High strength MoS2-polyimide-cyanate ester composite heat insulation material and production method thereof
A technology of polyimide and heat insulating material, applied in the field of polyimide-cyanate ester composite materials, can solve the problems of high brittleness, poor mechanical properties such as impact strength and tensile strength, poor mechanical properties, low toughness, etc. , to reduce brittleness, improve practicability and durability, and reduce wear and tear
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[0031] The silane coupling agent is KH-564, the main component is 3-[(2,3)-glycidoxy]propylmethyldimethoxysilane, the curing agent is NP-360 amide-based curing agent, and the dispersing agent is Vinylbisstearamide, a high-strength MoS 2 -Polyimide-cyanate ester composite thermal insulation material, the preparation method comprises the following steps:
[0032] Add 10-16 parts of tertiary butylated polyimide, 3-7 parts of molybdenum disulfide, 0.5-2 parts of silane coupling agent and 1-3 parts of dispersing agent to the 1000mL beaker in turn, stir evenly and place the beaker in the In the ultrasonic processor, heat to 90-95℃, the ultrasonic frequency is 28KHz, and ultrasonically disperse for 2-3h, then add 70-85 parts of bisphenol A dicyanate and 0.5-2 parts of curing agent to ultrasonically disperse for 1-2h , pour the evenly dispersed material into the mold, put it in a heating box and heat it to 200-220 ℃ for 3-5 hours. After curing, cool the material to room temperature. ...
Embodiment 1
[0034] (1) Preparation of tert-butylated polyimide: add a 1000mL three-necked flask to a reflux device, and feed an inert gas N into the reaction device by a negative pressure method 2 Remove the air, add 600 mL of anhydrous ethyl acetate into the three-necked flask, then take by weighing 65 parts of 3,5-di-tert-butylaniline and 30 parts of concentrated hydrochloric acid whose concentration is 10 mol / L, and stir at a constant speed for 20 min. , then slowly add 5 parts of paraformaldehyde, place the three-necked flask in a constant temperature water bath and heat it to 50°C, stir magnetically for 3h, add the reflux reaction for 6h when the temperature is raised to 80°C, and cool to room temperature after the reaction is completed. Slowly add ammonia water with a mass fraction of 26% to the necked flask until a large amount of white precipitates are formed, transfer the solution in the three-necked flask into a 2000mL separatory funnel, add an appropriate amount of distilled wat...
Embodiment 2
[0040] (1) Preparation of tert-butylated polyimide: add a 1000mL three-necked flask to a reflux device, and feed an inert gas N into the reaction device by a negative pressure method 2 Remove the air, add 600 mL of anhydrous ethyl acetate into the three-necked flask, then take by weighing 61 parts of 3,5-di-tert-butylaniline and 33 parts of concentrated hydrochloric acid whose concentration is 10 mol / L, and stir at a constant speed for 20 min. , then slowly add 6 parts of paraformaldehyde, place the three-necked flask in a constant temperature water bath and heat it to 55°C, stir magnetically for 4h, add the reflux reaction for 6h when the temperature is raised to 85°C, and cool to room temperature after the reaction is completed. Slowly add ammonia water with a mass fraction of 28% to the necked flask until a large amount of white precipitates are formed, transfer the solution in the three-necked flask into a 2000mL separatory funnel, add an appropriate amount of distilled wat...
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