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Room-temperature-setting high-temperature-resistant liquid modified bismaleimide resin and preparation method thereof

A bismaleimide resin and bismaleimide technology, applied in the field of new materials, can solve the problems of unmodified bismaleimide resin, etc. mild response

Active Publication Date: 2018-12-18
SHAANXI TIANCE NEW MATERIAL TECH
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  • Summary
  • Abstract
  • Description
  • Claims
  • Application Information

AI Technical Summary

Problems solved by technology

At present, there are no reports of such modified bismaleimide resins

Method used

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  • Room-temperature-setting high-temperature-resistant liquid modified bismaleimide resin and preparation method thereof
  • Room-temperature-setting high-temperature-resistant liquid modified bismaleimide resin and preparation method thereof
  • Room-temperature-setting high-temperature-resistant liquid modified bismaleimide resin and preparation method thereof

Examples

Experimental program
Comparison scheme
Effect test

Embodiment 1

[0057] (1) In a 500ml glass bottle equipped with a thermometer, a feeding funnel and a mechanical stirring device, add 150g of 3-allylbenzocyclobutene, raise the temperature to 120℃, and add 150g of 4,4' within 1 hour -Bismaleimide diphenylmethane, and keep the temperature for 1 hour. The temperature was lowered to 80° C. within 30 minutes, and 45 g of dipropargyl etherified bisphenol A was added. After the temperature was kept for 15 minutes, the temperature was reduced to room temperature to obtain the homogeneous and transparent component A.

[0058] (2) Add 60g of divinylbenzene into a 250ml Schlenk bottle with magnetic stirring and connected to nitrogen, increase the temperature to 60°C, add 60g of diallylbisphenol A under stirring, and keep it warm for 20 minutes. Turn on the nitrogen, circulate three times to remove the oxygen, and slowly add 6 g of triphenylphosphine by countercurrent feeding, and add 1.5 g of iron acetylacetonate after it is completely dissolved. After ...

Embodiment 2

[0065] In a 500ml glass bottle equipped with a thermometer, a feeding funnel and a mechanical stirring device, add 60g of 3-allylbenzocyclobutene, heat to 160℃, and add 180g of 4,4'-double horse within 1 hour Leimide diphenyl ether was kept and the reaction was kept for 3 hours. The temperature was lowered to 100°C within 30 minutes, and 84 g of diphenyl acetylene was added. After the temperature was kept for 30 minutes, the temperature was lowered to room temperature to obtain the homogeneous and transparent component A.

[0066] Add 100g of divinylbenzene into a 250ml Schlenk bottle with magnetic stirring and connected with nitrogen, and heat to 40°C. Add 20g of diallylbisphenol A under stirring and keep it warm for 20 minutes. Turn on nitrogen, circulate three times to eliminate oxygen, and slowly add 1.2 g of tris(pentafluorophenyl) phosphine by countercurrent feeding, and add 0.3 g of nickel acetylacetonate after complete dissolution. After 15 minutes of heat preservation, ...

Embodiment 3

[0070] In a 500ml glass bottle equipped with a thermometer, a feeding funnel and a mechanical stirring device, add 60g of 3-allylbenzocyclobutene, heat to 160℃, and add 180g of 4,4'-double horse within 1 hour Leimide diphenyl sulfone, and continue to keep the reaction for 3 hours. The temperature was lowered to 100°C within 30 minutes, and 63 g of diphenyl acetylene and 21 g of dipropargyl etherified bisphenol A were added. After the temperature was kept for 30 minutes, the temperature was reduced to room temperature to obtain the homogeneous and transparent component A.

[0071] Add 80g of divinylbenzene and 20g of styrene into a 250ml Schlenk flask with magnetic stirring and connected with nitrogen. The temperature is raised to 40°C, 40g of diallylbisphenol A is added under stirring, and the temperature is kept for 20 minutes. Turn on nitrogen, circulate three times to remove oxygen, and slowly add 3.5 g of tris(3-fluorophenyl) phosphine by countercurrent feeding, and add 0.6 g...

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Abstract

The invention relates to room-temperature-sizing high-temperature-resistant liquid modified bismaleimide resin and a preparation method thereof. The preparation method comprises the following steps of: firstly heating 3-allylbenzocyclobutene to 120-160 DEG C, and then adding a bismaleimide monomer for fuse-polymerization to prepare a prepolymer; cooling the prepolymer to 80-100 DEG C, then adding an active diluent, and uniformly stirring the mixture and reducing the temperature to obtain a component A; heating an ethylene compound to 40-60 DEG C, adding a system stabilizer and stirring the mixture till the obtained system is uniform and transparent; and in a protective atmosphere, successively adding a phosphine serial catalyst and an acetylacetone metal salt catalyst into the mixed system to perform an insulating reaction, and cooling and ultra-filtering the mixture to obtain a component B, thereby forming the room-temperature-sizing high-temperature-resistant liquid modified bismaleimide resin by the component A and the component B. The initial viscosity of the prepared resin at room temperature is 500cP, the viscosity within 4hr is maintained smaller than 1500cP, and the resin can be used for molding by means of winding or RTM at the room temperature or at slightly high temperature.

Description

【Technical Field】 [0001] The invention belongs to the technical field of new materials, and relates to a room temperature setting high temperature resistant liquid modified bismaleimide resin and a preparation method thereof. 【Background technique】 [0002] Bismaleimide is widely used as the matrix of advanced resin-based composite materials. Its heat resistance is excellent. After curing, the glass transition temperature is generally higher than 250 ℃. This alone is incomparable with epoxy resin. In addition, it has excellent heat and humidity resistance. The dielectric properties are also excellent, and the mechanical properties are excellent. The modified bismaleimide resin can obtain processing technology equivalent to epoxy resin, so it is favored by high-performance composite material process design and researchers. [0003] At present, the commonly used bismaleimide is the commercialized diphenylmethane type bismaleimide, but the bismaleimide monomer must be modified due to ...

Claims

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Application Information

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Patent Type & Authority Patents(China)
IPC IPC(8): C08G73/12
CPCC08G73/12
Inventor 赵宗严艾涛江汛殷武雄易增博
Owner SHAANXI TIANCE NEW MATERIAL TECH
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