Polyimide resin composition
A technology of polyimide resin and composition, applied in the field of polyimide resin composition, can solve the problems of low molding processability, low fluidity, no thermoplasticity, etc., and achieves good productivity, high crystallization temperature, excellent Effects of long-term heat resistance
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[0182] Next, although an Example is given and this invention is demonstrated in more detail, this invention is not limited to this. In addition, various measurement and evaluation in each manufacture example and an Example were performed as follows.
[0183]
[0184] The IR measurement of the polyimide resin was performed using "JIR-WINSPEC50" manufactured by JEOL Ltd.
[0185]
[0186] A polyimide resin obtained by dissolving 0.100 g of the polyimide resin in 20 mL of concentrated sulfuric acid (96%, manufactured by Kanto Chemical Co., Ltd.) after drying the polyimide resin at 190-200°C for 2 hours The solution was used as a measurement sample, and it measured at 30 degreeC using the Cannon-Finks viscometer. The logarithmic viscosity μ was obtained by the following formula.
[0187] μ=ln(ts / t 0 ) / C
[0188] t 0 : flow time of concentrated sulfuric acid
[0189] ts: Flow time of polyimide resin solution
[0190] C: 0.5g / dL
[0191]
[0192] The melting point Tm, ...
manufacture example 1
[0235] [Production example 1] Production of polyimide resin 1
[0236]2-(2-Methoxyethoxy)ethanol (Nippon Emulsifier Co., Ltd. Company make) 500g and pyromellitic dianhydride (Mitsubishi Gas Chemical Co., Ltd. make) 218.12g (1.00mol), after nitrogen purging, it stirred at 150 rpm so that it may become a uniform suspension solution. On the other hand, using a 500 mL beaker, 49.79 g (0.35 mol) of 1,3-bis(aminomethyl)cyclohexane (manufactured by Mitsubishi Gas Chemical Co., Ltd., cis / trans ratio=7 / 3), 1,8-octa 93.77 g (0.65 mol) of methylene diamine (manufactured by Kanto Chemical Co., Ltd.) was dissolved in 250 g of 2-(2-methoxyethoxy)ethanol to prepare a mixed diamine solution. The mixed diamine solution was slowly added using a plunger pump. Although exothermic heat is caused by dropwise addition, it is adjusted so that the internal temperature is within 40 to 80°C. During the dropwise addition of the mixed diamine solution, the nitrogen purging state was set, and the rotati...
Embodiment 1~9、 comparative example 1~2
[0247] Examples 1-9, Comparative Examples 1-2 (production and evaluation of polyimide resin composition)
[0248] The polyimide resin 1 obtained in Production Example 1 and each component shown in Table 2 and Table 3 were fully mixed by dry blending. The obtained mixed powder was extruded using a laboratory kneading extrusion device (Labo Plastomill, manufactured by Toyo Seiki Seisaku-sho, Ltd.) at a cylinder temperature of 350° C. and a screw rotation speed of 70 rpm. The strand extruded from the extruder was air-cooled, and pelletized by a pelletizer ("Fan cutter FC-Mini-4 / N" manufactured by Hoshi Plastic Co., Ltd.). The obtained pellets were dried at 190° C. for 10 hours, and then used for injection molding.
[0249] Injection molding was performed using an injection molding machine (manufactured by FANUC CORPORATION "ROBOSHOT α-S30iA") at a cylinder temperature of 350°C, a mold temperature of 200°C, and a molding cycle of 50 seconds, and moldings of predetermined shapes u...
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