Unsaturated cyclic anhydride end capped polyimides and polyamic acids and photosensitive compositions thereof
a polyimide and polyamic acid technology, applied in the field of unsaturated cyclic anhydride end capped polyamic acid and polyimide polymers, can solve the problems of poor photo imaging capability, insolubility of polyimides and/or precursor polyamic acids in commonly used solvents in the electronic industry, and is suitable for many applications. , to achieve the effect of excellent thermomechanical properties, low cure temperature and excellent photo imaging properties
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example 1
6FDA / 6BF / BZXPh-5 / 1A (48.1 / 29.6 / 19.8 / 2.5)
[0249]A mixture of 6BF (15.13 g, 30 mmol), BZXPh-5 (4.5 g, 20 mmol) and IA (0.28 g, 2.5 mmol) were dissolved in NMP (165.1 g) and stirred at ambient temperature under a nitrogen atmosphere. To this solution was then added 6FDA (21.63 g, 48.7 mmol) in small batches while stirring that generated about 5° C. exotherm. The reaction mixture was continued to stir at ambient temperature for 20 hours during which time the solution turned viscous. A small portion of this solution was diluted with DMAc for GPC analysis. GPC-DMAc—Mw=99,600, Mn=47,850, PDI=2.08.
[0250]The polyamic acid solution (127 g containing about 25 g polymer) thus obtained above was mixed with anhydrous pyridine (25 g), acetic anhydride (25 g) and cyclopentanone (100 g) and the solution heated to 90° C. for 4 hours under nitrogen atmosphere while stirring. The reaction mixture was allowed to cool to ambient temperature and added to excess water / methanol (80 / 20) mixture (1.5 L) to iso...
example 2
6FDA / PM DA / 6BF / PFMB / IA (24.1 / 24.1 / 29.6 / / 19.7 / 2.5)
[0251]6BF (15.13 g, 30 mmol) and PFMB (6.41 g, 20 mmol) were dissolved in NMP (150.7 g) and stirred at ambient temperature under a nitrogen atmosphere. A mixture of 6FDA (10.83 g, 24.4 mmol), PMDA (5.317 g, 24.4 mmol) and IA (0.28 g, 2.5 mmol) was added in small batches to the above solution while stirring. The reaction mixture was stirred at ambient temperature for an additional period of 20 hours during which time the solution turned viscous. An additional amount of NMP (33 g) was added to this viscous solution. A small portion of this solution was then diluted with DMAc for GPC analysis. GPC-DMAc—Mw=107,050, Mn=60,700, PDI=1.76. A small sample of the polymer solution was also added to excess water / acetone (80 / 20) mixture to isolate the polymer for 1H NMR analysis. The gummy product was washed with excess water / acetone (80 / 20) mixture and dried in a vacuum oven at 50-60° C. for 24 hours to obtain a solid product. 1H-NMR (500 MHz) sp...
example 3
6F DA / PMDA / HFBAPP / PFMB / IA (24.1 / 24.1 / 26.6 / 19.7 / 2.5)
[0253]HFBAPP (7.78 g, 15 mmol) and PFMB (3.2 g, 10 mmol) were dissolved in NMP (76.2 g) and stirred at ambient temperature under a nitrogen atmosphere. A mixture of 6FDA (5.41 g, 12.2 mmol), PMDA (2.66 g, 12.2 mmol) and IA (0.140 g, 1.25 mmol) was added in small batches to the above solution while stirring. The reaction mixture was stirred at ambient temperature for 20 hours during which time the solution turned viscous. An additional amount of NMP (21 g) was added to the viscous solution. A small portion of this solution was then diluted with DMAc for GPC analysis. GPC-DMAC—Mw=74,650, Mn=38,400, PDI=2.05.
[0254]The polyamic acid solution (100 g containing about 16 g polymer) thus obtained above was mixed with anhydrous pyridine (16 g), acetic anhydride (16 g) and cyclopentanone (75 g) and the solution was heated to 90° C. for 6 hours under nitrogen atmosphere while stirring. The polymer became insoluble as the imidization progressed...
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