Bimaleimide composition and preparation method thereof

Abstract

The invention provides a bimaleimide composition, and a preparation method and an application thereof. The composition comprises a compound of formula I, a compound of formula II and a compound of formula III. The invention also provides the preparation method of the bimaleimide composition. The bimaleimide composition has a high heatproof property, the Gardner color scale of a heatproof resin product made from the composition reaches 14# to 18#, the heatproof property of the heatproof resin composition is obviously higher than that of bimaleimide prepared through general technologies and commercial resin products, the foaming tolerance duration in tin immersion experiments reaches up to 19-24 min, and is far higher than that of common products, and the bimaleimide composition has the advantages of excellent heatproof property, high application values and good application prospect.

Description

technical field

[0001] The invention belongs to the field of resin materials, and relates to a bismaleimide composition and a preparation method thereof. Background technique

[0002] Bismaleimide is another type of resin system derived from polyimide resin system. At present, it mainly includes two preparation methods, one is toluene solvent method, and the other is acetone solvent method. Both methods are to synthesize bismaleimide monomers under acidic catalyst conditions, and use the solubility of bismaleimide in two solvents to continuously wash and purify to obtain pure products. However, during the synthesis process, a by-product of bismaleimide will be produced. There are many speculations about the synthesis mechanism of this by-product, but the monomer structure is a derivative of bismaleimide. The by-product is a viscous fluid liquid in the solvent phase, and becomes a granular, agglomerated solid when it meets water. The by-product is generally treated as waste ...

Examples

Embodiment 1

[0063] This embodiment prepares the bismaleimide composition through the following steps

[0064] (1) Dissolve diaminodiphenylmethane in a solvent, drop it into a solvent containing maleic anhydride at 20°C within 3 hours, wherein the molar ratio of maleic anhydride to diaminodiphenylmethane is 2 : 1, solvent is toluene, adds p-toluenesulfonic acid, wherein the weight ratio of p-toluenesulfonic acid and toluene is 0.25:1, is heated to reflux reaction 3h, in the reaction process, the water in the system is continuously separated with a water separator, Then cool down to 80°C, add water to the system, let it stand, filter out the insoluble matter obtained by the reaction, wherein the weight ratio of water to solvent is 1:1, stir and raise the temperature to 100°C, let it stand for stratification, and drain the lower layer of water, Collect the upper layer solution.

[0065] (2) Dissolve the insoluble matter obtained in step (1) and the upper layer solution in toluene, heat to 9...

Embodiment 2

[0069] This embodiment prepares the bismaleimide composition through the following steps

[0070] (1) Dissolve diaminodiphenylmethane in a solvent, drop it into a solvent containing maleic anhydride at 25° C. within 1 hour, wherein the reaction molar ratio of maleic anhydride to diaminodiphenylmethane is 1.5: 1, the solvent is toluene and dimethylformamide (the weight ratio of toluene and dimethylformamide is 1:1), add p-toluenesulfonic acid, wherein the weight ratio of p-toluenesulfonic acid and solvent is 0.5:1, heat After reflux for 1 hour, the water in the system was continuously separated with a water separator during the reaction, and then the temperature was lowered to 70°C, water was added to the system, and the insoluble matter obtained by the reaction was filtered off. The weight of water and solvent The ratio is 0.1:1. Stir and heat up to 80°C and let stand to separate layers. The water in the lower layer is drained and the upper layer solution is collected.

[007...

Embodiment 3

[0073] This embodiment prepares the bismaleimide composition through the following steps

[0074] (1) Dissolve diaminodiphenylmethane in a solvent, drop it into a solvent containing maleic anhydride at 10°C within 5 hours, wherein the reaction molar ratio of maleic anhydride to diaminodiphenylmethane is 3 :1, the solvent is toluene and acetone (the weight ratio of toluene and acetone is 1:0.5), adding p-toluenesulfonic acid, wherein the weight ratio of p-toluenesulfonic acid and solvent is 0.01:1, heated to reflux for 6h, the reaction process Use a water separator to continuously separate the water in the system, then cool down to 70°C, add water to the system, let it stand, filter out the insoluble matter obtained by the reaction, wherein the weight ratio of water to solvent is 2:1, stir Raise the temperature to 105°C and let stand to separate layers, drain the water from the lower layer, and collect the upper layer solution.

[0075] (2) Dissolve the insoluble matter obtain...

technical field

[0001] The invention belongs to the field of resin materials, and relates to a bismaleimide composition and a preparation method thereof. Background technique

[0002] Bismaleimide is another type of resin system derived from polyimide resin system. At present, it mainly includes two preparation methods, one is toluene solvent method, and the other is acetone solvent method. Both methods are to synthesize bismaleimide monomers under acidic catalyst conditions, and use the solubility of bismaleimide in two solvents to continuously wash and purify to obtain pure products. However, during the synthesis process, a by-product of bismaleimide will be produced. There are many speculations about the synthesis mechanism of this by-product, but the monomer structure is a derivative of bismaleimide. The by-product is a viscous fluid liquid in the solvent phase, and becomes a granular, agglomerated solid when it meets water. The by-product is generally treated as waste ...

Examples

Embodiment 1

[0063] This embodiment prepares the bismaleimide composition through the following steps

[0064] (1) Dissolve diaminodiphenylmethane in a solvent, drop it into a solvent containing maleic anhydride at 20°C within 3 hours, wherein the molar ratio of maleic anhydride to diaminodiphenylmethane is 2 : 1, solvent is toluene, adds p-toluenesulfonic acid, wherein the weight ratio of p-toluenesulfonic acid and toluene is 0.25:1, is heated to reflux reaction 3h, in the reaction process, the water in the system is continuously separated with a water separator, Then cool down to 80°C, add water to the system, let it stand, filter out the insoluble matter obtained by the reaction, wherein the weight ratio of water to solvent is 1:1, stir and raise the temperature to 100°C, let it stand for stratification, and drain the lower layer of water, Collect the upper layer solution.

[0065] (2) Dissolve the insoluble matter obtained in step (1) and the upper layer solution in toluene, heat to 9...

Embodiment 2

[0069] This embodiment prepares the bismaleimide composition through the following steps

[0070] (1) Dissolve diaminodiphenylmethane in a solvent, drop it into a solvent containing maleic anhydride at 25° C. within 1 hour, wherein the reaction molar ratio of maleic anhydride to diaminodiphenylmethane is 1.5: 1, the solvent is toluene and dimethylformamide (the weight ratio of toluene and dimethylformamide is 1:1), add p-toluenesulfonic acid, wherein the weight ratio of p-toluenesulfonic acid and solvent is 0.5:1, heat After reflux for 1 hour, the water in the system was continuously separated with a water separator during the reaction, and then the temperature was lowered to 70°C, water was added to the system, and the insoluble matter obtained by the reaction was filtered off. The weight of water and solvent The ratio is 0.1:1. Stir and heat up to 80°C and let stand to separate layers. The water in the lower layer is drained and the upper layer solution is collected.

[007...

Embodiment 3

[0073] This embodiment prepares the bismaleimide composition through the following steps

[0074] (1) Dissolve diaminodiphenylmethane in a solvent, drop it into a solvent containing maleic anhydride at 10°C within 5 hours, wherein the reaction molar ratio of maleic anhydride to diaminodiphenylmethane is 3 :1, the solvent is toluene and acetone (the weight ratio of toluene and acetone is 1:0.5), adding p-toluenesulfonic acid, wherein the weight ratio of p-toluenesulfonic acid and solvent is 0.01:1, heated to reflux for 6h, the reaction process Use a water separator to continuously separate the water in the system, then cool down to 70°C, add water to the system, let it stand, filter out the insoluble matter obtained by the reaction, wherein the weight ratio of water to solvent is 2:1, stir Raise the temperature to 105°C and let stand to separate layers, drain the water from the lower layer, and collect the upper layer solution.

[0075] (2) Dissolve the insoluble matter obtain...

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