Blocked polyisocyanate composition, hydrophilic polyisocyanate composition, resin composition, resin film and laminate
A technology of polyisocyanate and composition, applied in the field of resin films and laminates, can solve the problems of limited use, required heat resistance of substrates, unfavorable energy, etc.
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Examples
Embodiment 1-1～1-18 and comparative example 1-1～1-6
[0623]
[0624] For the blocked polyisocyanate compositions obtained in Examples and Comparative Examples, measurements and evaluations of various physical properties were performed according to the methods shown below
[0625] [Physical properties 1-1]
[0626] (Isocyanate group (NCO) content rate)
[0627] In order to measure the NCO content rate of a polyisocyanate, the polyisocyanate before blocking with a blocking agent was used as a measurement sample.
[0628] First, 2 g or more and 3 g or less (Wg) of a measurement sample are accurately weighed in a flask. Next, 20 mL of toluene was added to dissolve the measurement sample. Next, 20 mL of a toluene solution of 2 equivalents of di-n-butylamine was added and mixed, and then left to stand at room temperature for 15 minutes. Next, 70 mL of isopropanol was added and mixed. Next, this liquid is titrated into the indicator with 1 N hydrochloric acid solution (factor F). The obtained titration value was set as V2mL. Ne...
Synthetic example 1-1
[0660] (Synthesis of Polyisocyanate P-1)
[0661] Under nitrogen flow, put into the four-neck flask equipped with thermometer, stirring blade and reflux condenser: 100 parts by mass, and polyester polyol (manufactured by Daicel Chemical Co., Ltd.) derived from trihydric alcohol and ε-caprolactone. , "PLACCEL303" (trade name)): 5.1 parts by mass, the temperature in the reactor was kept at 90° C. for 1 hour with stirring, and the urethanization reaction was performed. Thereafter, the temperature in the reactor was kept at 60° C., an isocyanuration catalyst tetramethylammonium caprate was added, and when the yield reached 51% by mass, phosphoric acid was added to stop the reaction. After filtering the reaction liquid, unreacted HDI was removed using a thin-film evaporator, and an isocyanurate-type polyisocyanate (hereinafter may be referred to as "polyisocyanate P-1") was obtained. The obtained polyisocyanate P-1 had an NCO content of 18.8% by mass, a number average molecular we...
Synthetic example 1-2
[0663] (Synthesis of Polyisocyanate P-2)
[0664] Under nitrogen flow, put HDI: 80 mass parts, IPDI: 20 mass parts and trimethylolpropane as trihydric alcohol: 3.4 mass parts in the four-necked flask that thermometer, stirring blade and reflux condenser are installed, in The temperature in the reactor was kept at 90° C. for 1 hour while stirring to perform a urethanization reaction. Thereafter, the temperature in the reactor was kept at 77° C., an isocyanuration catalyst tetramethylammonium caprate: 0.012 parts by mass was added, and when the yield reached 45 mass %, phosphoric acid was added to stop the reaction. After filtering the reaction liquid, unreacted HDI and IPDI were removed using a thin film evaporator, and an isocyanurate type polyisocyanate (hereinafter may be referred to as "polyisocyanate P-2") was obtained. The obtained polyisocyanate P-2 had an NCO content of 19.1% by mass, a number average molecular weight of 1210, and an average number of isocyanate groups...
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