Epoxy resin composition, curable composition, and semiconductor-encapsulating material
A technology of epoxy resin and composition, applied in the direction of semiconductor devices, semiconductor/solid-state device parts, electric solid-state devices, etc. Excellent thermal properties and high quality retention
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[0081] Next, the present invention will be specifically described using Examples and Comparative Examples. Hereinafter, "parts" and "%" are based on mass unless otherwise specified. In addition, epoxy equivalent, the melt viscosity in 150 degreeC, GPC, and MS spectrum were measured on the following conditions.
[0082] ◆Determination of epoxy equivalent
[0083] Measurement was performed based on JIS K 7236.
[0084] ◆Measurement method of melt viscosity at 150℃
[0085] Based on ASTM D4287, the measurement was performed with an ICI viscometer.
[0086] ◆Determination of softening point
[0087] Measurement was performed based on JIS K7234.
[0088] ◆Measurement conditions of MS spectrum
[0089] Double focus type mass spectrometer "AX505H (FD505H)" manufactured by JEOL Ltd.
manufacture example 1
[0090] Production Example 1 Production of aralkyl-modified novolak-type resin (a-1)
[0091] 216.3 g of o-cresol and 14.5 g of 41% by mass formalin were put into a flask equipped with a thermometer, a condenser tube, a fractionation tube, a nitrogen introduction tube, and a stirrer, and 4.0 g of oxalic acid was added. The temperature was raised to 100°C, and the reaction was carried out at 100°C for 3 hours. Next, 76.7 g of 41% by mass formalin was added dropwise over 1 hour while trapping water with a fractionating tube. After completion of the dropwise addition, the temperature was raised to 150° C. over 1 hour, and the reaction was further carried out at 150° C. for 2 hours. After completion of the reaction, 600 g of methyl isobutyl ketone was further added, moved to a separating funnel, and washed with water. After washing with water until the washing water became neutral, unreacted o-cresol and methyl isobutyl ketone were distilled off from the organic layer under heati...
Embodiment 1
[0093] The manufacture of embodiment 1 epoxy resin composition (1)
[0094]Into a flask equipped with a thermometer, a dropping funnel, a condenser, and a stirrer, 148.5 g of the aralkyl-modified novolak-type resin (a-1) obtained before and 4,4'-linked 16.5 g of phenol, 463 g of epichlorohydrin, 139 g of n-butanol, and 2 g of tetraethylbenzyl ammonium chloride were dissolved. After heating up to 70° C., 220 g of a 20% aqueous sodium hydroxide solution was added dropwise over 5 hours, and stirring was continued for 0.5 hours under the same temperature conditions. Unreacted epichlorohydrin was distilled off by vacuum distillation, and 1000 g of methyl isobutyl ketone and 350 g of n-butanol were added to dissolve the product. 10 g of 10% sodium hydroxide aqueous solution was added to this solution, and it was made to react at 80 degreeC for 2 hours. After completion of the reaction, washing with 150 g of water was repeated three times, and it was confirmed that the pH of the wa...
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