Method for preparing polyisocyanate containing formimidoyl oxadiazine diketone
A technology of imino oxadiazine dione and diisocyanate is applied in the field of preparation of polyisocyanate to achieve the effect of improving storage stability
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Embodiment 1
[0033] Preparation of HDI polyisocyanate: 1500g of newly distilled HDI is first placed in a three-necked flask equipped with a stirring device, the HDI monomer is heated to 60°C, stirred for 1h under reduced pressure to drive out dissolved gas, and then covered with dry nitrogen Under stirring at 60°C, slowly add the above-mentioned catalyst 1 of the present invention, the amount of the catalyst is 100ppm based on the monomeric isocyanate, stir and mix until the temperature rises by 1-2°C as a sign to start the reaction. The mixture was stirred at this temperature for about 2-3 h. When the initial diisocyanate conversion rate reaches 39%, (the conversion rate is determined by gel chromatography) 300ppm benzoyl chloride is added to terminate the reaction, and stirring is continued at 60°C for 1h. The excess monomer HDI was removed in an evaporator to obtain a colorless or light yellow transparent viscous liquid. The component contents of the product are shown in Table 1.
Embodiment 2-6
[0035] The operation of Example 1 was repeated with catalysts 2-6 respectively. The content of the product components is shown in Table 1.
Embodiment 7
[0045] Preparation of HMDI and HDI mixed polyisocyanate: 1000g of newly distilled HDI and 500g of HMDI were first placed in a three-necked flask stirring device, stirred at 60°C for 1h under reduced pressure to drive out dissolved gases, and then covered with dry nitrogen at 80°C Slowly add catalyst 1 under stirring, the amount of catalyst is 150ppm based on monomeric isocyanate, stir and mix until the temperature rises by 1-2°C as a sign to start the reaction. The mixture was stirred at this temperature for about 3-4h. When the initial diisocyanate conversion rate reached 36%, (the conversion rate was determined by gel chromatography). Add 450ppm benzoyl chloride to terminate the reaction, continue stirring at 80°C for 1h, and remove excess monomer HDI and HMDI in a thin-film evaporator at a pressure of 10pa and a temperature of 160°C to obtain a colorless or light yellow transparent viscous liquid. The content of product components is shown in Table 2.
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