Preparation method of self-repair nanocapsule-thermosetting-resin-base composite material

A technology of nanocapsules and composite materials, which is applied in the field of preparation of self-healing nanocapsules/thermosetting resin-based composite materials, which can solve the problems of performance degradation and poor compatibility of thermosetting resin-based composite materials, and achieve good compatibility and dispersion Improvement, small size effect

Active Publication Date: 2015-11-25
SHAANXI UNIV OF SCI & TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, there are still many deficiencies in the existing microcapsule self-healing methods, such as poor compatibility between the repair agent system and the matrix, and the introduction of microcapsules leads to a decline in the performance of thermosetting resin-based composites, etc.

Method used

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  • Preparation method of self-repair nanocapsule-thermosetting-resin-base composite material
  • Preparation method of self-repair nanocapsule-thermosetting-resin-base composite material
  • Preparation method of self-repair nanocapsule-thermosetting-resin-base composite material

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preparation example Construction

[0031] A self-healing nanocapsule / thermosetting resin-based composite material of the present invention is prepared by the following steps:

[0032] 1) Add urea and formaldehyde into a three-necked flask with a molar ratio of 1:1 to 1:3 and stir, then add urea in batches to reduce the amount of free formaldehyde to form a urea-formaldehyde solution, and then add urea-formaldehyde at a mass ratio of 0 %~50% of melamine. Adjust the pH value to 8-9 with an alkali-adjusting agent, slowly raise the temperature to 60-80°C, and react in a water bath at a constant temperature of 60-80°C for 30-60 minutes. Check the end point of the reaction, stop heating and wait until the temperature drops to room temperature to obtain a transparent and viscous product. Polyurea-formaldehyde prepolymer (PUF prepolymer) or melamine-urea formaldehyde prepolymer (MUF prepolymer); wherein, the wall material raw materials are urea, formaldehyde and melamine;

[0033] 2) Take 8.0-20.0g epoxy resin as the ...

Embodiment 1

[0045] 1) Add 2.0 g of urea and 5.4 g of formaldehyde solution (37 wt%) into a three-necked flask and stir. Use triethanolamine to adjust the pH value to 9, slowly raise the temperature to 70°C, react at a constant temperature in a water bath for 30 minutes, detect the end point of the reaction, stop heating until the temperature drops to room temperature, and prepare a transparent and viscous urea-formaldehyde prepolymer (PUF prepolymer) );

[0046] 2) Take 8.0 g of bisphenol F glycidyl ether type epoxy resin as the core material, 2.0 g of 1-butyl glycidyl ether, 1.8 g of sodium dodecylbenzene sulfonate as emulsifier, and 0.5 g of n-octanol as disinfectant Foaming agent, add 100mL deionized water, stir at 600rpm for 1.5h to form an O / W emulsion. Stir with a high-speed mixer at 900rpm for 15min, then use an ultrasonic cell pulverizer to sonicate for 8min at a power of 1500W, and then sonicate at a power of 300W for 4min to form a fine emulsion;

[0047] 3) Pour the PUF prepo...

Embodiment 2

[0051] 1) Add 2.0 g of urea and 2.7 g of formaldehyde solution (37 wt%) into a three-necked flask and stir, then add 1.5 g of melamine. Use triethanolamine to adjust the pH value to 8, slowly heat up to 60°C, react at a constant temperature in a water bath for 30 minutes, detect the end point of the reaction, stop heating and wait until the temperature drops to room temperature to prepare a transparent and viscous melamine-urea formaldehyde prepolymer (MUF prepolymer) polymer);

[0052] 2) Take bisphenol A glycidyl ether type epoxy resin 11.3g as core material, 1-butyl glycidyl ether 1.5g, 0.5g sodium dodecylbenzenesulfonate as emulsifier, n-octanol 0.05g as disinfectant Foaming agent, add 100mL deionized water, and stir at 600rpm for 1h to form an O / W emulsion. Stir with a high-speed mixer at 800rpm for 10min, then use an ultrasonic cell pulverizer to sonicate for 6min at a power of 1000W, and sonicate for 1min at a power of 200W to form a fine emulsion;

[0053] 3) Pour th...

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Abstract

The invention discloses a preparation method of a self-repair nanocapsule-thermosetting-resin-base composite material, which comprises the following steps: 1) preparing a capsule wall prepolymer from urea, formaldehyde and melamine; 2) preparing a fine emulsion by using an epoxy resin as a core material; 3) uniformly mixing the prepolymer and fine emulsion, polycondensing, washing and drying to obtain the self-repair nanocapsule; and 4) adding the prepared self-repair nanocapsule into a thermosetting-resin-base composite material, curing, and carrying out after-treatment to obtain the composite material. By using the ultrasonic assisted in-situ polymerization process for preparing the self-repair nanocapsule, the method has the advantages of simple technique and controllable parameters, and the prepared nanocapsule has the advantages of small size, high stability and favorable compatibility with the thermosetting resin base, and satisfies the corresponding requirements of the composite material processing technique.

Description

technical field [0001] The invention belongs to the technical field of research on thermosetting resin-based composite materials, and in particular relates to a preparation method of a self-repairing nanocapsule / thermosetting resin-based composite material. Background technique [0002] In recent years, thermosetting resin-based composites have been widely used in aerospace, automotive and other commercial fields due to their high specific strength and specific stiffness. During the long-term use of thermosetting resin-based composites, when they are subjected to external forces, they will inevitably be damaged and produce microcracks, resulting in a decrease in mechanical properties or loss of function. Self-healing of thermosetting resin-based composites is of great significance for improving the stability of the material and prolonging its service life. [0003] With the maturity of microcapsule technology, microcapsule self-healing composite materials develop rapidly an...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L67/06C08L63/00C08L61/24C08L83/04C08K13/04C08K5/098C08K5/14C08K5/3445C08K7/14B01J13/02C08G12/36C08G12/38
Inventor 童晓梅闫子英郝芹芹任庆海
Owner SHAANXI UNIV OF SCI & TECH
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