Self-toughened benzoxazine thermosetting resin and method for preparing same

Abstract

The invention provides self-toughened benzoxazine thermosetting resin with structures shown as a formula I. The self-toughened benzoxazine thermosetting resin has the advantages that long alkyl chainsare led into chemical structures of benzoxazine, accordingly, toughening effects can be realized, and the self-toughened benzoxazine thermosetting resin has self-toughened characteristics; the long alkyl chains are led into the chemical structures of the benzoxazine in chemical bond forms, and accordingly the problem that the traditional added toughening agents are dissolved out due to poor compatibility can be effectively solved; the long alkyl chains are added into the self-toughened benzoxazine thermosetting resin, the concentration of oxazine rings can be diluted, and accordingly the curing temperature of the self-toughened benzoxazine thermosetting resin can be obviously lowered; the long alkyl chains are led into the structures of the benzoxazine, good internal plasticization effects can be realized, and accordingly the toughness of self-toughened benzoxazine thermosetting resin cured substances can be greatly improved.

Description

technical field

[0001] The invention relates to the technical field of organic polymer materials, in particular to a self-toughening benzoxazine thermosetting resin and a preparation method thereof. Background technique

[0002] Benzoxazine resin (benzoxazine) refers to a class of aromatic polymers containing oxazine rings. It is one of the organic polymer materials with the best comprehensive performance. It has high temperature resistance, flame retardancy, excellent mechanical properties, low surface energy, The advantages of flexible monomer structure design, corrosion resistance, etc., and small thermal expansion coefficient, good wear resistance, excellent dielectric properties, have been widely used in electronics, aerospace and other fields. However, because of its high rigid structure content, the cured polybenzoxazine has the problems of poor toughness and low elongation at break.

[0003] In view of the above problems, the conventional improvement method is to ad...

Examples

preparation example Construction

[0029] The invention provides a preparation method of the self-toughening benzoxazine thermosetting resin, comprising the following steps:

[0030] The aminomethylation reaction is carried out after mixing the decanediamine solution and the formaldehyde solution to obtain an aminomethylation reaction product system;

[0031] The aminomethylation reaction product system is mixed with bisphenol A and then subjected to Mannich reaction to obtain a self-toughening benzoxazine thermosetting resin having a structure shown in formula I.

[0032] In the present invention, the aminomethylation reaction is carried out after mixing the decanediamine solution and the formaldehyde solution to obtain an aminomethylation reaction product system. In the present invention, the molar ratio of decanediamine in the decanediamine solution to formaldehyde in the formaldehyde solution is preferably 1: (4-6).

[0033] In the present invention, the mass concentration of the decanediamine solution is ...

Embodiment 1

[0053] Dissolve bisphenol A in hot toluene at 50°C first, then allow it to cool and crystallize naturally, filter it with suction, and dry it for 12 hours at a relative vacuum degree of less than -0.085Mpa and a temperature of 60°C to obtain the first purified bisphenol A; Dissolve the obtained initially purified bisphenol A in hot 1,4-dioxane at 50°C, allow it to cool and crystallize naturally, filter it with suction, and put it under a relative vacuum less than -0.085Mpa at a temperature of Dry at 60°C for 12 hours, place the obtained bisphenol A in a desiccator for use;

[0054] According to the molar ratio of decanediamine to formaldehyde of 1:4, decanediamine was dissolved in 1,4-dioxane at 0°C to prepare 1,4-dioxane with a mass concentration of 5%. 4-dioxane solution, and the aqueous solution of formaldehyde with a mass concentration of 35% was added dropwise to the 1,4-dioxane solution of decanediamine in the form of dropwise addition. During the process, the temperatu...

Embodiment 2

[0060] Dissolve bisphenol A in hot toluene at 60°C first, then allow it to cool and crystallize naturally, filter it with suction, and dry it for 15 hours at a relative vacuum degree of less than -0.085Mpa and a temperature of 65°C to obtain the first purified bisphenol A; Dissolve the obtained initially purified bisphenol A in hot 1,4-dioxane at 55°C, allow it to cool and crystallize naturally, filter it with suction, and put it under a relative vacuum less than -0.085Mpa at a temperature of Dry at 65°C for 15 hours, place the obtained bisphenol A in a desiccator for use;

[0061] According to the molar ratio of decanediamine to formaldehyde of 1:4.5, decanediamine was dissolved in 1,4-dioxane at 2°C to prepare 1,4-dioxane with a mass concentration of 6%. 4-dioxane solution, and the aqueous solution of formaldehyde with a mass concentration of 37% was added dropwise in the 1,4-dioxane solution of decanediamine by means of dropwise addition. During the process, the temperatur...

technical field

[0001] The invention relates to the technical field of organic polymer materials, in particular to a self-toughening benzoxazine thermosetting resin and a preparation method thereof. Background technique

[0002] Benzoxazine resin (benzoxazine) refers to a class of aromatic polymers containing oxazine rings. It is one of the organic polymer materials with the best comprehensive performance. It has high temperature resistance, flame retardancy, excellent mechanical properties, low surface energy, The advantages of flexible monomer structure design, corrosion resistance, etc., and small thermal expansion coefficient, good wear resistance, excellent dielectric properties, have been widely used in electronics, aerospace and other fields. However, because of its high rigid structure content, the cured polybenzoxazine has the problems of poor toughness and low elongation at break.

[0003] In view of the above problems, the conventional improvement method is to ad...

Examples

preparation example Construction

[0029] The invention provides a preparation method of the self-toughening benzoxazine thermosetting resin, comprising the following steps:

[0030] The aminomethylation reaction is carried out after mixing the decanediamine solution and the formaldehyde solution to obtain an aminomethylation reaction product system;

[0031] The aminomethylation reaction product system is mixed with bisphenol A and then subjected to Mannich reaction to obtain a self-toughening benzoxazine thermosetting resin having a structure shown in formula I.

[0032] In the present invention, the aminomethylation reaction is carried out after mixing the decanediamine solution and the formaldehyde solution to obtain an aminomethylation reaction product system. In the present invention, the molar ratio of decanediamine in the decanediamine solution to formaldehyde in the formaldehyde solution is preferably 1: (4-6).

[0033] In the present invention, the mass concentration of the decanediamine solution is ...

Embodiment 1

[0053] Dissolve bisphenol A in hot toluene at 50°C first, then allow it to cool and crystallize naturally, filter it with suction, and dry it for 12 hours at a relative vacuum degree of less than -0.085Mpa and a temperature of 60°C to obtain the first purified bisphenol A; Dissolve the obtained initially purified bisphenol A in hot 1,4-dioxane at 50°C, allow it to cool and crystallize naturally, filter it with suction, and put it under a relative vacuum less than -0.085Mpa at a temperature of Dry at 60°C for 12 hours, place the obtained bisphenol A in a desiccator for use;

[0054] According to the molar ratio of decanediamine to formaldehyde of 1:4, decanediamine was dissolved in 1,4-dioxane at 0°C to prepare 1,4-dioxane with a mass concentration of 5%. 4-dioxane solution, and the aqueous solution of formaldehyde with a mass concentration of 35% was added dropwise to the 1,4-dioxane solution of decanediamine in the form of dropwise addition. During the process, the temperatu...

Embodiment 2

[0060] Dissolve bisphenol A in hot toluene at 60°C first, then allow it to cool and crystallize naturally, filter it with suction, and dry it for 15 hours at a relative vacuum degree of less than -0.085Mpa and a temperature of 65°C to obtain the first purified bisphenol A; Dissolve the obtained initially purified bisphenol A in hot 1,4-dioxane at 55°C, allow it to cool and crystallize naturally, filter it with suction, and put it under a relative vacuum less than -0.085Mpa at a temperature of Dry at 65°C for 15 hours, place the obtained bisphenol A in a desiccator for use;

[0061] According to the molar ratio of decanediamine to formaldehyde of 1:4.5, decanediamine was dissolved in 1,4-dioxane at 2°C to prepare 1,4-dioxane with a mass concentration of 6%. 4-dioxane solution, and the aqueous solution of formaldehyde with a mass concentration of 37% was added dropwise in the 1,4-dioxane solution of decanediamine by means of dropwise addition. During the process, the temperatur...

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