Polyimide and heat-resistant materials
A polyimide precursor and heat-resistant technology, applied in the field of polyimide and heat-resistant materials, can solve the problems of unknown materials, lack of heat-resistant substituents, etc., and achieve improved fragility and high vitrification Effect of transition temperature, excellent film toughness
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[0138] Hereinafter, although an Example demonstrates this invention concretely, this invention is not limited to these Examples. In addition, the physical property values in the following examples were measured by the following methods.
[0139]
[0140] The infrared absorption spectrum of the BO group-containing diamine was measured by the KBr plate method using a Fourier transform infrared spectrophotometer (FT-IR5300 manufactured by JASCO Corporation). In addition, infrared absorption spectra of the polyimide precursor film and the polyimide film (about 5 μm thick) were measured by the transmission method.
[0141] 1 H-NMR spectrum>
[0142] Using NMR spectrophotometer (ECP400) manufactured by Nippon Electronics Co., Ltd., the concentration of diamine containing BO group was measured in deuterated dimethyl sulfoxide. 1 H-NMR spectrum.
[0143]
[0144] The melting point and melting curve of the BO group-containing diamine were measured in a nitrogen atmosphere with a...
Synthetic example 1
[0156]
[0157] In a 3-necked flask, p-HAB (manufactured by Wakayama Seika Co., Ltd., 2.61 g, 12 mmol) was dissolved in well-dehydrated N-methyl-2-pyrrolidone (hereinafter referred to as NMP.) (81 mL), Pyridine (2.9 mL, 36 mmol) was added thereto as a deacidifying agent, and it was sealed with a septum cap to prepare a liquid A. Next, in another eggplant-shaped flask, 4-nitrobenzoyl chloride (4.49 g, 24 mmol) was dissolved in NMP (17 mL), and sealed with a septum cap to prepare B solution. Cool liquid A in an ice bath, add liquid B to liquid A in small portions with a syringe while stirring with a rotor, and continue stirring for 3 hours after the addition to synthesize a diamide.
[0158] Next, the ice bath was removed, and after stirring at room temperature for several hours, in order to complete the dehydration and cyclization reaction, an appropriate amount of p-toluenesulfonic acid (1.90 g, 11 mmol) was added to the reaction solution, and an oil bath at 200° C. was used...
Embodiment 1
[0170] Add 5 mmol of BO group-containing diamine represented by the above formula (6) to a well-dried airtight reaction vessel with a stirrer, and dissolve it in NMP dehydrated sufficiently with molecular sieve 4A at about 50° C. After cooling to room temperature, 5 mmol (total solute concentration: 13% by mass) of 2,3,6,7′-naphthalene tetracarboxylic dianhydride (manufactured by JFE Chemical, hereinafter referred to as NTDA) powder was added to this solution. Then, it stirred at room temperature for 72 hours, and obtained the solution (polyimide precursor solution) containing a homogeneous and viscous polyimide precursor.
[0171] In NMP, the intrinsic viscosity of the polyimide precursor measured by the Ostwald viscometer at the concentration of 0.5 mass % at 30 degreeC was 1.15 dL / g.
[0172] The above-mentioned polyimide precursor solution was applied to a glass substrate, and dried at 80° C. for 3 hours in a hot air dryer to prepare a polyimide precursor film.
[0173] ...
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