Preparation method and application of novel modified amine epoxy curing agent

An amine epoxy and curing agent technology is applied in the field of preparation of a new type of modified amine epoxy curing agent, which can solve the problems of poor molecular structure designability and high formaldehyde content of the curing agent, and can improve the high free formaldehyde content and control the formaldehyde content. , the effect of promoting the reaction

Inactive Publication Date: 2021-11-16
SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still some deficiencies in these phenalkamine curing agents, such as: the content of formaldehyde is too high, the designability of the molecular structure of the curing agent is poor, etc.

Method used

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  • Preparation method and application of novel modified amine epoxy curing agent
  • Preparation method and application of novel modified amine epoxy curing agent
  • Preparation method and application of novel modified amine epoxy curing agent

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0039] In a three-necked flask equipped with a mechanical stirrer, a condenser, and a thermometer, 18.82 g (0.2 mol) of phenol, 13.2 g (0.44 mol) of paraformaldehyde, and 200 mL of toluene were sequentially added, and the temperature was slowly raised to 55° C. in an oil bath; then At intervals of 15 minutes, add 20.44 g (0.2 mol) of N,N-dimethyl-1,3-diaminopropane in three batches. The mass fraction of the solute in the system is 30%. When N,N-dimethyl-1 , After adding all the 3-diaminopropane, slowly raise the temperature to 85°C, stir and react for 4 hours, wash and dry after the reaction, and obtain a light yellow product, namely benzoxazine P-dampa, whose structure is shown in formula (3) As shown, the yield is 92.7%.

[0040]

[0041] The prepared benzoxazine has carried out infrared spectroscopic analysis, and the results are as follows: figure 1 shown. As can be seen from the figure, the 921cm -1 Is the characteristic absorption peak of oxazine ring, 1034cm -1 a...

Embodiment 2

[0043] In a three-neck flask equipped with magnetic stirring, a condenser, and a thermometer, 4.42 g (0.02 mol) of benzoxazine P-dampa and 2.33 g (0.02 mol) of hexamethylenediamine prepared in Example 1 were added successively, and in a solvent-free 1. Under the condition of nitrogen protection, put it in an oil bath and slowly raise the temperature to 90° C., and stir for 5 hours to obtain curing agent-I (①), whose structure is shown in formula (4), and the yield is 95.6%.

[0044]

[0045] Prepared curing agent-I has carried out infrared spectroscopic analysis, and the results are as follows: figure 2 shown. As can be seen from the figure, the 921cm -1 The characteristic peak of the oxazine ring disappeared, 3313cm -1 There is an absorption peak of -OH at 1137cm -1 There is a C-N-C vibration peak at 1381cm -1 -CH 3 vibration peak. Therefore, it can be shown that the synthesized compound has the correct structure.

Embodiment 3

[0047] In the there-necked flask equipped with magnetic stirring, condenser, and thermometer, benzoxazine P-dampa 4.42g (0.02mol) and triethylenetetramine 2.92g (0.02mol) prepared in Example 1 were added successively. Under the conditions of solvent and nitrogen protection, put it in an oil bath and slowly raise the temperature to 100°C, and stir for 4 hours to obtain curing agent-II (②), whose structure is shown in formula (5), and the yield is 98.1%.

[0048]

[0049] Prepared curing agent-II has carried out infrared spectroscopic analysis, and the results are as follows: image 3 shown. As can be seen from the figure, the 921cm -1 The characteristic peak of the oxazine ring disappeared, 3282cm -1 There is an absorption peak of -OH at 1117cm -1 There is a C-N-C vibration peak at 1380cm -1 -CH 3 vibration peak. Therefore, it can be shown that the synthesized compound has the correct structure.

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Abstract

The invention relates to the technical field of curing agents, in particular to a preparation method and the application of a novel modified amine epoxy curing agent. The preparation method comprises the following steps: carrying out Mannich reaction on a phenol source, an amine source and aldehyde in a solvent to prepare benzoxazine, and carrying out ring-opening reaction on the benzoxazine and polyamine to obtain the novel modified amine epoxy curing agent. According to the invention, benzoxazine and polyamine react, and a phenol Mannich bridge structure is introduced into a modified amine curing agent, so that the curing reaction of polyamine and epoxy resin is promoted. The polyamine is modified by adopting different types of benzoxazine resins, and the types and content of phenol Mannich bridge structures in the modified amine curing agent structure are adjusted, so that the curing temperature and the curing time are adjusted, and different process conditions and performance requirements of the epoxy resin are met. Benzoxazine is introduced into polyamine, so that the proportion of phenolic aldehyde amine can be accurately adjusted and controlled, the defects that a traditional Mannich base modified amine curing agent is high in free formaldehyde content and the like are overcome, the green and environment-friendly requirements are met, and the application in the aspects of coatings, adhesives, composite materials and the like is expanded.

Description

technical field [0001] The invention relates to the technical field of curing agents, in particular to a preparation method and application of a novel modified amine epoxy curing agent. Background technique [0002] Epoxy resin is a common thermosetting resin, which contains one or more active epoxy groups in its molecular structure. However, it must be cured by adding a curing agent, and the curing shrinkage rate is low. Because the cured product has excellent thermal stability, mechanical properties, adhesiveness, dielectric properties, and processing properties, it is widely used in coatings, industrial molds, and adhesives. Agents, aerospace, electronic materials and other fields. Among them, there are many kinds of curing agents, such as amines, alkalis, acid anhydrides, mercaptans, etc. Since the network morphology and crosslink density of epoxy resin are determined by the curing agent, different types of curing agent will affect the physical properties and gelation ...

Claims

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Application Information

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IPC IPC(8): C07C213/00C07C215/50C08G59/62
CPCC07C213/00C07C215/50C07D265/16C08G59/623
Inventor 夏益青盛玉萍刘淋泽王炼颜帅石锐赵星宇高晨廖斌李新跃
Owner SICHUAN UNIVERSITY OF SCIENCE AND ENGINEERING
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