Polyimide resin composition
A technology of polyimide resin and composition, which is applied in the field of polyimide resin composition, can solve the problems of low molding processability, low fluidity, and difficulty in molding processing, and achieve excellent long-term heat resistance and blackness high effect
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[0169] 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, an Example, and a comparative example were performed as follows.
[0170]
[0171] The IR measurement of the polyimide resin was performed using "JIR-WINSPEC50" manufactured by JEOL Ltd.
[0172]
[0173] 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.
[0174] μ=ln(ts / t 0 ) / C
[0175] t 0 : flow time of concentrated sulfuric acid
[0176] ts: Flow time of polyimide resin solution
[0177] C: 0.5g / dL
[0178]
[0179...
manufacture example 1
[0236] [Production example 1] Production of polyimide resin 1
[0237] 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 rotat...
Embodiment 1~5、 comparative example 1~3
[0249] The polyimide resin 1 obtained in Production Example 1, and the nanocarbon material (B) shown in Table 2 or other carbon materials were thoroughly mixed at the compounding ratio shown in Table 2 by dry blending. The obtained mixed powder was melt-mixed and extruded using a laboratory mixing and extrusion device (Labo Plastomill, manufactured by Toyo Seiki Seisakusho Co., Ltd.) at a barrel temperature of 350° C. and a screw speed of 70 rpm. After air-cooling the strands extruded through the extruder, they were cut into pellets with a granulator (“Fan cutter FC-Mini-4 / N” manufactured by Hoshi Plastic Co., Ltd.), and pelletized at 190°C , and dried for 10 hours to obtain pellets of the polyimide resin composition.
[0250] In addition, the length of the pellet of a polyimide resin composition is 3-4 mm, and a diameter is 2-3 mm.
[0251] Using the obtained pellets, various evaluations were performed by the aforementioned methods, and the results are shown in Table 2.
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