Sulfuric Acid → Titanium disulfate

Titanium-containing ore was dissolved with sulfuric acid to obtain a titanium sulfate solution. The titanium sulfate solution was hydrolyzed to obtain aqueous titanium oxide. 0.50 part by weight of ammonium phosphate, 0.30 part by weight of potassium sulfate and 0.30 part by weight of aluminum sulfate were added to 100 parts of the aqueous titanium oxide in terms of TiO2. The aqueous titanium oxide was heated in a laboratory rotating muffle furnace until a product temperature reached 1,020° C. Titanium dioxide fine particles formed were cooled to room temperature, and observed with a transmission electron microphotograph. As a result, it was found that the fine particles are anatase type particles having an average primary particle size of 0.13 μm. 15 parts by weight of the titanium dioxide fine particles as a surface-treated white pigment, 5 parts by weight of a polyoxyalkylene-added polyalkylene amine (DISCOL N-518, a product of Dai-Ichi Kogyo Seiyaku Co., Ltd.) as a dispersant, and 80 parts by weight of diethylene glycol diethyl ether were mixed to obtain a slurry. Zirconia beads (1.0 mm diameter) in an amount of 1.5 times the amount of the slurry were charged, and dispersion was conducted for 2 hours with a sand mill (a product of Yasukawa Electric Corporation). The beads were removed to obtain a monomer dispersion B containing 60 wt % of the titanium dioxide fine particles. Using the monomer dispersion B containing 60 wt % of the titanium dioxide fine particles, White Ink Composition 6 (Comparative Example 3) was prepared with the following composition. Specifically, diethylene glycol diethyl ether, γ-butyrolactone, tetraethylene glycol dimethyl ether and a surfactant were dispensed in a vessel, and stirred and mixed for 30 minutes with a magnetic stirrer to sufficiently mix. 40 parts by weight of the dispersion B were added to the resulting mixture, followed by stirring and mixing for 1 hour. A product obtained was filtered using a 10 μm PTFE-made membrane filter to obtain White Ink Composition 6 (Comparative Example (2-3)).

ORD record

ord-04876af8b3b4464e834a5318b1a4a4bd

Source dataset

uspto-grants-2013_05

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US08440743B2