Bismaleimide resin for microdiameter pultrusion process and preparation method thereof

A technology of bismaleimide and pultrusion molding, which is applied in the field of bismaleimide and its synthesis and preparation, can solve the problems of poor solubility, short pot life, less pultrusion molding process, etc., and achieve good heat resistance Performance, Suppression of Segment Motion, Wide Range of Effects

Inactive Publication Date: 2012-09-05
NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

[0003] Bismaleimide resin is usually solid at room temperature, and the curing temperature is high and takes a long time. Unmodified bismaleimide resin has disadvantages such as high melting point, poor solubility, high molding temperature, and high brittleness of the cured product.
The pultrusion molding process is a kind of composite material molding process. It has the characteristics of strong designability of material properties, stable size of composite materials, and high degree of automation. It is required that the resin raw materials used in the pultrusion process have a lower viscosity at the set dipping temperature. and longer pot life, while micro-diameter pultrusion requires resin to have better wettability to carbon fiber, glass fiber and other reinforcing materials. If the unmodified bismaleimide resin meets the requirements of pultrusion Viscosity requires a higher dipping temperature, and at this high temperature, the bismaleimide resin has reached the self-polymerization reaction temperature, and the viscosity of the resin system rises rapidly with the increase of the molecular weight, and the pot life is extremely short, which cannot meet the requirements of compounding. Material pultrusion process requirements
[0004] The current public reports mainly focus on the toughening and viscosity reduction of bismaleimide resins, involving various molding processes including resin transfer molding (RTM), but there are very few pultrusion molding processes.

Method used

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Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0031] Add 90 g of 4,4'-diallyl bisphenol A and 15 g of 4,4'-diaminodiphenyl sulfone into a 500 mL four-neck flask equipped with mechanical stirring, thermometer, reflux condenser and nitrogen introduction device and 100 g of 4,4'-bismaleimide diphenylmethane, stir and start to use an oil bath to raise the temperature until the constant temperature is 100°C. After the reaction raw materials are completely dissolved and become an orange transparent homogeneous system, add phase transfer under nitrogen protection Catalyst ethyl triphenylphosphine bromide methanol solution 0.18g (the weight percent concentration of ethyl triphenylphosphine bromide is 70%), then heat up to 120°C at a rate of 2°C / min, and keep warm at 120°C for reaction After 30 minutes, lower the temperature to 100°C, add 0.26 g of tert-butyl peroxybenzoate and 7.5 g of bisphenol A epoxy resin E-54 (epoxy equivalent of 181 to 187 g / mol), stir and mix evenly, The temperature was lowered to obtain a light yellow sem...

Embodiment 2

[0034] Add 100 g of 4,4'-diallyl bisphenol A and 5 g of 4,4'-diaminodiphenyl sulfone into a 500 mL four-neck flask equipped with mechanical stirring, thermometer, reflux condenser and nitrogen introduction device , stirred and began to use an oil bath to raise the temperature until the constant temperature was 100°C. After the reaction raw materials were completely dissolved, an orange transparent homogeneous system was formed. Under the protection of nitrogen, 100g of 4,4'-bismaleimide diphenylmethane was slowly added to keep Stir to make the reaction system in a clear and homogeneous state, add 0.2 g of phase transfer catalyst benzyltrimethylammonium bromide, then raise the temperature to 130°C at a rate of 3°C / min, keep the reaction at 130°C for 45 minutes, then lower the temperature To 100°C, add 0.27g of tert-butyl peroxybenzoate, 5 g of bisphenol A epoxy resin E-54 (epoxy equivalent of 181-187g / mol), stir and mix evenly, then cool down to obtain a light yellow semi-solid ...

Embodiment 3

[0037] Add 50 g of 4,4'-diallyl bisphenol A and 5 g of 4,4'-diaminodiphenylsulfone into a 250 mL open beaker, stir with a glass rod and heat with an oil bath at 100°C, wait until The reaction raw materials are completely dissolved into an orange transparent homogeneous system, slowly add 50g of 4,4'-bismaleimide diphenylmethane, keep stirring to make the reaction system in a clear and homogeneous state, add the phase transfer catalyst ethyltriphenyl Phosphine bromide methanol solution 0.18g (the weight percent concentration of ethyltriphenylphosphine bromide is 70%), heat and keep it in an oil bath at 130°C for 1 hour, add 0.1g dicumyl peroxide, benzoic acid peroxide 0.1 g tert-butyl ester, stir well, add 2.5 g bisphenol A epoxy resin E-54 (epoxy equivalent: 181-187 g / mol), 0.5 g 3-aminopropyltriethoxysilane, stir well , the temperature was lowered to obtain a light yellow resin product.

[0038] Using the bismaleimide resin prepared above, using Toray T300 6K carbon fiber as...

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Abstract

The invention discloses a modified bismaleimide resin for a microdiameter pultrusion process. The modified bismaleimide resin is prepared from the following raw materials in part by weight: 100 parts of 4,4'-bismaleimide diphenylmethane, 1 to 30 parts of diamido diphenyl sulfone, 10 to 150 parts of dially bisphenol A and 1 to 50 parts of liquid epoxy resin. The bismaleimide resin has high formingprocessibility and a cured substance has high heat resistance. The invention also discloses a preparation method of the modified bismaleimide resin. The bismaleimide resin with viscosity and activitymeeting a composite material pultrusion process is prepared by prepolymerizing the 4,4'-bismaleimide diphenylmethane, the diamido diphenyl sulfone, the dially bisphenol A and the liquid epoxy resin by using a high-temperature type radical initiator. The reaction is stable; the process condition is easy to control; byproduct separation is not required in the reaction process; no 'three wastes' aregenerated; and the method is applicable to industrialized production.

Description

technical field [0001] The invention relates to the field of bismaleimide and its synthesis and preparation, in particular to a bismaleimide resin used in a composite material microdiameter pultrusion molding process and a preparation method thereof. Background technique [0002] Bismaleimide (BMI) is a kind of resin system derived from polyimide resin system, and it is a bifunctional compound with maleimide (MI) as the active terminal group. The temperature of its resin is between that of epoxy resin and polyimide. The bismaleimide resin-based composite material has the characteristics of excellent high temperature resistance, radiation resistance, heat and humidity resistance, and good processability. It is mainly used in the aviation field. Composite components with high temperature and large load. [0003] Bismaleimide resin is usually solid at room temperature, and the curing temperature is high and takes a long time. Unmodified bismaleimide resin has disadvantages suc...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/12
Inventor 任华陈雯娜胡晶晶肖军
Owner NANJING UNIV OF AERONAUTICS & ASTRONAUTICS
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