Preparation method of spiropyrane type photochromic nano-composite microsphere
A nano-composite and photochromic technology, applied in the field of photochromism, can solve the problems of reduced color changing space, reduced color changing coating space, and low color changing efficiency
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Embodiment 1
[0072] Embodiment 1: Preparation of photochromic nanocomposite microspheres, photochromic coating liquid and photochromic lens
[0073] (1) Preparation of photochromic nanocomposite microspheres:
[0074] (1) Add 9.7g of zinc nitrate hexahydrate to 1600g of ethylene glycol, stir evenly, add 1.6g of sublimated sulfur powder, heat up to 150°C for 24 hours, cool to 55°C, add 85g of mercaptoethanol dropwise and stir; Then add 6.7 g of the spiropyran photochromic compound represented by formula III, stir vigorously for 30 minutes, continue to cool to room temperature, filter and wash the precipitate, and dry it in a vacuum oven at 65°C for 8 hours to obtain spiropyran coating Zinc sulfide nanospheres;
[0075] (2) Add 8g of spiropyran-coated zinc sulfide nanospheres and 8.2g of diphenylmethane-4,4'-diisocyanate (MDI) to 1000g of butyl acetate solvent, stir well, and then add 7g to mix the reaction agent (1.2g n-butanol, 5.8g polytetrahydrofuran ether glycol), 18g Tween80, the tem...
Embodiment 2
[0090] (1) Preparation of photochromic nanocomposite microspheres:
[0091](1) Add 6.5g of zinc nitrate to 1600g of ethylene glycol, stir evenly, add 1.7g of sublimated sulfur powder, heat up to 150°C for 24 hours, cool to 55°C, add 70g of mercaptoethanol dropwise and stir; then add 3.5 g of spiropyran photochromic compound (I), vigorously stirred for 30 minutes, cooled to room temperature, filtered and washed the precipitate, and dried in a vacuum oven at 65° C. for 8 hours to obtain spiropyran-coated zinc sulfide nanospheres;
[0092] (2) Get 5.5g spiropyran-coated zinc sulfide nanospheres, 5g MDI is added in 1000g butyl acetate solvent, after stirring evenly, add 5.5g mixed reactants (1.0g n-butanol, 4.5g polytetrahydrofuran ether) Diol), 20g Tween80, keep the temperature at 25°C, prepolymerize at 500r / min for 50min, add 6g chain extender (4.5g ethylene glycol, 1.5g ethylenediamine), 0.1g DBTL, heat to 65°C Polymerization chain extension reaction was carried out for 15 min...
Embodiment 3
[0101] (1) Preparation of photochromic nanocomposite microspheres:
[0102] (1) Add 11g of zinc nitrate hexahydrate to 1600g of ethylene glycol, stir evenly, add 3g of sulfur powder, heat up to 145°C for 24 hours, cool to 50°C, add 92g of mercaptoethanol dropwise and stir; then add 8g The spiropyran photochromic compound (I), vigorously stirred for 35 minutes, continued to cool to room temperature, filtered and washed the precipitate, and dried in a vacuum oven at 60°C for 9 hours to obtain spiropyran-coated zinc sulfide nanospheres;
[0103] (2) Get 10g spiropyran-coated zinc sulfide nanospheres, 10.8g m-xylylene diisocyanate (XDI) and join in 1000g butyl acetate solvent, after stirring evenly, add 7.4g mixed reaction agent (1.0 g n-butanol, 6.4g polytetrahydrofuran ether glycol), 16g Tween80, keep the temperature at 25°C, prepolymerize at 600r / min for 60min, add 8g chain extender (5.5g ethylene glycol, 2.5g ethylenediamine) , 0.2g DBTL, heated to 60°C for polymerization cha...
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