A kind of preparation method of fluorescent polyurethane emulsion
A polyurethane emulsion and fluorescence technology, which is applied in the field of preparation of fluorescent polyurethane emulsion, can solve the problems of insufficient brightness of the dyed object, less amount of dye monomer, and low solid content, and achieve excellent light stability and thermal stability, fluorescence The effect of uniform group distribution and high fluorescence quantum yield
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Embodiment 1
[0045]Into a 250ml flask equipped with a thermometer, a stirrer, a reflux condenser and a dropping funnel, add 50g of polyoxypropylene glycol, and dehydrate for 1.5h at 110°C and 0.1MPa. Cool to 70°C by blowing nitrogen gas, add 26g of diisocyanate TDI and 0.02g of dibutyltin dilaurate and react at 90°C for 2 hours. Add 2g of diethylene glycol and react at 80°C for 2 hours, then add 8g of N-methyldiethanolamine and 10g of N-methylpyrrolidone, react at 80°C for 4 hours, cool down to 40°C, add 30g of acetone, and then add 4.5g of ice Acetic acid, reacted for 30 minutes. Transfer to the emulsification tank, under the condition of 1500 rpm, add 8g of 4-amino-N-cyclohexane-1,8 naphthalene diimide, 140g of deionized water and 0.1g of Tween-60 at 0°C, and disperse at a high speed 30 minutes. Remove the solvent at 60°C and 0.6 MPa, and filter to obtain a cationic water-based polyurethane fluorescent emulsion. The obtained product has a fluorescence quantum yield of 0.90, a solid co...
Embodiment 2
[0047] Add 50 g of polytetrahydrofuran diol, and dehydrate for 1.5 h at 110° C. and 0.1 MPa. Cool to 70°C by blowing nitrogen gas, add 33g of isophorone diisocyanate IPDI and 0.03g of stannous octoate, and react at 90°C for 2 hours. Add 1.5g of 1,4-butanediol and 1g of trimethylolpropane and react at 80°C for 2 hours, then add 6.9g of diethanolamine and 10g of N-methylpyrrolidone, react at 80°C for 4 hours, cool down to 40°C, and add 30g of acetone , Then add 4.0g glacial acetic acid, react for 30 minutes. Transfer to an emulsification tank, add 130g of deionized water and 0.1g of octylphenol dissolved in 9g of 4-p-amino-N-dimethylphenyl-1,8 naphthalene diimide at 5°C under the condition of 1500 rpm Polyoxyethylene ether, high-speed dispersion for 30 minutes. Remove the solvent at 60°C and 0.6 MPa, and filter to obtain a cationic water-based polyurethane polymer fluorescent emulsion. The obtained product has a fluorescence quantum yield of 0.92, a solid content of 42%, and ...
Embodiment 3
[0049] Add 50g of polycaprolactone diol, 110°C, 0.1MPa, dehydration treatment for 1.5h, add 37.5g of 4,4-diphenylmethane diisocyanate MDI, react at 80°C for 4 hours, add 1g of diethylene disulfide Alcohol, 7g N-methyldiethanolamine and 10g N-methylpyrrolidone, react at 70°C for 7 hours, cool down to 30°C, add 30g methyl ethyl ketone, transfer to an emulsification tank, add 3.5g glacial acetic acid for 5 minutes, at 2000 rpm At 0°C, 150 g of deionized water and 0.1 g of octylphenol polyoxyethylene ether dissolved in 6 g of N-p-aminophenyl-1,8 naphthalene diimide were added at 0°C, and dispersed at high speed for 30 minutes. Remove the solvent at 60°C and 0.6 MPa, and filter to obtain a cationic water-based polyurethane fluorescent emulsion. The obtained product has a fluorescence quantum yield of 0.93, a solid content of 65%, and a viscosity of 30 mPa·S.
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