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Preparation method of self-repair thermosetting epoxy resin based on disulfide bond exchange

A technology of epoxy resin and disulfide bond, which is applied in the field of preparation of self-healing thermosetting epoxy resin based on disulfide bond exchange, can solve the problem of harsh conditions and reconfigurable thermosetting resin system limited to laboratory stage and other problems , to achieve the effect of low cost, favorable for large-scale production and excellent mechanical properties

Inactive Publication Date: 2018-10-12
NORTHWESTERN POLYTECHNICAL UNIV
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  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In 2016, Odriozola (A.R.Luzuriaga, R.Martin and N Markaide.Materials Horizons, 2016, 3:241-247.) proposed to use the exchange reaction of disulfide bonds to prepare dynamically reversible fiber-reinforced resin-based composite materials. There is a very short relaxation time (20S), but this material needs to be processed at 200°C and 20Mp for 30 minutes to achieve repair, and the conditions are too harsh
At present, research on reconfigurable thermosetting resin systems is limited to the laboratory stage. How to apply them to structural parts, curing process and actual performance still need to be explored. The mechanical strength, durability and durability of reconfigurable resin systems under normal conditions Thermal properties and how to ensure the balance between self-healing and mechanical properties of dynamically reversible materials still need to be explored

Method used

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  • Preparation method of self-repair thermosetting epoxy resin based on disulfide bond exchange
  • Preparation method of self-repair thermosetting epoxy resin based on disulfide bond exchange
  • Preparation method of self-repair thermosetting epoxy resin based on disulfide bond exchange

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preparation example Construction

[0030] The preparation method of thermosetting epoxy resin containing disulfide bonds is characterized in that it has the following classic steps:

[0031] Step 1: Synthesis of epoxy resin containing disulfide bonds:

[0032] Step a1: Add 4-mercaptophenol and methyl alcohol successively in a container equipped with a magnetic stirrer, and slowly add iodine simple substance (I 2 ), react overnight at room temperature. 4-Mercaptophenol monomer and I 2 The molar ratio of methanol is 1:0.2-0.6, and the mass ratio of methanol to 4-mercaptophenol monomer is 6-10:1.

[0033] Step b1: After confirming the completion of the reaction by TLC, add anhydrous sodium sulfite to the system until the solution fades to pale yellow, then rotatively evaporate and control the temperature at 30-50°C. After the solvent was completely removed, 100-300 mL of deionized water was added to the system, and extracted three times with ethyl acetate. The organic phase was washed with saturated brine for ...

specific Embodiment

[0039] Step 1: Synthesis of epoxy resin monomer containing disulfide bonds:

[0040] First: add 30g of 4-mercaptophenol, 300ml methyl alcohol successively in the container that magnetic stirrer is housed and slowly add 30.5g iodine simple substance (I 2 ) element, and react overnight at room temperature. After the completion of the reaction was confirmed by TLC, 3 g of anhydrous sodium sulfite was added to the system until the solution faded to light yellow, and the rotary evaporation was performed with the temperature controlled at 30-50 ° C. After the solvent was completely removed, 200 mL of deionized water was added to the system, and the Ethyl ester extracted 3 times. The organic phase was washed with saturated brine for 3 times, dried with anhydrous sodium sulfate, filtered, and then the solvent was removed by rotary evaporation to obtain the product bis(4-hydroxyphenyl)disulfide.

Embodiment 1

[0041] Embodiment 1: In the container that magnetic stirrer is housed, add the double (4-hydroxyphenyl) disulfide of 4.83g successively, 200mlDMF, 17.7ml epibromohydrin, 27.5g anhydrous potassium carbonate, ventilate After 3 times, at N 2 The reaction was carried out at 60°C under protection for 4h. After the completion of the reaction was confirmed by TLC, 300 mL of deionized water was added to the system, extracted three times with dichloromethane, the organic phase was washed with saturated brine, dried over anhydrous sodium sulfate, and the dichloromethane was removed by rotary evaporation to obtain a crude product. The crude product was recrystallized in methanol, filtered and dried to obtain 5.7 g of bis(4-glycidyloxyphenyl) disulfide as a white solid.

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Abstract

The invention relates to a preparation method of self-repair thermosetting epoxy resin based on disulfide bond exchange. The method is characterized in that a disulfide bond-containing epoxy monomer is prepared through a two-step reaction, and the disulfide bond-containing epoxy monomer and a multi-amine monomer are subjected to a ring-opening crosslinking reaction under solvent-free condition toobtain the thermosetting epoxy resin containing the disulfide bond. The disulfide bond is subjected to an exchange reaction while being heated, so that the cured epoxy resin has certain plasticity while being heated, realizes self restoration and repeated processing, and solves the disadvantages of difficult restoration and one-time moulding. The epoxy resin has good degradation characteristic ina mercaptan system due to an exchange reaction of the disulfide bond and a sulfhydryl group, and solves the problem of environment pollution due to excessive usage of the thermosetting epoxy resin.

Description

technical field [0001] The invention relates to a preparation method of self-repairing thermosetting epoxy resin based on disulfide bond exchange, and relates to the synthesis of disulfide bond-containing epoxy monomer and the preparation method of disulfide bond-containing self-repairing thermosetting epoxy resin. Background technique [0002] Resin-based composite materials have many advantages such as high specific strength, high specific modulus, and strong designability. They can effectively reduce the weight of engineering parts, and at the same time endow composite materials with special functions such as heat insulation and wave absorption. , aerospace, military manufacturing, automobile industry and many other fields are indispensable important materials. With the wide application of resin-based composite materials in aerospace and daily life, it is difficult to recycle structural parts of thermosetting resin-based composite materials, and environmental pollution an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/32C08G59/50C08G59/06
CPCC08G59/063C08G59/3263C08G59/5006C08G59/5033C08G59/504
Inventor 张秋禹郭子健周凤涛郑华雷星锋
Owner NORTHWESTERN POLYTECHNICAL UNIV
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