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Preparation method of self-repairing reshapeable multi-deformation thermosetting shape-memory resin system

A self-healing, thermosetting technology, applied in the field of shape memory functional high-performance resin matrix, can solve the problems of memory resin that cannot be reshaped, micro-crack damage, complex shape deformation can not be effectively realized, etc., to achieve stable shape memory performance, The effect of many recovery cycles and excellent heat resistance

Active Publication Date: 2018-09-21
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

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Problems solved by technology

[0005] The purpose of the present invention is to propose a remodelable shape with crack self-repairing function in view of the problems that the current thermosetting shape memory resin cannot be reshaped, cannot effectively realize complex shape deformation, and will have micro-crack damage during use. Multiple deformation thermosetting shape memory resin system and preparation method thereof

Method used

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  • Preparation method of self-repairing reshapeable multi-deformation thermosetting shape-memory resin system
  • Preparation method of self-repairing reshapeable multi-deformation thermosetting shape-memory resin system
  • Preparation method of self-repairing reshapeable multi-deformation thermosetting shape-memory resin system

Examples

Experimental program
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Effect test

Embodiment 1

[0033]Dissolve 5g of bismaleimidodiphenylmethane (BMI) and 4g of 4,4'-diaminodiphenylsulfone in acetone in a cooling reflux device, and react at a controlled temperature of 60°C for 12 hours under stirring conditions , the solution was removed by rotary evaporation to remove the acetone solvent, and then vacuum-dried at 70° C. for 12 hours to obtain bismaleimide / aromatic diamine oligomer powder. Add the oligomer to 75g of epoxy resin (E-54), melt into a transparent solution at 100°C, add 4g of accelerator zinc acetylacetonate, stir for about 3 minutes, then add 12g of glutaric anhydride, stir quickly and mix well Finally, it is poured into a flat mold, and after vacuum defoaming at 110°C, it is treated according to the curing process 110°C / 1h+140°C / 8h+160°C / 2h, and the cured material is taken out after natural cooling.

[0034] figure 1 It is a diagram of the transesterification reaction and crack repair mechanism. In the material of the present invention, under the condition...

Embodiment 2

[0041] Dissolve 13g of bismaleimidodiphenylmethane (BMI) and 9g of 4,4'-diaminodiphenylsulfone in acetone in a cooling reflux device, and react at a controlled temperature of 70°C for 12h under stirring conditions , the solution was removed by rotary evaporation to remove the acetone solvent, and then vacuum-dried at 70° C. for 12 hours to obtain bismaleimide / aromatic diamine oligomer powder. Add the oligomer to 100g of epoxy resin (E-51), melt into a transparent solution at 100°C, add 6.7g of accelerator zinc acetylacetonate, stir for about 3 minutes, then add 15g of glutaric anhydride, stir and mix quickly After uniformity, it is poured into a flat mold, and after vacuum defoaming at 110°C, it is treated according to the curing process 110°C / 1h+140°C / 8h+160°C / 2h, and the cured material is taken out after natural cooling.

[0042] Figure 4 is the shape memory cycle curve (DMA test) of the material of Example 2. The glass transition temperature of the prepared material is 1...

Embodiment 3

[0045] After dissolving 25g of bismaleimide diphenyl ether and 18g of 4,4'-diaminodiphenyl ether in acetone in a cooling reflux device, under stirring conditions, the temperature was controlled at 70°C for 12 hours, and the After the acetone solvent was removed by rotary evaporation, the solution was vacuum-dried at 70° C. for 12 hours to obtain bismaleimide / aromatic diamine oligomer powder. Add the oligomer to 120g of novolac epoxy resin (F-51), melt it into a transparent solution at 100°C, add 8g of accelerator zinc acetylacetonate, stir for about 5 minutes, and then add 18g of hexahydrophthalo Acid anhydride, after stirring quickly and mixing evenly, pour it into a flat mold, after vacuum defoaming at 110°C, treat it according to the curing process 110°C / 1h+140°C / 8h+160°C / 2h, and take out the solidified material after natural cooling.

[0046] Figure 6 is the shape memory cycle curve (DMA test) of the above materials. The glass transition temperature of the prepared mate...

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Abstract

The invention discloses a preparation method of a self-repairing reshapeable multi-deformation thermosetting shape-memory resin system. The resin system mainly comprises the following raw materials: bismaleimide, aromatic diamine, epoxy resin, dicarboxylic anhydride and a transesterification accelerant; bismaleimide resin is subjected to a chain extension reaction by the aromatic diamine to form alinear oligomer, then the epoxy resin, the accelerant and the dicarboxylic anhydride are added, and after a certain thermal curing process is performed, a reshapeable multi-deformation thermosettingshape-memory material with self-repairing function is obtained. The material prepared with the method can not only be reshaped into a new shape, but also is good in shape memory effect when the deformation recovery cycle reaches 5 times or more than 5 times, and materials prepared therefrom are good in self-repairing capability and has the fracture toughness repairing efficiency being 62% or morethan 62%. Therefore, the prepared materials have wide application potential in high-performance structural-functional integration materials.

Description

[0001] The present invention is a divisional application for a self-repairable reshapeable multiple deformation thermosetting shape memory resin material and its preparation method, the application date is December 12, 2016, and the application number is 201611141129X. technical field [0002] The invention belongs to the technical field of shape-memory functionalized high-performance resin matrix, and relates to a preparation method of a self-repairable remodelable multiple-deformation thermosetting shape-memory resin system. Background technique [0003] Shape memory polymers (SMPs) are unique stimuli-responsive polymers whose shape can be programmed into a temporary shape and return to their original initial shape under specific external stimuli. As a class of smart materials capable of autonomous deformation, SMPs have the advantages of light weight, low cost, easy processing, easy control of shape change, and easy adjustment of transition temperature. As thermosetting S...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08L63/00C08L63/04C08L79/08C08G59/42C08G59/58C08G59/70C08G73/12
CPCC08G59/4207C08G59/4215C08G59/58C08G59/70C08G73/12C08L63/00C08L63/04C08L2201/12C08L2201/08C08L79/08
Inventor 袁莉丁振杰顾嫒娟梁国正管清宝
Owner SUZHOU UNIV
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