Flame-retardant heat-resistant bismaleimide resin and preparation method thereof

A bismaleimide resin and bismaleimide technology are applied in the field of bismaleimide and its synthesis and preparation to achieve the effects of inhibiting chain segment movement, improving flame retardancy and good heat resistance.

Inactive Publication Date: 2014-12-10
HAIAN INST OF HIGH TECH RES NANJING UNIV
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

However, through the external addition method, it is inevitable to encounter the technical problems of dispersion and compatibility between the additive and the resin. This type of method often has to sacrifice the processability and mechanical properties of the bismaleimide resin.

Method used

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  • Flame-retardant heat-resistant bismaleimide resin and preparation method thereof
  • Flame-retardant heat-resistant bismaleimide resin and preparation method thereof
  • Flame-retardant heat-resistant bismaleimide resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0027] Add 32 g 1-amino-5-naphthol and 90 g acetone to a 250 mL four-necked flask equipped with mechanical stirring, thermometer, reflux condenser and nitrogen introduction device, slowly increase the temperature of the oil bath to 80°C, wait for 1- After the amino-5-naphthol was completely dissolved, 15 g of phenylphosphorus oxychloride was added dropwise to the reaction system, the 0.5h feeding was completed, the reaction temperature was controlled at 110°C, and the reaction was continued for 4h. After the reaction is completed, the unreacted 1-amino-5-naphthol is removed by concentration and filtration, washed with deionized water at 80°C for 5 times, and the solvent and excess water are removed by distillation under reduced pressure to obtain a brown viscous liquid. The resulting brown viscous liquid product 25g, 20g maleic anhydride, epichlorohydrin, and 15g acetone were mixed and dissolved in a 125 ml four-necked flask with stirring, reflux condenser and thermometer. The o...

Embodiment 2

[0030] Add 32 g 1-amino-5-naphthol and 90 g acetone into a 250 mL four-neck flask equipped with mechanical stirring, thermometer, reflux condenser and nitrogen introduction device, slowly increase the temperature of the oil bath to 80℃, After the amino-5-naphthol was completely dissolved, 15 g of phenylphosphorus oxychloride was added dropwise to the reaction system, the 0.5h feeding was completed, the reaction temperature was controlled at 110°C, and the reaction was continued for 4h. After the reaction is completed, the unreacted 1-amino-5-naphthol is removed by concentration and filtration, washed with deionized water at 80°C for 5 times, and the solvent and excess water are removed by distillation under reduced pressure to obtain a brown viscous liquid. The resulting brown viscous liquid product 25g, 20g maleic anhydride, epichlorohydrin, and 15g acetone were mixed and dissolved in a 125 ml four-necked flask with stirring, reflux condenser and thermometer. The oil bath tempe...

Embodiment 3

[0033] Add 600 g 1-amino-5-naphthol and 350 g acetone into a 2500 mL four-necked flask equipped with mechanical stirring, thermometer, reflux condenser and nitrogen introduction device, slowly increase the temperature of the oil bath to 80℃, and wait for 1 After the amino-5-naphthol was completely dissolved, 500 g of phenylphosphorus oxychloride was added dropwise to the reaction system, the 0.5h addition was completed, the reaction temperature was controlled at 115°C, and the reaction was continued for 4h. After the completion of the reaction, it was concentrated and filtered to remove unreacted 1-amino-5-naphthol, washed with deionized water at 80°C for 3 times, and distilled under reduced pressure to remove the solvent and excess water to obtain a brown viscous liquid. The resulting tan viscous liquid product 500g, 400g maleic anhydride, epichlorohydrin, and 300g acetone were mixed and dissolved in a 1500ml four-necked flask equipped with stirring, reflux condenser and thermo...

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Abstract

The invention discloses flame-retardant heat-resistant bismaleimide resin and a preparation method thereof, belonging to the technical field of high performance thermosetting resin. According to the technical scheme, the flame-retardant heat-resistant bismaleimide resin is prepared from the following raw materials in parts by weight: 5-20 parts of phenylphosphonic dichloride, 21-52 parts of 1-amino-5-naphthol and 10-40 parts of maleic anhydride. The bismaleimide resin has a good molding technology and a cured product has high heat resistance and excellent flame retardance; the glass-transition temperature of the cured product reaches 370 DEG C, and the limit oxygen index reaches 48; benzyl di(5-amino) naphthoxy phosphonic acid is prepared by reaction between phenylphosphonic dichloride and excessive 1-amino-5-naphthol, and prepared benzyl di(5-amino) naphthoxy phosphonic acid is reacted with maleic anhydride to obtain the flame-retardant heat-resistant bismaleimide resin. The flame-retardant heat-resistant bismaleimide resin and the preparation method disclosed by the invention have the beneficial effects that the reaction is stable, the process condition is easy to control, unreacted raw materials can be recycled, and no three wastes are generated, so that the flame-retardant heat-resistant bismaleimide resin and the preparation method are suitable for industrialized production.

Description

Technical field [0001] The invention relates to the field of bismaleimide and its synthesis and preparation, in particular to a flame-retardant and heat-resistant bismaleimide resin and a preparation method thereof. Background technique [0002] Bismaleimide (BMI) is a type of resin system derived from polyimide resin system. It is a bifunctional compound with maleimide (MI) as the active end group. The use temperature of its resin is between epoxy resin and polyimide. Bismaleimide resin-based composite material has excellent high temperature resistance, radiation resistance, damp heat resistance, and good manufacturability. It is mainly used in aerospace , Composite material matrix in the fields of machinery and electronics, transportation and so on. [0003] General-purpose bismaleimide resin is usually solid at room temperature, with high curing temperature, long time, and general flame retardancy. In order to further improve the flame retardant performance of bismaleimide res...

Claims

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Application Information

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Patent Type & Authority Applications(China)
IPC IPC(8): C08G73/12
Inventor 任华曹婷婷张亚仇叶云
Owner HAIAN INST OF HIGH TECH RES NANJING UNIV
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