Polyisocyanate composition, composition for film formation, film, film laminated body, adhesive resin composition, adhesive resin cured product, composition for coating materials, and coating material cured product
A polyisocyanate and adhesive resin technology, applied in the direction of synthetic resin layered products, polyurea/polyurethane coatings, film/flake adhesives, etc. Sufficient effects, excellent stability, excellent blocking resistance and solvent resistance
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Embodiment
[0358] The present embodiment will be described in further detail below based on examples and comparative examples, but the present embodiment is not limited by the following examples. It should be noted that "%" and "parts" in the text refer to mass standards unless otherwise specified.
[0359] The measuring method of the physical property of the polyisocyanate composition obtained in the synthesis example, and the evaluation method of the film and film laminated body obtained in the Example and the comparative example are shown below.
[0360]
[0361] [Physical property 1] Viscosity
[0362] Measured at 25° C. using an EMILA type rotational viscometer.
[0363] [Physical properties 2] Number average molecular weight
[0364] The number average molecular weight is a polystyrene-based number average molecular weight measured by gel permeation chromatography (GPC) using the following apparatus. A polyisocyanate composition was used as a sample. The measurement conditions ...
Synthetic example 1
[0513] [Synthesis Example 1] (Synthesis of polyisocyanate p-1)
[0514] Set the 4-necked flask equipped with a stirrer, thermometer, reflux condenser, nitrogen blowing tube, and dropping funnel into a nitrogen atmosphere, and add HDI: 600 parts and polyester polyol derived from trihydric alcohol and ε-caprolactone (Daicel Co., Ltd. product, brand name "PLACCEL 303"): 30 parts, the temperature inside the reactor was kept at 90 degreeC 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 a predetermined yield was reached, phosphoric acid was added to stop the reaction. The reaction solution was filtered, and then unreacted HDI was removed with a thin film evaporation tank. Production of polyisocyanate was confirmed by measuring the number average molecular weight of the reaction product by GPC and measuring the isocyanate ...
Synthetic example 2
[0515] [Synthesis Example 2] (Synthesis of polyisocyanate p-2)
[0516] Set the 4-necked flask equipped with a stirrer, thermometer, reflux condenser, nitrogen blowing tube, and dropping funnel into a nitrogen atmosphere, add HDI: 600 parts, keep the temperature in the reactor at 60°C, and add isocyanurate Tetramethylammonium decanoate was used as catalyst, and when the isocyanate content of the reaction solution reached 38.7% by mass, phosphoric acid was added to stop the reaction. The reaction solution was filtered, and then unreacted HDI was removed with a thin film evaporation tank. Production of polyisocyanate was confirmed by measuring the number average molecular weight of the reaction product by GPC and measuring the isocyanate content rate by titration. The obtained polyisocyanate p-2 had a viscosity at 25° C. of 2,700 mPa·s, an isocyanate content of 21.7%, a number average molecular weight of 660, and an average number of isocyanate groups of 3.4.
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