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High-steric-hindrance urea bond-containing curing agent as well as preparation method and application thereof

A curing agent and large steric hindrance technology, applied in the field of curing agent containing large sterically hindered urea bond and its preparation, can solve the problems of difficulty in reprocessing or recycling, affecting the service life of products, etc., and achieve good thermal stability and good mechanical properties. , The effect of simple reprocessing conditions

Pending Publication Date: 2022-07-22
国科广化精细化工孵化器(南雄)有限公司 +3
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, the irreversible covalent network will cause irreparable mechanical damage to the interior when the resin is subjected to external effects such as impact and extrusion during use, which will seriously affect the service life of the product and cause problems that are difficult to reprocess or recycle.

Method used

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  • High-steric-hindrance urea bond-containing curing agent as well as preparation method and application thereof
  • High-steric-hindrance urea bond-containing curing agent as well as preparation method and application thereof
  • High-steric-hindrance urea bond-containing curing agent as well as preparation method and application thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0047] 1. Preparation of secondary amines

[0048] (1) under nitrogen atmosphere condition, dissolve 1 mole part of MDA and 2 mole parts of triethylamine in 1.7 mole part of toluene solvent in reaction flask, transfer to 80 ℃ constant temperature oil bath pot with magnetic stirring to form a homogeneous solution;

[0049] (2) After mixing 2 molar parts of benzyl bromide and 0.28 molar parts of toluene solvent, transfer to a constant pressure funnel, place it on the top of the reaction flask, and slowly drop the benzyl bromide-toluene solution into the reaction flask, and the dropping time is 2h , the whole reaction system was refluxed for 12h (that is, the reaction was continued for 10h after the addition was completed);

[0050] (3) after the reaction finishes, carry out suction filtration, washing, drying with anhydrous magnesium sulfate, suction filtration again, to obtain secondary amine-toluene solution, then rotary evaporation is carried out to remove toluene, drying, to o...

Embodiment 2

[0066] 1. Preparation of secondary amines

[0067] (1) under nitrogen atmosphere condition, dissolve 1 mol part of MDA and 2 mol part of triethylamine in 1.6 mol part of toluene solvent in reaction flask, transfer to 80 ℃ constant temperature oil bath pot with magnetic stirring to form a homogeneous solution;

[0068] (2) After mixing 2 molar parts of benzyl bromide and 0.28 molar parts of toluene solvent, transfer to a constant pressure funnel, place it on the top of the reaction flask, and slowly drop the benzyl bromide-toluene solution into the reaction flask, and the dropping time is 2h , the whole reaction system was refluxed for 12h (that is, the reaction was continued for 10h after the addition was completed);

[0069] (3) after the reaction finishes, carry out suction filtration, washing, drying with anhydrous magnesium sulfate, suction filtration again, to obtain secondary amine-toluene solution, then rotary evaporation is carried out to remove toluene, drying, to obt...

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Abstract

The invention discloses a curing agent containing a large-steric-hindrance urea bond as well as a preparation method and application of the curing agent. The method mainly comprises the following steps: dissolving bifunctional aromatic amine and alkali in a solvent, adding halogenated hydrocarbon at 70-85 DEG C, and reacting for 8-12 hours to obtain an intermediate product secondary amine; the preparation method comprises the following steps: adding diol and an anhydrous solvent into bifunctional isocyanate, and reacting at 50-60 DEG C for 2-6 hours to obtain a polyurethane prepolymer; and adding secondary amine and an anhydrous solvent into the polyurethane prepolymer, and reacting at 50-60 DEG C for 6-8 hours to obtain the large-steric-hindrance urea bond-containing curing agent. The prepared curing agent containing the large-steric-hindrance urea bonds can overcome the defects of other dynamic covalent bonds, and epoxy resin prepared based on the curing agent containing the large-steric-hindrance urea bonds is good in mechanical property, thermal stability and solvent-resistant chemical stability; the large-steric-hindrance urea bond-containing curing agent can also be used for preparing electronic packaging materials.

Description

technical field [0001] The invention belongs to the field of synthesizing a curing agent for polymer materials, and particularly relates to a curing agent containing a large sterically hindered urea bond and a preparation method and application thereof. Background technique [0002] Thermosetting resins have excellent mechanical properties, adhesive properties, heat resistance and low curing shrinkage due to their cross-linked network or body structure, and are widely used in electronic packaging materials, adhesives and coatings. However, the irreversible covalent network causes irreversible mechanical damage to the resin when it is subjected to external effects such as impact and extrusion during use, which seriously affects the service life of the product, and also leads to problems that are difficult to reprocess or recycle. [0003] Inspired by the intrinsic self-healing phenomenon of organisms, dynamic covalent bonds with reversible behavior can participate in reversib...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G59/40C08G18/32C08G18/10
CPCC08G59/4021C08G18/10C08G18/3206C08G18/325
Inventor 梁利岩陈碧芳王波
Owner 国科广化精细化工孵化器(南雄)有限公司
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