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Thermosetting shape memory resin based on bismaleimide and preparation method thereof

A bismaleimide, thermosetting technology, applied in the field of thermosetting shape memory resin and its preparation, can solve problems such as deterioration and lowering of tensile strength, achieve moderate crosslinking density, avoid brittle fracture, and excellent rotational flexibility. Effect

Active Publication Date: 2018-09-04
SUZHOU UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

In order to solve these problems, people try to introduce aliphatic chains and (or) adjust the cross-linking density and other methods, but often lead to T g Reduction and / or deterioration of tensile strength
[0005] In summary, the existing technology has made great progress in the research and development of shape memory polymers. However, the research and development have both excellent heat resistance ( T g >130℃), high strain, high impact strength, high tensile strength thermosetting shape memory resin is still a huge challenge

Method used

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  • Thermosetting shape memory resin based on bismaleimide and preparation method thereof
  • Thermosetting shape memory resin based on bismaleimide and preparation method thereof
  • Thermosetting shape memory resin based on bismaleimide and preparation method thereof

Examples

Experimental program
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Effect test

Embodiment 1

[0041] Add 89.6 g of N,N-(4,4-methylenediphenyl)bismaleimide and 22.5 g of 1,6-hexanedithiol to 500 mL of m-cresol to form 0.8 mol L -1 solution; add 2 mL of triethylamine dropwise to the solution, N 2 Under protection and stirring conditions, react at room temperature for 4h. After the reaction, the reaction solution was added into methanol acidified with glacial acetic acid, precipitated, filtered, washed with methanol, and dried to obtain a linear oligomer, which was designated as PSM. The number average molecular weight of PSM is 2434 g mol -1 , the dispersion index (PDI=Mw / Mn) is 1.48. Infrared (IR) spectrum and H NMR spectrum of PSM ( 1 H NMR) see attached figure 1 and 2 .

[0042] 10.0g of O,O´-diallyl bisphenol A, 55.2g of PSM (this PSM is used in the following examples, no special note) and 3.5g of N,N-(4,4-methylenebisphenol Phenyl)bismaleimide was mixed and vigorously stirred at 130°C for 30min to obtain a clear and transparent prepolymer. Pour the prepolym...

Embodiment 2

[0046] Mix 10.0g O,O´-diallyl bisphenol A, 47.3g PSM and 4.6g N,N-(4,4-methylenediphenyl)bismaleimide at 130℃ Stir vigorously for 30 minutes to obtain a clear and transparent prepolymer. Pour the prepolymer into the preheated mold, and put the mold into a vacuum oven at 130°C for degassing. Then, the mold is put into a blast drying oven. Curing and post-treatment were performed sequentially according to the procedures of 140°C / 2h+160°C / 2h+180°C / 2h and 200°C / 6h. After the end, it was naturally cooled in an oven to obtain a bismaleimide-based thermosetting shape memory resin, denoted as 6BHD. Its glass transition temperature, crosslinking density, initial decomposition temperature, impact strength, tensile strength, fracture strain and shape memory properties are respectively shown in the attached image 3 , 4 , 5, 6, 7, 8 and Schedule 1.

[0047] See attached image 3 , which is the loss factor (Tan δ )-Temperature curve. As can be seen therefrom, the glass transition ...

Embodiment 3

[0060] Mix 10.0g O,O´-diallyl bisphenol A, 39.5g PSM and 5.8g N,N-(4,4-methylenediphenyl)bismaleimide at 130°C Stir vigorously for 30 minutes to obtain a clear and transparent prepolymer. Pour the prepolymer into the preheated mold, and put the mold into a vacuum oven at 130°C for degassing. Then, the mold is put into a blast drying oven. Curing and post-treatment were performed sequentially according to the procedures of 130°C / 2h+150°C / 1h+165°C / 4h+180°C / 2h and 200°C / 6h. After the end, cool naturally with the oven to obtain a thermosetting shape memory resin based on bismaleimide; glass transition temperature T g The temperature is 145°C, the initial decomposition temperature is not lower than 370°C, the tensile strength at room temperature is greater than 51MPa, the elongation at break is greater than 35%, and the shape recovery rate and shape fixation rate are both greater than 96%.

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Abstract

The invention relates to high-deformation thermosetting shape memory resin based on bismaleimide and a preparation method thereof. The method includes the following steps that the bismaleimide and 1,6-ethanthiol are added into m-cresol to form a solution; triethylamine is added into the solution dropwisely, and under the protection of N2 and a stirring condition, a reaction is carried out at roomtemperature to obtain a linear oligomer; the bismaleimide, the linear oligomer and O,O'-diallylbisphenol A are mixed by mass, and the reaction is carried out at 130-150 DEG C for 25-45 min to obtain aprepolymer; the prepolymer is subjected to vacuum defoamation at the temperature of 130-150 DEG C, and through solidification and post-treatment, the thermosetting shape memory resin based on the bismaleimide is obtained. Compared with the prior art, the resin has a high deformation capability, and the breaking elongation of the resin at programming temperatures is higher than 30%; moreover, thethermosetting resin has both high glass-transition temperature (larger than 131 DEG C) and initial decomposition temperature (larger than 370 DEG C), high tenacity and outstanding shape memory performance.

Description

technical field [0001] The invention relates to a thermosetting shape memory resin based on bismaleimide and a preparation method thereof, belonging to the field of thermosetting shape memory polymers. Background technique [0002] In order to meet the development trend of large-scale space unfolding structures, the space unfolding structures should be foldable and can be stably unfolded after reaching the specified position. Mechanical expansion structures and inflatable expansion structures are two commonly used spatial expansion structures, but the former has the disadvantages of large vibration and heavy weight, while the latter often shows the disadvantage of low strength. Therefore, there is an urgent need to develop light-weight, high-strength space-expanding structures. [0003] A class of smart materials with active deformation properties - shape memory polymers has attracted the attention of researchers. Not only can they be deformed, but they can be "locked" int...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G75/025C08G75/0236C08L81/02
CPCC08G75/0236C08G75/0272C08L81/02C08L2201/12
Inventor 顾嫒娟陈帮辉梁国正袁莉
Owner SUZHOU UNIV
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