Polyamide acid resin composition, polyimide film using same, and method for producing said polyimide film
A polyamic acid resin, polyamic acid technology, applied in coating, transportation and packaging, thin material processing and other directions, can solve the problems of unavailability and high mechanical properties, and achieve the effect of excellent physical properties and low viscosity
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[0115] Hereinafter, although an Example etc. are given and this invention is demonstrated, this invention is not limited to these examples. In addition, regarding the measurement n number, unless otherwise specified, the measurement was performed with n=1.
[0116] (1) Viscosity measurement
[0117] The obtained varnish was diluted with N-methyl-2-pyrrolidone so that the solid content concentration became 10 mass %, and it measured at 25 degreeC using the viscometer (Toki Sangyo Co., Ltd. make, TVE-22H).
[0118] (2) Determination of weight average molecular weight
[0119] The weight average molecular weight was determined in terms of polystyrene using gel permeation chromatography (Waters 2690, manufactured by Nippon Waters Co., Ltd.). Tosoh TXK-GEL α-2500 and α-4000 manufactured by Tosoh Corporation were used as columns, and N-methyl-2-pyrrolidone was used as a mobile phase.
[0120] (3) Fabrication of polyimide film
[0121] The varnish was filtered under pressure usin...
Synthetic example 1
[0148] Synthesis Example 1: Compound A
[0149] A thermometer and a stirring bar with stirring wings were installed in a 300 mL 4-necked flask. Next, THF100g was injected|thrown-in under dry nitrogen gas flow, and it stirred at room temperature. Next, 10.00 g (49.94 mmol) of DAE and 61.01 mg (499.4 μmol) of DMAP were added and washed in with 10 g of THF. After cooling to 10° C. or lower, a diluted solution obtained by diluting 8.607 g (102.4 mmol) of diketene with 10 g of THF was added dropwise. After completion of the dropwise addition, the temperature was raised to 30° C. and stirred for 1 hour. After cooling, the precipitate was recovered by filtration. After drying, compound A represented by the following chemical formula (A) was obtained. The yield was 12.03 g (65% yield).
[0150]
Synthetic example 2
[0151] Synthesis Example 2: Compound B
[0152] A thermometer and a stirring bar with stirring wings were installed in a 300 mL 4-necked flask. Next, THF100g was injected|thrown-in under dry nitrogen gas flow, and it stirred at room temperature. Next, 10.00 g (92.47 mmol) of p-PDA and 113.0 mg (924.7 μmol) of DMAP were added and washed in with 10 g of THF. After cooling to 10° C. or lower, a diluted solution obtained by diluting 15.94 g (189.6 mmol) of diketene with 10 g of THF was added dropwise. After completion of the dropwise addition, the temperature was raised to 30° C. and stirred for 1 hour. After cooling, the precipitate was recovered by filtration. After recrystallization with ethanol and drying, compound B represented by the following chemical formula (B) was obtained. The yield was 19.99 g (yield 78%).
[0153]
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