Method of purifying niobium compound and/or tantalum compound
A technology of tantalum compounds and niobium compounds, which is applied in the fields of niobium compounds, tantalum compounds, chemical instruments and methods, etc., and can solve problems such as difficulty in obtaining absorbents, dissolution of organic solvents into water, etc.
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Embodiment 1
[0022] After adding 500g of 75%-HF or 495g of 75%-HF and 5g of 98% sulfuric acid into a transparent PFA container with a capacity of 1L with a stirrer, add the metal impurities shown in Table 1 within about 3 hours while stirring. After adding 150 g of ferroniobium alloy, it was stirred at room temperature. Thereafter, a niobium hydrofluoric acid solution of approximately 300 g / L in terms of niobium element was prepared by removing insoluble matter by filtration.
[0023] Thereafter, while stirring the above-mentioned niobium hydrofluoric acid solution, carry out crystallization at -20°C for 2 hours, then take out the crystallization through filtration, add 28% ammonia water 65g to this niobium crystal solution, and make niobium After precipitation as niobium hydroxide, ammonium fluoride and the like were removed by filtration to obtain niobium hydroxide.
[0024] The obtained niobium hydroxide was fired in an electric furnace at 1000° C. to obtain niobium oxide. The obtaine...
Embodiment 2
[0026] Put 500g of 100%-HF (anhydrous hydrofluoric acid), 75%-HF, 50%-HF or 30%-HF into a transparent PFA container with a capacity of 1L with a stirrer, and keep it at -20°C or room temperature While stirring, 150 g of niobium oxide containing metal impurities shown in Table 2 was added over about 3 hours, followed by stirring. Furthermore, the 50%-HF and 30%-HF solutions were stirred under reflux at 70°C. Thereafter, a niobium hydrofluoric acid solution of approximately 300 g / L in terms of niobium element was prepared by removing a small amount of insoluble matter by filtration. Similarly, niobium oxide was dissolved after adding 495 g of 50%-HF and 5 g of 98% sulfuric acid or 69% nitric acid to a transparent PFA container having a stirrer and a capacity of 1 L.
[0027] The niobium oxide used above is a 98% niobium oxide industrial product after pretreatment to reduce the concentration of impurities.
[0028] Here, the above-mentioned prepared solutions were analyzed with...
Embodiment 3
[0032] Add 50%-HF 500g to a transparent PFA container with a capacity of 1L equipped with a stirrer, and add 130g of tantalum oxide containing metal impurities shown in Table 3 while stirring at room temperature, and then add at 70°C. Stir at warm reflux for about 5 hours.
[0033] Thereafter, it is prepared as a tantalum hydrofluoric acid solution in which a small amount of insoluble matter is removed by filtration, and converted to about 300 g / L of tantalum element. Similarly, tantalum oxide was dissolved after adding 495 g of 50%-HF and 5 g of 98% sulfuric acid or 69% nitric acid to a transparent PFA container having a stirrer and a capacity of 1 L. Furthermore, the tantalum oxide used this time is a 98% tantalum oxide industrial product that has been pre-treated to reduce the concentration of impurities.
[0034] Thereafter, while stirring the above-mentioned tantalum hydrofluoric acid solution or tantalum mixed acid solution, carry out crystallization at -20°C for 2 hour...
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