Preparation method of titanium dioxide/hollow microsphere composite filler
A technology of hollow microspheres and titanium dioxide, applied in the direction of reflection/signal coatings, etc., can solve problems such as difficult control of reaction speed, particle agglomeration, and uneven coating
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Embodiment 1
[0030] (1) After the surface is cleaned and degreased, the hollow ceramic microspheres are sieved to obtain hollow ceramic microspheres with a particle size distribution in the range of 150-1250nm.
[0031] (2) Add 50g of hollow microspheres to the mixed solution of 1gTx-10, 0.8g of dimethylamine and 60g of water, and stir until the mixture is uniform.
[0032] (3) Put the mixed solution obtained in step (2) into 1000 g of n-octane and stir vigorously to form an inverse microemulsion.
[0033] (4) Slowly add 20g of tetraethyl titanate to the mixture obtained in step (3) at 10°C, and at the same time turn on the ultrasonic oscillator with an oscillation frequency of 60KHz and a power of 700W, and continue the oscillation reaction for 8 hours.
[0034] (5) Take out the material obtained in step (4) and place it in a closed autoclave, add 30g of propanol and 70g of water, and heat to 165°C for a constant reaction for 16h.
[0035] (6) Wash and separate after the reaction, filter...
Embodiment 2
[0040] (1) After the surface is cleaned and degreased, the hollow ceramic microspheres are sieved to obtain hollow ceramic microspheres with a particle size distribution in the range of 150-1250nm.
[0041] (2) Add 50g of hollow microspheres into the mixed solution of 6g of Tween 20, 3g of ethylenediamine and 150g of water, and stir until the mixture is uniform.
[0042] (3) Put the mixed solution obtained in step (2) into 2000 g of cyclohexane and stir vigorously to form an inverse microemulsion.
[0043] (4) Slowly add 100g of tetraethyl titanate to the mixture obtained in step (3) at 8°C, and at the same time turn on the ultrasonic oscillator with an oscillation frequency of 40KHz and a power of 600W, and continue the oscillation reaction for 16 hours.
[0044] (5) Take out the material obtained in step (4) and place it in a closed autoclave, add 100g of ethanol and 500g of water, and heat to 175°C for a constant reaction for 36h.
[0045] (6) Wash and separate after the r...
Embodiment 3
[0047] (1) After the surface is cleaned and degreased, the hollow ceramic microspheres are sieved to obtain hollow ceramic microspheres with a particle size distribution in the range of 150-1250nm.
[0048] (2) Add 50g of hollow microspheres to the mixed solution of 10gspan-20, 2g of 1,2-propylenediamine and 300g of water, and stir until they are evenly mixed.
[0049] (3) Put the mixed solution obtained in step (2) into 3000 g of oleic acid and stir vigorously to form an inverse microemulsion.
[0050] (4) Slowly add 150g of tetrabutyl titanate into the mixture obtained in step (3) at 6°C, and at the same time turn on the ultrasonic oscillator with an oscillation frequency of 50KHz and a power of 700W, and continue the oscillation reaction for 26 hours.
[0051] (5) Take the material obtained in step (4) and place it in a closed autoclave, add 180g of ethanol and 200g of water, and heat to 195°C for a constant reaction for 40h.
[0052] (6) After the reaction, wash and separ...
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