A kind of high-performance colorless transparent polyimide film and its preparation method
A technology of transparent polyimide and polyimide film, applied in the field of polymer materials, can solve the problem of the deterioration of the color and optical transparency of the high-refractive index PI film, limit the wide application of the high-refractive index PI film, and the refractive index of the PI film. Reduce and other problems, to achieve the effect of low haze value, good industrialization prospects, and excellent comprehensive performance
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Embodiment 1
[0040]Example 1: Synthesis APOT monomer
[0041]10.1 g (0.04 mol) of 2,7-DFT, 9.2 g (0.084 mol) of 3-aminophenol, 14.4 g (0.104 mol) anhydrous carbonated in a 250 mL three-mouth flask equipped with a nitrogen inlet, a moisture, and a thermometer. Potassium, 69 mL N-methylpyridone (NMP) and 37 mL of toluene, the mixture was heated to 135 ° C under stirring, and the water was removed by azeotrophylation. After 16 h, toluene was removed and the resulting solution was stirred at 180 ° C for 4 h. The mixture was then cooled to room temperature and poured into a aqueous aqueous acetic acid under vigorous stirring, and the precipitate was collected, washed with water, and dried under vacuum at 80 ° C. The crude solid was recrystallized twice from the mixture of ethanol / N, N-dimethylformamide solution (8: 2, v / v) to give 8.6 g of a light brown crystal. The structure of the compound is as follows:
[0042]
[0043]The melting point of the compound was 171 ° C.
[0044]Infrared spectroscopyfigure 1 I...
Embodiment 2
[0046]Example 2: Preparation of polyimide films from SBPDA and APOT
[0047]21.5270 g (50 mmol) APOT and 135 g (50 mmol) APOT and 135 g NMP were added to a 500 ml three-bottle equipped with a nitrogen inlet, a stirred bar, and a cold water bath, stirred to dissolved and formed a homogeneous solution; 14.7010 g (50 mmol) SBPDA and remaining were added to the above solution. 10 g NMP, 4h removal of cold water bath, stirred at room temperature for 20 h, resulting in a viscous polyamic acid solution having a solid content of 20 wt%. 47 ml (500 mmol) of acetic anhydride and 32 mL (400 mmol) pyridine were added to the polyamic acid solution, and the reaction was continued at room temperature to obtain a viscous polyimide solution. The polyimide solution was poured into ethanol to give a filamentous resin, and the precipitate was collected and dried in vacuo at 80 ° C for 8 h to obtain a polyimide resin. The above polyimide resin was dissolved in N, N-dimethylacetamide (DMAC), and equipped in...
Embodiment 3
[0055]Example 3: Preparation of polyimide films from ABPDA and APOT
[0056]21.5270 g (50 mmol) APOT and 135 g (50 mmol) Apot and 135 g NMP were added to a 500 ml three-mouth bottle equipped with a nitrogen inlet, a stirred bar, and a cold water bath, stirred to dissolved formation average phase solution; 14.7010 g (50 mmol) ABPDA and remaining were added to the above solution. 10 g NMP, 4h removal of cold water bath, stirred at room temperature for 20 h, resulting in a viscous polyamic acid solution having a solid content of 20 wt%. 47 ml (500 mmol) of acetic anhydride and 32 mL (400 mmol) pyridine were added to the polyamic acid solution, and the reaction was continued at room temperature to obtain a viscous polyimide solution. The polyimide solution was poured into ethanol to give a filamentous resin, and the precipitate was collected and dried in vacuo at 80 ° C for 8 h to obtain a polyimide resin. The above polyimide resin was dissolved in N, N-dimethylacetamide (DMAC), and equipp...
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