High-fluidity wide-processing-widow polyimide pre-polymer and preparation method thereof
A polyimide and processing window technology is applied in the field of thermosetting prepolymer materials and their preparation, which can solve the problems of high melt viscosity and low glass transition temperature, and achieve low melt viscosity and lower glass transition temperature. , the effect of reducing production costs
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Embodiment 1
[0032] Under nitrogen protection, N,N-dimethylacetamide (DMAc, 20g) after vacuum distillation was added in a three-necked round bottom flask with mechanical stirring, and then 3,4'-diaminodiphenyl ether ( 3,4'-ODA, 0.04mol, 8g), after it is completely dissolved, accurately weigh 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride (a-ODPA, 0.02mol, 6.2g) , add DMAc again, control reaction concentration (the sum of diamine and dianhydride is solute) at 30%, reaction temperature adds end-capping agent phenylacetylene phthalic anhydride (PEPA, 0.04mol, 9.92g) after reacting at room temperature for 4 hours, Continue to react for 2 hours, then add triethylamine (0.08mol, 8.08g) and acetic anhydride (0.12mol, 12.24g) dropwise in the polyamic acid solution generated, react at room temperature for 5 hours, and finally the solution obtained Rinse twice with 1000mL of distilled water until the pH value of the filtered water is approximately equal to 7. At the same time, place the obtain...
Embodiment 2
[0034] Under nitrogen protection, N,N-dimethylacetamide (DMAc, 20g) after vacuum distillation was added in a three-necked round bottom flask with mechanical stirring, and then 3,4'-diaminodiphenyl ether ( 3,4'-ODA, 0.04mol, 8g), after it is completely dissolved, accurately weigh 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride (a-ODPA, 0.027mol, 8.27g) , add DMAc again, control reaction concentration (the sum of diamine and dianhydride is solute) at 30%, reaction temperature adds end-capping agent phenylacetylene phthalic anhydride (PEPA, 0.02mol, 6.61g) after reacting at room temperature for 4 hours, Continue to react for 2 hours, then add triethylamine (0.08mol, 8.08g) and acetic anhydride (0.12mol, 12.24g) dropwise in the polyamic acid solution generated, react at room temperature for 5 hours, and finally the solution obtained Rinse twice with 1000mL of distilled water until the pH value of the filtered water is approximately equal to 7. At the same time, place the obta...
Embodiment 3
[0040] Under nitrogen protection, N,N-dimethylacetamide (DMAc, 20g) after vacuum distillation was added in a three-necked round bottom flask with mechanical stirring, and then 3,4'-diaminodiphenyl ether ( 3,4'-ODA, 0.04mol, 8g), after it is completely dissolved, accurately weigh 2,3,3',4'-diphenyl ether tetracarboxylic dianhydride (a-ODPA, 0.032mol, 9.2g) , add DMAc again, control reaction concentration (the sum of diamine and dianhydride is solute) at 30%, reaction temperature adds end-capping agent phenylacetylene phthalic anhydride (PEPA, 0.016mol, 3.968g) after reacting at room temperature for 4 hours, Continue to react for 2 hours, then add triethylamine (0.08mol, 8.08g) and acetic anhydride (0.12mol, 12.24g) dropwise in the polyamic acid solution generated, react at room temperature for 5 hours, and finally the solution obtained Rinse twice with 1000mL of distilled water until the pH value of the filtered water is approximately equal to 7. At the same time, place the obt...
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