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Preparation method of high-strength thermosetting resin hydrogel material

A hydrogel and thermosetting technology, which is applied in the field of preparation of high mechanical strength thermosetting resin hydrogel composite materials, can solve the problems of low chemical crosslinking density, high brittleness of cured products, and degradation of broken chains, and achieve high practical use value , outstanding material properties, fast viscosity growth effect

Active Publication Date: 2021-08-20
UNIV OF ELECTRONICS SCI & TECH OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, benzoxazine resins face two prominent problems in the process of practical application: 1. The curing temperature is high, and the curing temperature of most benzoxazine resins is not lower than 200℃; 2. .The cured product is brittle. Because of the high rigid hydrogen bond content of benzoxazine resin and the low chemical crosslinking density, its toughness is lower than that of commonly used epoxy resin systems.
[0004]Existing hydrogel materials are mostly used in biomedicine, flexible electronics and other fields, and their mechanical strength is low, so it is impossible to be used as a matrix for high-strength structural materials. Both thermosetting and thermoplastic polymers will face the problems of water absorption swelling, performance degradation and even chain scission degradation when used in water environment or wet environment.
In addition, as a new type of high-performance thermosetting resin, benzoxazine often needs to be cured at a temperature of about 200°C, and the cured product has poor toughness. When used as a structural material, it is not resistant to impact and has a great influence of defects.
In order to prepare high-strength structures and structure-function integrated materials suitable for water and wet environments with good toughness, hydrogel materials based on high-performance thermosetting resins are an innovative and promising idea, and there is currently no Patents and other literature reports on the preparation of hydrogels from oxazine resin monomers

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0036] (1) Add 50% concentrated hydrochloric acid dropwise to N,N-dimethylformamide to obtain a colorless and transparent clear solution;

[0037](2) Graphene is added in the solution that step (1) obtains, ultrasonic dispersion 15 minutes, obtain uniform black suspension;

[0038] (3) benzoxazine monomer (bisphenol A-aniline type benzoxazine) is added to the suspension obtained in step (2), dissolved under the assistance of ultrasound to obtain a uniform black suspension, The mass of the resin monomer is controlled to account for 30wt% of the total mass of the suspension, the molar ratio of hydrochloric acid to the resin monomer is 1:30, and the graphene accounts for 20wt% of the mass of the resin monomer.

[0039] (4) Stir and prepolymerize the suspension obtained in step (3) in a water bath or a heating mantle at 80°C, observe the viscosity of the system, and place it in an oven at 80°C when the viscosity is high and the flow is difficult , the system quickly gelled within...

Embodiment 2

[0043] (1) Add 50% concentrated sulfuric acid dropwise to N,N-dimethylformamide to obtain a colorless and transparent clear solution;

[0044] (2) Graphene is added in the solution that step (1) obtains, ultrasonic dispersion 15 minutes, obtain uniform black suspension;

[0045] (3) benzoxazine monomer (bisphenol A-aniline type benzoxazine) is added to the suspension obtained in step (2), dissolved under the assistance of ultrasound to obtain a uniform black suspension, The mass of the resin monomer is controlled to account for 40wt% of the total mass of the suspension, the molar ratio of sulfuric acid to the resin monomer is 1:30, and the graphene accounts for 20wt% of the mass of the resin monomer.

[0046] (4) Stir and prepolymerize the suspension obtained in step (3) in a water bath or a heating mantle at 80°C, observe the viscosity of the system, and place it in an oven at 80°C when the viscosity is high and the flow is difficult , the system quickly gelled within 10 min...

Embodiment 3

[0050] (1) dissolving phosphorus pentachloride powder in N,N-dimethylformamide to obtain a colorless transparent or light yellow transparent clear solution;

[0051] (2) Graphene is added in the solution that step (1) obtains, ultrasonic dispersion 15 minutes, obtain uniform black suspension;

[0052] (3) Add benzoxazine monomer (phenol-4,4'-diaminodiphenylmethane type benzoxazine) to the suspension obtained in step (2), and dissolve under the assistance of ultrasound to obtain For a uniform black suspension, the mass of the resin monomer accounts for 35 wt% of the total mass of the suspension, the mass of phosphorus pentachloride accounts for 4 wt% of the mass of the resin monomer, and the graphene accounts for 15 wt% of the mass of the resin monomer.

[0053] (4) Stir and prepolymerize the suspension obtained in step (3) in a water bath or a heating mantle at 80°C, observe the viscosity of the system, and place it in an oven at 80°C when the viscosity is high and the flow is...

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Abstract

The invention belongs to the field of processing methods and functional application of high-performance thermosetting resins, and discloses a preparation method of a high-strength thermosetting resin hydrogel material. According to the preparation method, crosslinking is performed at medium and low temperatures under the catalysis of a high-activity catalyst to obtain organic solvent gel, and solvent replacement isperformed to obtain the thermosetting resin hydrogel, and therefore, the processing manufacturability of benzoxazine resin can be improved, the mechanical strength of the hydrogel material can be improved; and the prepared thermosetting resin hydrogel has characteristics of high mechanical strength and high toughness, and can be used as a novel high-performance resin matrix used in the water environment, and meets the use requirements of a high-strength structural material and a structure-function integrated material suitable for a water environment and a wet environment are met.

Description

technical field [0001] The invention relates to a novel processing method and functional application field of high-performance thermosetting resin, and more specifically relates to a preparation method of a high-mechanical-strength thermosetting resin hydrogel composite material cured at a medium and low temperature. Background technique [0002] High-performance thermosetting resins and high-performance composite materials and functional materials based on them have huge demands and extremely broad application prospects in the fields of automobiles, ships, aviation, aerospace, and weaponry. However, in the process of practical application, the curing process of high-performance thermosetting resin usually requires a higher curing temperature and a longer curing time, so the control and equipment requirements for the processing process are very high. In addition, thermosetting resins also face the problems of high brittleness, poor impact resistance and bending performance. ...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J3/075C08G73/06C08L79/04
CPCC08J3/075C08G73/06C08J2379/04
Inventor 张帅孙弘毅夏舜珂汪淑贤黄宇敏刘孝波
Owner UNIV OF ELECTRONICS SCI & TECH OF CHINA
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