A kind of self-toughening benzoxazine thermosetting resin and preparation method thereof

Abstract

The invention provides a self-toughening benzoxazine thermosetting resin with the structure shown in formula I. The present invention introduces long alkyl chains into the chemical structure of benzoxazine, so as to play a role of toughening, so that the obtained benzoxazine thermosetting resin has the characteristic of self-toughening; at the same time, through the form of chemical bonds, the long The introduction of the alkyl chain into the chemical structure of benzoxazine effectively avoids the problem of precipitation due to poor compatibility of traditional toughening agents. In addition, in the self-toughening benzoxazine thermosetting resin provided by the present invention, due to the addition of long alkyl chains, the concentration of oxazine rings is effectively diluted, thereby also significantly reducing the concentration of the self-toughening benzoxazine. The curing temperature of a thermosetting resin. In addition, long alkyl chains are introduced into the structure of benzoxazine, which can play a good role in internal plasticization, so the toughness of the self-toughening benzoxazine thermosetting resin cured product is also 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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