Preparation method of fluorine-containing nano-SiO2 microspheres with photo-initiating activity and nano-SiO2
A technology of photoinitiation and photoinitiator, which is applied in the field of polymer material synthesis, can solve the problems of oxygen inhibition and coating surface properties to be improved, and achieve the effect of improving stability, good gloss and good weather resistance
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Embodiment 1
[0032] A fluorine-containing nano-SiO with photoinitiated activity 2 The preparation method of microspheres comprises the following steps:
[0033] (1) Add 100mL of ethanol, 2.5g of ammonia water to a 250mL three-necked flask, stir after 16.2g of deionized water, mix well, wherein alcohols are the reaction medium, take 44.274g of trimethoxypropylamine silane and set it In a constant pressure funnel, it was added dropwise to the above mixed solution within 1 hour at room temperature. After the dropwise addition, the temperature was raised to 45 °C, and the reaction was stirred for 6 hours to obtain nano-silica microspheres with polymerizable groups on the surface. solution; the concentrations of ammonia, water and trimethoxypropylaminosilane in the whole solution are 0.9mol / L, 5.52mol / L and 1.2mol / L respectively.
[0034] (2) Pour nitrogen into the nano-silica microsphere solution prepared in step (1), use a constant pressure dropping funnel, and dropwise add 56.8 g of heptade...
Embodiment 2
[0045] A fluorine-containing nano-SiO with photoinitiated activity 2 The preparation method of microspheres comprises the following steps:
[0046] (1) Add 100 mL of methanol, 1 g of ammonia water, and 10 g of deionized water to a 250 mL three-necked flask with mechanical stirring, mix well, take 22.137 g of trimethoxypropylaminosilane and place it in a constant pressure funnel, dropwise It was added to the above mixed solution within 1 hour at room temperature. After the dropwise addition was completed, the temperature was raised to 40 °C, and the reaction was stirred for 6 hours to obtain a nano-silica microsphere solution with polymerizable groups on the surface. The concentration of propylaminosilane in the whole solution is 0.44mol / L, 4.17mol / L and 0.75mol / L respectively;
[0047] (2) Pour nitrogen into the nano-silica microsphere solution prepared in step (1), use a constant pressure dropping funnel, and add 56.8 g of heptadecafluorodecyltriethoxysilane dropwise to the ...
Embodiment 3
[0058] A fluorine-containing nano-SiO with photoinitiated activity 2 The preparation method of microspheres comprises the following steps:
[0059] (1) Add 100 mL of isopropanol, 0.5 g of ammonia water, and 18 g of deionized water into a 250 mL three-necked flask with mechanical stirring, and mix well. 33.205 g of γ-mercaptopropyltrimethoxysilane was placed in a constant pressure funnel, and added to the above mixed solution in a dropwise manner within 1 h at room temperature. After the dropwise addition, the temperature was raised to 60 °C, and the reaction was stirred for 3 h to obtain a nano-silica microsphere solution with polymerizable groups on the surface; the concentrations of ammonia, water, and γ-mercaptopropyltrimethoxysilane in the entire solution were respectively. are 0.19mol / L, 6.72mol / L and 1mol / L;
[0060] (2) Pour nitrogen into the nano-silica microsphere solution prepared in step (1), use a constant pressure dropping funnel, and add 56.8 g of heptadecafluo...
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