Toughening modification preparation method of benzoxazine

A benzoxazine, toughening modification technology, applied in the field of benzoxazine toughening modification preparation, composite materials, can solve the problems of reduced toughness, poor film formation, poor processing performance, etc. Improved film properties, simple curing process, and improved mechanical properties

Active Publication Date: 2021-11-02
CIVIL AVIATION FLIGHT UNIV OF CHINA
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0005] The defect of the above-mentioned patents is that the modifiers are mostly inorganic fillers, adding a large amount will reduce the mechanical properties of the benzoxazine material, and the addition of the toughening agent will increase the viscosity of the benzoxazine and deteriorate the processing performance; in addition, the benzoxazine The ring-opening polymerization temperatures of oxazine and thermosetting resins are similar, and there is competition between the two types of thermosetting resins during polymerization and crosslinking. Reduced, poor film formation

Method used

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  • Toughening modification preparation method of benzoxazine
  • Toughening modification preparation method of benzoxazine
  • Toughening modification preparation method of benzoxazine

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0032] Embodiment 1 (PHT / PHB-a)

[0033] Such as Figures 1 to 4 As shown, this example provides a preparation method for toughening and modifying benzoxazine. mmol), 3-phenyl-6-formyl-3,4-dihydro-2H-1,3-benzoxazine (PHB-a) (0.32mmol) and formaldehyde (2mmol) were added to a glass bottle, and Add 2.0ml of N-methylpyrrolidone (NMP) as a solvent, stir the mixed solution at room temperature until it is completely dissolved, filter it and pour it on a clean glass plate, react the blended system at 50°C for 12h, and react at 200°C for 2h for curing to obtain Dark red blend polymer interpenetrating network, the interpenetrating network has good mechanical properties and thermal properties: nitrogen atmosphere, 800 ℃ residual carbon were 45.4%, 53.1%, 59.2%, elongation at break 5.31%, 8.47% , 6.43%, tensile strength of 106.6MPa, 105.9MPa, 97.5MPa.

[0034] from figure 2 It was found that the resin was too brittle to form a film; from image 3 It can be found that the cross-sect...

Embodiment 2

[0037] Example 2 (PHT / bis-M)

[0038]This example provides a preparation method for the toughening modification of benzoxazine. 1,3-bis(4-aminophenoxy)benzene[4,4'-(1,3-Phenylenedioxy)dianiline](0.4mmol), Bis(4-phenyl-3,4-dihydro-2H-1,3-benzoxazine)methane (bis-M) (0.16mmol) and formaldehyde (2mmol) were added to a glass bottle, and 2.0mL N- Methylpyrrolidone (NMP) was used as a solvent, and the mixed solution was stirred at room temperature until it was completely dissolved. After filtering, it was poured onto a clean glass plate. The blend system was reacted at 80°C for 6h, and then solidified at 180°C for 6h to obtain a dark red benzoxan In the oxazine system, the residual carbon at 800°C is 42.2%, 45.1%, 54.8%, the elongation at break is 6.40%, 7.47%, 10.5%, and the tensile strength is 101.6MPa, 121.9MPa, 122.5MPa.

[0039] The reaction formula involved in embodiment 2 is as follows:

[0040]

Embodiment 3

[0041] Example 3 (PHT / bis-MO)

[0042] This example provides a preparation method for the toughening modification of benzoxazine. 1,3-bis(4-aminophenoxy)benzene[4,4'-(1,3-Phenylenedioxy)dianiline](0.4mmol), Add bis(4-phenyl-3,4-dihydro-2H-1,3-benzoxazine)methanone (bis-MO) (1.28mmol) and formaldehyde (2mmol) into a glass bottle, and add 2.0ml N -Methylpyrrolidone (NMP) was used as a solvent, the mixed solution was stirred at room temperature until it was completely dissolved, filtered and poured onto a clean glass plate, the blend system was reacted at 60°C for 10h, and reacted at 190°C for 4h to solidify to obtain a dark red benzo Oxazine system, nitrogen atmosphere, 800 ℃ residual carbon is 46.4%, 48.7%, 54.8%, elongation at break is 7.02%, 8.13%, 9.27%, tensile strength is 98.2MPa, 116.3MPa, 114.8MPa.

[0043] The reaction formula involved in embodiment 3 is as follows:

[0044]

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Abstract

The invention discloses a toughening modification preparation method of benzoxazine, relates to the technical field of composite materials. The method solves the defects of insufficient toughness and poor film-forming property of the existing benzoxazine, and comprises the following steps: adding 1, 3-bis (4-aminophenoxy) benzene, a benzoxazine resin monomer and formaldehyde into a glass bottle, and adding N-methyl pyrrolidone as a solvent to obtain a mixed solution; stirring the mixed solution at room temperature until the mixed solution is completely dissolved, filtering and pouring onto a glass plate; curing the mixed solution poured on the glass plate in the step 2 at 50-80 DEG C for 6-12 hours, curing at 180-200 DEG C for 2-6 hours, and naturally cooling to obtain a polyhexahydrotriazine/benzoxazine condensate film; wherein the modified benzoxazine cured product keeps good thermal performance, the mechanical property of benzoxazine is remarkably improved, and the problem that the benzoxazine is poor in film-forming property is solved.

Description

technical field [0001] The invention relates to the technical field of composite materials, more specifically to the technical field of preparation of benzoxazine toughening modification. Background technique [0002] Benzoxazine is a new type of high-performance thermosetting resin, which has the advantages of flexible molecular design, ring-opening crosslinking without catalyst, zero shrinkage during curing, and excellent thermal performance. Based on the above advantages, benzoxazine is a high-performance The application potential of composite material matrix resin is huge, but the disadvantages of benzoxazine cured product such as high brittleness and poor film-forming property further limit its application. [0003] In order to overcome these shortcomings and obtain benzoxazine resins with better properties, blending with high-toughness resins is a commonly used toughening modification method for benzoxazines. Such as blending with other materials such as liquid rubber...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08J5/18C08L61/34C08L79/04C08G14/06
CPCC08J5/18C08G14/06C08J2361/34C08J2479/04Y02T50/40
Inventor 徐艺李政白朱珂琪孙鑫悦杨楠李超
Owner CIVIL AVIATION FLIGHT UNIV OF CHINA
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