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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

Active Publication Date: 2013-03-13
WANHUA CHEM GRP +1
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0006] In CN99109785, the polyisocyanate prepared by the catalysis of phosphorus polyfluoride, although the iminooxadiazinedione content is relatively high (can be greater than 50mol%), but the product prepared according to this method contains undesired uretonimine, Allophanate and other by-products

Method used

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  • Method for preparing polyisocyanate containing formimidoyl oxadiazine diketone
  • Method for preparing polyisocyanate containing formimidoyl oxadiazine diketone
  • Method for preparing polyisocyanate containing formimidoyl oxadiazine diketone

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Experimental program
Comparison scheme
Effect test

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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Abstract

The invention relates to a method for preparing polyisocyanate containing formimidoyl oxadiazine diketone. The method is used for preparing the polyisocyanate containing the formimidoyl oxadiazine diketone by performing trimerization reaction on monomeric diisocyanate in the presence of a phosphazene catalyst. The polyisocyanate containing the formimidoyl oxadiazine diketone prepared by the method has the advantage of high formimidoyl oxadiazine diketone content, and does not contain uretonimine and carbodiimide.

Description

technical field [0001] The invention relates to a method for preparing polyisocyanate containing iminooxadiazinedione, especially a method for preparing polyisocyanate with iminooxadiazinedione content higher than 50 mol%. Background technique [0002] Polyisocyanates containing iminooxadiazinedione structures prepared by catalyzing the trimerization of aliphatic diisocyanates have been widely used in the non-yellowing polyurethane paint and coating industries. For diisocyanate polymers containing not less than three NCO groups , the iminooxadiazinedione has the advantage of having the lowest viscosity. The existing catalysts for the preparation of polyisocyanates containing iminooxadiazinediones mainly include alkyl phosphines, N silyl compounds, triazolium salt compounds, polyfluoride salts, etc., but the above catalysts will have low catalytic selectivity , there are disadvantages such as by-product formation, especially by-product uretonimine and carboimide, which will ...

Claims

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Application Information

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IPC IPC(8): C08G18/79C08G18/02C07D251/34C07D273/04
Inventor 唐义权尚永华孙立冬李建峰华卫琦严成岳
Owner WANHUA CHEM GRP
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