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Waterborne blocked polyisocyanate cross-linking agent with polyethyleneimine skeleton and preparation method of waterborne blocked polyisocyanate cross-linking agent

A technology of polyethyleneimine and polyisocyanate, which is applied in the field of water-based blocked polyisocyanate crosslinking agent and its preparation, can solve the problems of difficult control of the copolymerization process, great differences in product structure and residual active group content, etc., and achieve production The process is easy to control, the repeatability is strong, and the molecular structure is highly controllable.

Inactive Publication Date: 2015-03-25
YANCHENG INST OF TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

The above studies are based on stepwise polymerization of monomers with different functionalities to prepare water-based blocked polyisocyanate crosslinking agents, but the copolymerization process of monomers with different functionalities is extremely difficult to control, and the product structure between different batches and the content of residual active groups vary greatly

Method used

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  • Waterborne blocked polyisocyanate cross-linking agent with polyethyleneimine skeleton and preparation method of waterborne blocked polyisocyanate cross-linking agent
  • Waterborne blocked polyisocyanate cross-linking agent with polyethyleneimine skeleton and preparation method of waterborne blocked polyisocyanate cross-linking agent
  • Waterborne blocked polyisocyanate cross-linking agent with polyethyleneimine skeleton and preparation method of waterborne blocked polyisocyanate cross-linking agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0029] Example 1, under nitrogen protection and mechanical stirring, 10 grams of hexamethylene diisocyanate, 0.13 grams of dibutyltin dilaurate and 10 grams of cyclohexanone were added to a four-necked flask, and the temperature was slowly raised to 75 ° C. Add 5.89 grams of 3,5-dimethylpyrazole in batches to a four-necked flask, the addition time is 0.5 hours, and react for 3 hours; then add 10 grams of cyclohexanone and 11.67 grams of polyethyleneimine (molecular weight 1000) Into the reaction system, the feeding time is 30 minutes, and the reaction is 1.5 hours; finally, the reaction system is cooled to room temperature, and 16.22 grams of acetic acid are added in batches, the feeding time is 10 minutes, and the reaction is continued for 1 hour to obtain a water-based closed type polyethylenimine skeleton. Polyisocyanate crosslinker. figure 1 It is the infrared spectrum of the water-based blocked polyisocyanate crosslinking agent of the obtained polyethylenimine skeleton, F...

Embodiment 2

[0030] Example 2, under nitrogen protection and mechanical stirring, 10 grams of toluene diisocyanate, 0.18 grams of dibutyltin dilaurate and 15 grams of butanone were added to a four-necked flask, and the temperature was slowly raised to 60 ° C. 3.52 grams of Add imidazole into the four-necked flask in batches, the addition time is 0.5 hours, and react for 2 hours; then add 20 grams of butanone and 19.71 grams of polyethyleneimine (molecular weight 2000) to the reaction system, the addition time is 45 minutes, and react for 1 hour Finally, the reaction system was cooled to room temperature, and 27.5 grams of acetic acid was added in batches for 12 minutes, and the reaction was continued for 1 hour to obtain a water-based blocked polyisocyanate crosslinking agent with a polyethyleneimine skeleton. Such as figure 2 Shown is the infrared spectrum of the water-based blocked polyisocyanate crosslinking agent of the obtained polyethyleneimine skeleton, FT-IR (KBr, cm -1 ): 3346(N...

Embodiment 3

[0031] Example 3, under nitrogen protection and mechanical stirring, 10 grams of isophorone diisocyanate, 0.28 grams of stannous octoate and 12 grams of 1,4-dioxane were added to a four-necked flask, and the temperature was slowly raised to At 70°C, add 3.84 grams of methyl ethyl ketone oxime to a four-necked flask in batches for 0.5 hours, and react for 2.5 hours; then add 30 grams of 1,4-dioxane and 33.56 grams of polyethyleneimine (molecular weight 4000) Added to the reaction system, the feeding time is 1 hour, and the reaction is 2 hours; finally, the reaction system is cooled to room temperature, and 46.83 grams of acetic acid is added in batches, the feeding time is 15 minutes, and the reaction is continued for 1 hour to obtain the aqueous sealing of polyethyleneimine skeleton. Type polyisocyanate crosslinking agent. Such as image 3 Shown is the infrared spectrum of the water-based blocked polyisocyanate crosslinking agent of the obtained polyethyleneimine skeleton, FT...

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Abstract

The invention provides a waterborne blocked polyisocyanate cross-linking agent with a polyethyleneimine skeleton and a preparation method of the waterborne blocked polyisocyanate cross-linking agent. The preparation method comprises the steps of firstly, blocking one isocyanate group in a diisocyanate monomer by using a blocking agent; then, enabling the residual isocyanate group to react with parts of secondary amino groups on a polyethyleneimine molecule; introducing the blocked isocyanate group as a branched chain to a water-soluble polyethyleneimine skeleton; and next, carrying out neutralization reaction on acetic acid serving as a neutralizing agent as well as the secondary amino groups and tertiary amino groups in a polyethyleneimine molecular chain to prepare the blocked polyisocyanate cross-linking agent. The water solubility of the cross-linking agent provided by the invention is derived from the water solubility of a polyethyleneimine molecular skeleton, the content of the finally-deblocked active isocyanate groups is determined by a certain reaction ratio and is conveniently and easily regulated; the molecular structure of the cross-linking agent is high in controllability; the production process is easily controlled; and the waterborne coating system has wide application prospect.

Description

technical field [0001] The invention belongs to the technical field of polymer materials, and in particular relates to a water-based blocked polyisocyanate crosslinking agent with polyethyleneimine skeleton and a preparation method thereof. Background technique [0002] Blocked polyisocyanate crosslinking agent can release highly reactive isocyanate groups (NCO) after deblocking at high temperature, so it can be used as a crosslinking agent for coating systems, especially for coating systems containing active hydrogen groups Among them, the strength, hardness, solvent resistance and scratch resistance of the cured coating can be greatly improved. Compared with low-volatility organic solvents, water is a non-toxic solvent. In recent years, more and more researchers have devoted themselves to the development of various green paints that use water as a solvent. Since the usual oily blocked polyisocyanate crosslinkers are not compatible with waterborne coating systems, waterbor...

Claims

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Application Information

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IPC IPC(8): C08G73/04C08G18/80
Inventor 韦军孙祥路璐
Owner YANCHENG INST OF TECH
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