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

Inactive Publication Date: 2010-03-10
EI DU PONT DE NEMOURS & CO
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

A crystallization aid is mentioned, but the co...

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  • Processes for the hydrothermal production of titanium dioxide
  • Processes for the hydrothermal production of titanium dioxide
  • Processes for the hydrothermal production of titanium dioxide

Examples

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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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Abstract

The present invention provides hydrothermal processes for the production of titanium dioxide from titanyl hydroxide. The use of specific crystallization directors, or additives, can promote the formation of rutile, anatase, or brookite. Variation of process operating parameters can lead to either pigmentary-sized or nano-sized rutile.

Description

field of invention [0001] The invention relates to a method for hydrothermally preparing titanium dioxide from titanyl hydroxide. Background of the invention [0002] Titanium dioxide (TiO 2 ) are used as white pigments in paints, plastics, paper and specialty applications. Titanium concentrate is a naturally occurring mineral containing titanium and iron with the chemical formula FeTiO 3 . [0003] Two main methods are currently used to prepare TiO 2 Pigments, as described in Haddeland, G.E. and Morikawa, S., "Titanium Pigment", SRI international Report #117 by sulfation method and as described in Battle, T.P., Nguygen, D. and Reeves, J.W., The Paul E. Queneau International Chlorination methods described in Symposium on Extractive Metallurgy of Copper, Nickel and Cobalt, Vol. I: Fundamental Aspects, Reddy, R.G. and Weizenbach, R.N. eds., The Minerals, Metals and Materials Society, 1993, pp. 925-943. [0004] Lahti et al. (GB 2221901 A) disclose a process for the prepar...

Claims

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Application Information

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IPC IPC(8): C01G23/053
CPCC01G23/053C09C1/3607C01P2002/72C01P2002/77C01P2004/64C01P2002/60C01P2004/03C01P2004/52C01P2002/54C01P2004/51C01P2004/62B82Y30/00B82B3/00C04B35/46
Inventor K·W·哈钦森S·李D·R·科宾C·托拉迪E·M·麦卡伦
Owner EI DU PONT DE NEMOURS & CO
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