Polyurethane high-refractive-index resin and preparation method thereof
A technology of polyurethane and resin, which is applied in the field of polyurethane high-refractive resin and its preparation, and can solve problems such as poor anti-yellowing performance, low refractive index, and low electron density
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[0091] The present invention also provides a method for preparing the polyurethane high-refractive resin described in the above technical solution, comprising the following steps:
[0092] a) Mixing bridged isocyanate, polythiol, UV absorber, phosphate release agent, organotin catalyst and antioxidant to obtain a reaction mixture; the bridged isocyanate has formula (I), formula (II) , formula (III), formula (IV), formula (V) or the structure shown in formula (VI):
[0093]
[0094]
[0095] In formula (I) ~ formula (VI), R 1 Independently selected from -CH 2 -, -S-, -Se-, -CH 2 CH 2 -or-CH 2 CH 2 CH 2 -;
[0096] In formula (IV) ~ formula (VI), R 2 independently selected from -O-, -S-, -Se- or -CH 4 CH 4 -;
[0097] b) injecting the reaction mixture obtained in step a) into a mold through a filter membrane, performing first curing, and performing second curing after demolding to obtain a polyurethane high-refractive resin.
[0098] In the invention, firstly, ...
Embodiment 1
[0114] (1) Add 958 g of o-dichlorobenzene in the four-necked flask, add 154 g of bis(aminomethyl) norbornane (containing isomer mixture) and 700 g of o-dichlorobenzene in the raw material pipe; then hydrogen chloride gas is pressurized to 0.1MPa, the temperature of the reaction vessel is raised to 120°C, and then hydrogen chloride gas is blown in at a rate of 50g / h, and dilute triethylamine is added to the raw material pipe at a rate of 428.1g / h, and the reaction is kept for 1 hour to obtain the hydrochloride reaction material The hydrochloride reaction material that obtains is heated up to 160 DEG C again, the solid phosgene (50%) that carbon disulfide dissolves is added to reaction solution with the speed of 200g / h, 160 DEG C of insulations 6 hours, utilize nitrogen to purge after reaction finishes. Reaction gas, finally through underpressure distillation, obtains the bridge type isocyanate with formula (I-1) structure, and its infrared spectrogram sees figure 1 shown;
[0...
Embodiment 2
[0120] (1) Add 200g of 3-hydroxy-8-methyl-8-azabicyclo[3.2.1]octane-2-carboxylic acid, 15g of benzoic acid, 50g of quinoline and 5g of copper powder into a four-necked flask and mix and stir , heated to reflux at 140°C for 2h, then added 300g of dimethyl sulfoxide, 105g of hydroxylamine hydrochloride and 25g of sodium methoxide, mixed and stirred, and heated to reflux at 130°C for 5h to obtain bis(methylammonium salt)bicyclo[2.2.1] Octane suspension, then filtered and rotary steamed to obtain bis(methylammonium salt)bicyclo[2.2.1]octane; in another four-necked flask, add 958g of o-dichlorobenzene, and add the above steps into the raw material tube to obtain Bis(methylammonium salt)bicyclo[2.2.1]octane 154g, o-dichlorobenzene 700g, then pressurize the hydrogen chloride gas to 0.1MPa, the reaction vessel is heated to 120°C, and then blow into Hydrogen chloride gas, and dilute triethylamine was added to the raw material pipe at a rate of 428.1g / h, and the heat preservation reacti...
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