Titanium oxide black pigment and preparation method thereof
A titanium oxide, black pigment technology
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[0015] A preparation method of titanium oxide black pigment, comprising the steps of:
[0016] The titania nuclei are wet-milled, and Al is coated on the titania nuclei after wet milling by a sol-gel method. 2 o 3 film and SiO 2 membrane;
[0017] Coating the Al by sol-gel method 2 o 3 For film, the heating rate of calcination is 2°C / min~7°C / min, the temperature of constant temperature calcination is 350°C~800°C, and the time is 1h~10h;
[0018] Coating the SiO with the sol-gel method 2 For the film, the heating rate of calcination is 2°C / min to 7°C / min, the temperature of constant temperature calcination is 100°C to 600°C, and the time is 1h to 10h.
[0019] The process conditions of the sol-gel method are easy to control, and can be operated at lower temperatures and milder conditions. The content of various components can be precisely controlled and uniformly mixed at the molecular level, thereby effectively controlling the particle size and morphology. and nature. ...
Embodiment 1
[0047] This embodiment provides a black titanium oxide pigment and a preparation method thereof.
[0048] Use the sol-gel method in the following sequence:
[0049] (1) Dispersion of nuclei: use 50 parts by mass of Ti with a particle size of 35nm to 91nm 2 o 3 and 50 mass parts Ti 3 o 5 As titanium oxide nuclei, ethanol was added to the nuclei and subjected to wet grinding to obtain intermediate I.
[0050] (2) Coating Al 2 o 3 Membrane: uniformly mix intermediate I with aluminum isopropoxide, ethanol, and deionized water, add hydrochloric acid and / or ammonia water, control the pH to 5-6, react for 1 hour, heat to 90°C and dry at constant temperature for 3 hours. Heating to 600°C at a heating rate of 5°C / min in the atmosphere, and calcination at a constant temperature for 8 hours to obtain intermediate II;
[0051] Wherein, the molar ratio of aluminum isopropoxide to deionized water is 1:50.
[0052] (3) coated SiO 2 Membrane: Mix intermediate II with tetraethyl ortho...
Embodiment 2
[0056] This embodiment provides a black titanium oxide pigment and a preparation method thereof.
[0057] Use the sol-gel method in the following sequence:
[0058] (1) Dispersion of nuclei: use 50 parts by mass of Ti with a particle size ranging from 87nm to 137nm 2 o 3 and 50 mass parts Ti 3 o 5 As the titania nuclei, deionized water was added to the nuclei for wet grinding to obtain intermediate I.
[0059] (2) Coating Al 2 o 3 Membrane: uniformly mix intermediate I with aluminum isopropoxide, ethanol, and deionized water, add hydrochloric acid and / or ammonia water, control the pH to 8-9, react for 3 hours, heat to 80°C and dry at constant temperature for 6 hours, then Heating to 600°C at a heating rate of 5°C / min in the atmosphere, and calcination at a constant temperature for 8 hours to obtain intermediate II;
[0060] Wherein, the molar ratio of aluminum isopropoxide to deionized water is 1:50.
[0061] (3) coated SiO 2 Membrane: Mix intermediate II with tetraet...
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