Ammonium fluotitanate, also known as ammonium hexafluorotitanate, is commonly used in ceramics and glass as an anti-corrosive cleaner and in the manufacture of artificial gems; In addition, it can also be used to synthesize the titanium oxide precursor with special morphology. Ammonium fluoride titanate powder is stable at room temperature and insoluble in water. In the existing preparation methods of ammonium fluoride, the raw materials used are usually more complex, the cost is higher, and the preparation method is more complex.
The main purpose of the invention is to provide a preparation method of ammonium fluotitanate, which is designed to make the preparation method simple, the raw material simple and easy to obtain, and the cost is low.
To achieve the above purposes, the preparation method of ammonium fluotitanate is proposed, which includes the following steps: the titanate ester is mixed with an organic solvent to obtain the first solution; The second solution is obtained by mixing ammonium fluoride with water. The first solution and the second solution are mixed to obtain a mixed solution; The mixed solution is poured into the reactor for reaction and the mixed sediment is obtained; The mixed sediment is cooled, filtered, washed and dried to obtain ammonium fluotitanate.
Optionally, in the first solution, the quantity shares of titanates shall be 1%-2%; In the second solution, the mass concentration of ammonium fluoride is 0.1g/mL-0.3g/mL; In the mixed solution, the molality concentration of titanate is 0.03mol/L-0.06mol/L, and the molar ratio of F/Ti is 20:1-30:1.
Optionally, the moisture content of the mixed solution is 7%-9%.
Optionally, the titanate class is tebutyl titanate or isopropyl titanate.
Optionally, the organic solvent is at least one of anhydrous ethanol, n-propanol, isopropanol and n-butanol; And/or, the water is distilled water or deionized water.
Optionally, the reactor is a solvent-heat reactor with a ptFE liner.
Optionally, the solution filling degree of the solvent heat reactor is 70%-80%.
Optionally, in the process of pouring the mixed solution into the reactor for reaction, the reactor is sealed for a reaction time of 6h-12h and a reaction temperature of 140℃-180℃.
Alternatively, in the steps of cooling, filtering, washing and drying the mixed sediment, the mixed sediment is naturally cooled to room temperature, filtered, washed with anhydrous ethanol, and dried for 10h-12h at 60-100 ℃.
The invention also provides an ammonium fluoride titanate, which is prepared by the preparation method of ammonium fluoride titanate as described above.
Of the technical scheme of the invention, the use of titanate class the first solution mixed with organic solvent, ammonium fluoride is mixed with water and the second solution for the preparation of ammonium fluoride titanate material, among them, the ester titanate as titanium source, ammonia source of ammonium fluoride and fluorine source, both as a reactant, organic solvent as reaction solvent, water as ammonium fluoride solution, is obtained by solvent thermal synthesis preparation ammonium fluoride titanate of reactants, reactant ammonium fluoride titanate by cooling, filtering, washing and drying process can get pure phase of ammonium fluoride titanate powder. The preparation method is simple, and the formula material is easy to obtain and the cost is reduced.
