High heat-resistant transparent soluble biphenyl polyimide film and its preparation method and application
A soluble biphenyl type polyimide, biphenyl type polyimide technology, applied in the field of polyimide film, can solve the problems of heat resistance, solubility and light transmittance cannot be taken into account, and achieve excellent Heat resistance, increased rotational barrier, good solubility effects
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Embodiment 1
[0036] Under nitrogen protection, add 0.6629g 3,3′,5,5′-tetramethyl-4,4′-diaminophenyl-4″-pyridinemethane (PyDPM), 0.5884g3,3′ , 4,4'-biphenyltetracarboxylic dianhydride (BPDA), 7.51g m-cresol and 0.13g isoquinoline, then seal the tube, and stir magnetically at room temperature for 60 minutes to obtain a clear solution; move the reaction tube to Biotage Initiator + In the microwave synthesizer, use a microwave with a frequency of 2.45GHz, set the power to 400W, first irradiate and react at 70°C for 30 minutes, and then irradiate and react at 200°C for 30 minutes to obtain a light yellow viscous polyimide solution;
[0037]The polyimide solution was added dropwise to 177.8 g of ethanol, and a fibrous precipitate was precipitated, which was left to filter; the precipitate was vacuum-dried at 90° C. for 10 hours to obtain a fibrous polyimide;
[0038] Take partially dried fibrous polyimide and dissolve it in N,N-dimethylacetamide to control the solid content to 10%. After fully ...
Embodiment 2
[0044] Under nitrogen protection, add 0.6629g 3,3′,5,5′-tetramethyl-4,4′-diaminophenyl-4″-pyridinemethane (PyDPM), 0.6061g3,3′ , 4,4'-biphenyltetracarboxylic dianhydride (BPDA), 11.42g N-methylpyrrolidone and 0.08g triethylamine, then seal the tube, and stir magnetically at room temperature for 40 minutes to obtain a clear solution; To Biotage Initiator + In the microwave synthesizer, use a microwave with a frequency of 2.45GHz, set the power to 300W, first irradiate the reaction at 50°C for 15 minutes, and then irradiate it at 210°C for 20 minutes to obtain a light yellow viscous polyimide solution;
[0045] The polyimide solution was added dropwise to 383.1 g of ethanol, and a fibrous precipitate was precipitated, which was left to filter; the precipitate was vacuum-dried at 90° C. for 9 hours to obtain a fibrous polyimide;
[0046] Take partially dried fibrous polyimide and dissolve it in N,N-dimethylacetamide to control the solid content to 12%. After fully stirring and d...
Embodiment 3
[0049] Under nitrogen protection, add 0.6629g 3,3′,5,5′-tetramethyl-4,4′-diaminophenyl-4″-pyridinemethane (PyDPM), 0.6355g3,3′ , 4,4'-biphenyltetracarboxylic dianhydride (BPDA), 5.19gN,N-dimethylformamide and 0.06g pyridine, then seal the tube, and stir magnetically at room temperature for 50 minutes to obtain a clear solution; Tube moved to Biotage Initiator + In the microwave synthesizer, use a microwave with a frequency of 2.45 GHz, set the power to 200 W, first irradiate at 90°C for 20 minutes, and then 190°C for 15 minutes to obtain a light yellow viscous polyimide solution.
[0050] The polyimide solution was added dropwise to 131.1 g of ethanol, and a fibrous precipitate was precipitated, which was left to filter; the precipitate was vacuum-dried at 100° C. for 10 hours to obtain a fibrous polyimide;
[0051] Take partially dried fibrous polyimide and dissolve it in N,N-dimethylacetamide to control the solid content to 15%. After fully stirring and dissolving, apply it...
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