Solvent-free closed colored polyisocyanate curing agent as well as preparation method and application thereof
A polyisocyanate, closed-type technology, applied in polyurea/polyurethane coatings, coatings, etc., can solve problems such as high toxicity, high pollution, and strong odor, and achieve the effect of improving water resistance and improving physical and chemical properties
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[0024] The invention discloses a preparation method of a solvent-free blocked colored polyisocyanate curing agent, which comprises the following steps:
[0025] 1) Preparation of modified polyisocyanate monomer (L)
[0026] Under the protection of nitrogen, add the polyisocyanate (A) and polymerization inhibitor (B) of the designed formula ratio into the four-port reactor equipped with a thermometer and a condenser, and heat it to 60-80°C with an electric heating mantle , slowly add enol or acrylate (C) dropwise for about 1 hour, keep warm for 2 to 4 hours, and then start to measure the NCO content. Isocyanate monomer (L).
[0027] 2) Preparation of modified polyisocyanate prepolymer (G)
[0028] Under nitrogen protection, place part of the modified polyisocyanate monomer (L) at the bottom of the reaction bottle, stir and mix the remaining modified polyisocyanate monomer (L) with the initiator (D), and slowly add it dropwise into the reaction bottle ( The dropwise addition ...
Embodiment 1
[0046] Under the protection of nitrogen, 952 parts of hexamethylene diisocyanate (HDI), 1.4 parts of polymerization inhibitor (p-hydroxymethyl anisole) are added with a thermometer and a condenser, in a four-port reactor with stirring, Heat to 60-80°C with an electric heating mantle, slowly add 489 parts of hydroxyethyl acrylate dropwise, finish dropping in about 1 hour, keep warm for 2-4 hours, and then start to measure the NCO content, when the NCO value is ≤21.24% (according to the experimental design , the NCO content when the hydroxyl group in the raw material is completely reacted accounts for the percentage of the total amount of the resin), the temperature is lowered and the material is discharged, and the modified polyisocyanate monomer is obtained.
[0047] Under nitrogen protection, place 289 parts of modified polyisocyanate monomers prepared above at the bottom of the reaction bottle, stir and mix 1152 parts of modified polyisocyanate monomers with 9 parts of azobis...
Embodiment 2
[0052] Under the protection of nitrogen, 1235 parts of hexamethylene diisocyanate (HDI), 1.2 parts of polymerization inhibitor (p-hydroxymethyl anisole) are added in a four-port reactor equipped with a thermometer and a condenser, with stirring, Heat it to 60-80°C with an electric heating mantle, slowly add 495 parts of hydroxyethyl methacrylate dropwise for about 1 hour, keep it warm for 2-4 hours, and then start to measure the NCO content. When the NCO value is ≤27.08% (according to Experimental design, the NCO content when the hydroxyl groups in the raw materials are completely reacted accounts for the percentage of the total amount of the resin), the temperature is lowered and the material is discharged, and the modified polyisocyanate monomer is obtained.
[0053] Under nitrogen protection, place 346 parts of modified polyisocyanate monomers prepared above at the bottom of the reaction bottle, stir and mix 1384 parts of modified polyisocyanate monomers with 9 parts of azob...
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