2
[0043] Heat 1 mol of zirconium n-propoxide to 30°C, add 70.00 g (0.7 mol) of acetylacetone dropwise, control the rate of addition, finish adding dropwise in 2 hours, and react under reflux for 4 hours. The temperature was lowered to 40°C, and the solution of 180.00 g (10.0 mol) of water and 180 g (2.0 mol) of oxalic acid was continued to be slowly added dropwise, and the reaction was continued for 2 hours after the dropwise addition was completed in 3 hours. Atmospheric pressure distillation to the system temperature of 110°C after dropping. The temperature was lowered to room temperature, and the solvent was removed under reduced pressure at 70° C. to obtain a zirconia polymer ceramic precursor (PNZ).
[0044] Use the prepared PNZ polymer solid to configure a solution with a mass fraction of 30% in water, and measure the viscosity of the solution to be 200mPa.s. See the attached photo for the photo after it has been stored for 3 months. figure 2 ; At room temperature, this ...
Embodiment 3
[0046] Heat 1 mol of zirconium n-propoxide to 45°C, add 90.00 g (0.9 mol) of acetylacetone dropwise, control the rate of addition, finish adding dropwise in 2 hours, and then reflux for 3 hours. The temperature was lowered to 60° C., and the mixed solution of 144.00 g (8.0 mol) of water and 268.18 g (2 mol) of malic acid was continued to be slowly added dropwise, and the reaction was heated for 2 hours after the dropwise addition was completed in 3 hours. Atmospheric pressure distillation to the system temperature of 115°C after dropping. The temperature was lowered to room temperature, and the solvent was removed under reduced pressure at 80° C. to obtain a zirconia polymer ceramic precursor (PNZ).
[0047] Use the prepared PNZ polymer solid to configure a solution with a mass fraction of 40% in water. The measured solution viscosity is 400mpa.s. At room temperature, this precursor aqueous solution is uniform and stable and the precursor solid can be dissolved in acetone, tol...
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