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Diphenylmethane diisocyanate monomer addition product capped by methyl ethyl ketoxime and preparation method thereof

A technology of diphenylmethane and diisocyanate, which is applied in the field of methyl ethyl ketone oxime-blocked diphenylmethane diisocyanate monomer adducts and its preparation, can solve the problems of high reactivity and moisture sensitivity, and achieve simple process and coating Stable performance and easy recycling

Inactive Publication Date: 2011-01-12
HENAN SIWEI TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] The purpose of the present invention is to provide a methyl ethyl ketoxime blocked diphenylmethane diisocyanate monomer adduct and its preparation method

Method used

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Examples

Experimental program
Comparison scheme
Effect test

preparation example Construction

[0024] A method for preparing a methyl ethyl ketoxime blocked diphenylmethane diisocyanate monomer adduct, characterized in that it comprises the following steps:

[0025] (1), take 15-30 parts of capping agent methyl ethyl ketoxime and dissolve in 15-25 parts of ethyl acetate or xylene solvent to make a capping agent solution;

[0026] (2), 20-35 parts of diphenylmethane diisocyanate monomers are dissolved in 25-35 parts of ethyl acetate or xylene solvent to make a monomer solution;

[0027] (3) Under the condition of stirring at 45-120° C., add the monomer solution dropwise into the end-capping agent solution for reaction to obtain an insoluble methyl ethyl ketoxime-blocked diphenylmethane diisocyanate monomer adduct.

[0028] The following step is also included after the above step (3): separating the obtained insoluble adduct from the solvent. After the obtained insoluble adduct is separated from the solvent, the following steps are also included: drying the separated add...

Embodiment 1

[0031] Embodiment 1: Take 15g of methyl ethyl ketoxime and put it into 25g of ethyl acetate solvent, stir until it is completely dissolved; take 35g of diphenylmethane diisocyanate monomer and put it into 35g of ethyl acetate solvent and stir until it is completely dissolved; Mix the above two solutions , gradually warming up to 120°C, stirring, and reacting under reflux conditions, controlling the temperature at 120°C, and stopping heating after 5 hours of reaction. Cool to room temperature in a cooling tank, stand still for 10 hours to crystallize, separate the crystals by centrifuge, put them in a vacuum oven and dry them at 30°C for 4 hours, so that the organic solvent content in the material is less than 3%, and then dry them at 40°C Carry out secondary drying at high temperature to make the organic solvent content in the material less than 1%, and grind with a mortar to obtain methyl ethyl ketoxime blocked diphenylmethane diisocyanate.

Embodiment 2

[0032] Embodiment 2: Get 30g of methyl ethyl ketoxime and put it into 15g of xylene solvent, stir until it completely dissolves; Get 20g of diphenylmethane diisocyanate monomer and put it into 25g of xylene solvent and stir until it completely dissolves; Mix the above two solutions, gradually Raise the temperature to 100° C., stir, and react under reflux conditions. The temperature is controlled at 100° C. After 6 hours of reaction, stop heating. Cool to normal temperature in a cooling tank, stand still for 10 hours to crystallize, separate the crystals by a centrifuge, put them in a vacuum oven and dry them at 80°C for 4 hours, so that the organic solvent content in the material is less than 3%, and then dry them at 90°C Carry out secondary drying at high temperature to make the organic solvent content in the material less than 1%, and grind with a mortar to obtain methyl ethyl ketoxime blocked diphenylmethane diisocyanate.

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Abstract

The invention relates to a diphenylmethane diisocyanate monomer addition product capped by methyl ethyl ketoxime and a preparation method thereof, which is used for directly capping the diphenylmethane diisocyanate monomer by adopting a capping agent of the methyl ethyl ketoxime and avoiding bringing impurities to components by using the capping agent. The diphenylmethane diisocyanate monomer addition product capped by the methyl ethyl ketoxime is prepared from the following components in parts by weight: 15-30 parts of methyl ethyl ketoxime, 20-35 parts of diphenylmethane diisocyanate and 40-60 parts of ethyl acetate or xylene solvent. The preparation method comprises the following steps of: capping the isocyanate monomer under a certain condition by adopting the methyl ethyl ketoxime so as to obtain a closed isocyanate monomer addition product capable of stably existing at a room temperature. The closed isocyanate monomer addition product of the invention is used as a modified component of a self adhesive and can obviously improve the adhesion strength and the storage stability of the adhesive and prolong the shelf life.

Description

technical field [0001] The invention belongs to the technical field of adhesives and coatings, and specifically relates to a methyl ethyl ketone that directly blocks diphenylmethane diisocyanate monomer by using a blocking agent methyl ethyl ketone oxime, which avoids the use of the blocking agent to bring impurities to the components. An oxime-blocked diphenylmethane diisocyanate monomer adduct and a preparation method thereof. Background technique [0002] Polyurethane is one of the six synthetic materials with excellent performance. As the main raw material for the synthesis of polyurethane, isocyanate monomers are toxic and contain isocyanate groups with highly unsaturated double bonds (-NCO, structural formula -N=C=O), so the chemical properties very lively. -N=C=O has high reactivity with nucleophiles, and the system is very active at room temperature and cannot exist as a single component. The components that easily react with each other have to be separated and mixe...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C07C271/60C07C269/02
Inventor 鞠凤坦
Owner HENAN SIWEI TECH
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