Processes for the hydrothermal production of titanium dioxide
A technology of titanium oxyhydroxide and oxide, which is applied in the direction of titanium dioxide, titanium oxide/hydroxide, and nanostructure manufacturing, and can solve problems such as the composition of crystallization aids that are not mentioned
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Embodiment 1
[0041] Preparation of titanyl hydroxide precipitate from reagent grade ammonium titanyl oxalate
[0042] A 4 L glass beaker was charged with a mixture containing 150 g of reagent grade ammonium titanyl oxalate monohydrate (Acros; CAS# 10580-03-7) and 1200 g of deionized water. The mixture was stirred via a magnetic stir bar for 30 minutes at room temperature and filtered through a 0.45 μm disposable nylon filter cup to remove any undissolved impurities. The filtrate was collected and transferred back into a 4 L glass beaker and heated to 80°C on a hot plate with constant stirring. Gradually add concentrated NH 4 OH (28 to 30% by weight NH 3 ; CAS#1336-21-6) to titrate the pH of the ammonium titanyl oxalate solution to 8.0 to 8.3 while maintaining the temperature of the mixture at 80°C. The reaction mixture was maintained at this temperature for an additional 15 minutes and then filtered through 24 cm #54 Whatman filter paper to obtain 463 g of precipitated titanyl hydroxide...
Embodiment 2
[0044] Hydrothermal crystallization of nanoscale rutile TiO by precipitation of titanyl hydroxide derived from reagent grade ammonium titanyl oxalate 2
[0045] A titanyl hydroxide precipitate containing 4 g of reagent grade ammonium titanyl oxalate derived titanyl oxalate (see Example 1 for precipitate preparation and characterization), 0.0102 g of ZnCl was diluted with deionized water. 2 (Reagent Grade, CAS#7646-85-7) and 3.9 g of dilute HCl solution to a concentration of 4 g TiO 2 per 100 grams of slurry. A dilute HCl solution can be prepared by mixing 2.8 g of 12.1 N reagent grade HCl solution (CAS# 7647-01-0) with 32.6 g of deionized water. The mixture containing the titanium precipitate was added to a 10 mL gold tube with a welded bottom. The top of the gold tube was then crimped and the tube was inserted vertically into a 1L Zr-702 pressure vessel. To facilitate heat transfer within the 1 L reactor, water was added to submerge the lower half of the inserted gold tub...
Embodiment 3
[0047] Hydrothermal crystallization of pigment-grade rutile TiO by titanyl hydroxide precipitation (10 mL scale) derived from reagent-grade ammonium titanyl oxalate at 250 °C 2
[0048] A titanyl hydroxide precipitate containing 4 g of reagent grade ammonium titanyl oxalate derived titanyl hydroxide (see Example 1 for precipitate preparation and characterization), 0.0582 g of ZnCl was diluted with deionized water. 2 (Reagent Grade, CAS#7646-85-7) and 2.1 g of dilute HCl solution to a concentration of 4 g TiO 2 per 100 grams of slurry. A dilute HCl solution can be prepared by mixing 2.8 g of 12.1 N reagent grade HCl solution (CAS# 7647-01-0) with 33.3 g of deionized water. The mixture containing the titanium precipitate was added to a 10 mL gold tube with a welded bottom. The top of the gold tube was then crimped and the tube was inserted vertically into a 1L Zr-702 pressure vessel. To facilitate heat transfer within the 1 L reactor, water was added to submerge the lower ha...
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