Method for preparing polyisocyanic acid ester

A technology of diisocyanate and polyisocyanate, applied in organic chemical methods, polyurea/polyurethane coatings, coatings, etc., can solve problems such as slow reaction process and disadvantages

Inactive Publication Date: 2008-04-23
BAYER AG
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0014] A disadvantage of the methods of the prior art is, on the one hand, that highly active catalysts with a salt structure are suitable for producing trimers almost exclusively and very little uretdione, whereas (preferably) uretdione-selective catalysts are all covalent structure, so that relatively high concentrations have to be used, based on the mass of catalyst and isocyanate to be oligomeric, and only relatively slow reaction progress can be obtained
Both are disadvantageous from an economical (space-time yield in the preparation) and from a paint technology point of view (negative effect of the catalyst and / or catalyst follow-up products in the polyisocyanate)

Method used

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  • Method for preparing polyisocyanic acid ester
  • Method for preparing polyisocyanic acid ester
  • Method for preparing polyisocyanic acid ester

Examples

Experimental program
Comparison scheme
Effect test

Embodiment

[0063] All percentages, unless otherwise indicated, are to be understood as percentages by weight.

[0064] The NCO content of the resins described in the inventive and comparative examples was determined by titration according to DIN53185.

[0065] The dynamic viscosity of the polyisocyanate was measured at 23°C using a Haake VT550 viscometer with a PK100 plate / cone measurement setting. Measurements at different shear rates ensured that both the rheology of the described polyisocyanate mixtures according to the invention and that of the comparative products corresponded to the behavior of an ideal fluid. Therefore, it is no longer necessary to give the shear rate.

[0066] The mol % or the molar ratio of the different types of structures to each other is given according to the results of NMR spectroscopy. Unless stated otherwise, reference is always made to the sum of the various types of structures resulting from the modification (oligomerization) of the hitherto free NCO ...

example 1～3

[0082] Example 1~3: the oligomerization reaction of the present invention

[0083] General procedure

[0084] The rolled flange container with septum seal was evacuated twice and filled with argon. In each case, 5 mL of diisocyanate were introduced by means of a syringe into the container thus prepared, and the corresponding amount of catalyst solution was then added with stirring. See Tables 1 and 2 for catalyst numbering, the "mol %" figures in Tables 3-6 refer in each case to the target amount of diisocyanate and catalyst used to achieve the conversions obtained in the respective experiments. The resulting reaction mixture is reacted at the desired temperature using an oil bath or a stirring heating block (for example, Variomag reaction block, type 48.2 / RM, manufactured by H&P). After the end of the reaction—either by the specified reaction time or by the arrival of a specified viscosity—an aliquot (20-40 mg) of the reaction mixture was dissolved in 3 mL of chloroform a...

example 4

[0109] The inventive preparation of HDI polyisocyanate

[0110] 1680g (10mol) of freshly distilled HDI was first stirred in a 3-neck flask stirring device at 60°C under reduced pressure (0.1mbar) for 1h in order to drive out the dissolved gas, then covered with dry nitrogen and heated at 60°C under stirring Catalyst solution 13 was added dropwise and mixed until the reaction started as indicated by a temperature rise of 1-2°C. By sporadically adding further catalyst (total: 4.6 g catalyst solution = 0.046 mol% catalyst based on the amounts of HDI and 1,2,3-triazolyltetradecyl(trihexyl)phosphonium salt), the reaction was Within 1h, under the temperature condition of the mixture of 60-70℃ to the required conversion rate, the required conversion rate is determined by the refractive index n D 20 detection. in n D 20 =1.4668, the further reaction was terminated by adding 1.9 g of a 42% strength p-toluenesulfonic acid solution in isopropanol. The crude product thus obtained wa...

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Abstract

The invention relates to a method for making oligomeric isocyanates by reacting diisocyanates in the presence of a catalyst, wherein the catalyst comprises a saline compound prepared from an anion selected from 1,2,3- or 1,2,4-triazole, a substituted species of 1,2,3- or 1,2,4-triazole and carbocyclically and / or heterocyclically annellated species of 1,2,3- or 1,2,4-triazole and the cation selected from an alkali metal, alkaline-earth metal and / or monovalent ammonium cation and / or phosphonium cation of formula (5), wherein the E, R1, R2, R3, R4 are as defined in the descriotion. The invention also relates to a products obtained by the said method and polymer prepared by the products. The catalyst system for polyisocyanates has high reality and prompts to generate thiourea dione accounting for large proportion of polyisocyanates.

Description

[0001] This application is a divisional application of the invention patent application with application number 02809955.9 and application date of May 7, 2002. technical field [0002] The present invention relates to a new process for the preparation of polyisocyanates, the polyisocyanates thus prepared and their use. Background technique [0003] The oligomerization of isocyanates is a well-established and long-known method in the practice of modifying low-molecular-weight difunctional isocyanates in general, with the aim of obtaining products with excellent performance properties, for example in the field of paints and coatings, commonly referred to herein as polyisocyanates. Isocyanates (J. Prakt. Chem. / Chem. Ztg. 1994, 336, 185-200). [0004] For light-stable, non-yellowing paints and coatings, polyisocyanates based on aliphatic diisocyanates are generally used. The term "aliphatic" here refers to the carbon atom in the monomer to which the NCO group is attached; in ot...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07D207/00C07D209/00C07D231/00C07D233/00C07D249/00C07D257/00C08G18/79C07D251/34C07B61/00C07D229/00C07D273/04C08G18/02C08G18/20C08G18/80C09D175/04
CPCC08G18/807C08G18/027C08G18/022C08G18/2036C08G18/20
Inventor J·科彻尔F·里奇特H·-J·拉亚斯M·温特曼特尔
Owner BAYER AG
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