Curable resin composition and cured product thereof
A technology for curing resins and compositions, which can be used in electric solid state devices, semiconductor/solid state device parts, electrical components, etc., can solve problems such as resin deterioration, and achieve the effect of excellent light resistance and coloring.
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Synthetic example 1
[0221] As the first-stage reaction, 114 parts of β-(3,4-epoxycyclohexyl) ethyltrimethoxysilane, 234 parts of silanol-terminated methylphenyl silicone oil ( Silanol equivalent 850, calculated as 1 / 2 of the weight-average molecular weight measured by GPC) and 18 parts of 0.5% potassium hydroxide (KOH) methanol solution (0.09 parts in terms of KOH) were put into the reaction vessel, and the bath The temperature was set to 75°C for heating. After heating up, the reaction was carried out under reflux for 8 hours.
[0222] As the second-stage reaction, 305 parts of methanol was added, and then 86.4 parts of 50% distilled water methanol solution was added dropwise over 60 minutes, and the reaction was carried out at 75° C. under reflux for 8 hours. After the reaction, neutralize with 5% sodium dihydrogen phosphate aqueous solution, and then carry out distillation and recovery of methanol at 80°C. Add 380 parts of methyl isobutyl ketone (MIBK), and repeat the water wash three times....
Synthetic example 2
[0224] As the first-stage reaction, 257 parts of β-(3,4-epoxycyclohexyl) ethyl trimethoxysilane, 505 parts of silanol-terminated methyl phenyl silicone oil ( Silanol equivalent of 850, calculated as 1 / 2 of the weight average molecular weight measured by GPC) and 40 parts of 0.5% potassium hydroxide (KOH) methanol solution (0.2 parts in terms of KOH) were put into the reaction vessel, and the bath The temperature was set to 75°C for heating. After heating up, the reaction was carried out under reflux for 8 hours.
[0225] As the second-stage reaction, 510 parts of methanol was added, and then 130 parts of 50% distilled water methanol solution was added dropwise over 60 minutes, and the reaction was carried out at 75° C. under reflux for 8 hours. After the reaction, neutralize with 5% sodium dihydrogen phosphate aqueous solution, and then carry out distillation and recovery of methanol at 80°C. Add 704 parts of methyl isobutyl ketone (MIBK), and repeat the water wash three tim...
Synthetic example 3
[0227]In a flask equipped with a stirrer, a reflux condenser, and a stirring device, 20 parts of tricyclodecane dimethanol, 100 parts of methylhexahydrophthalic anhydride (manufactured by Shinnihon Chemical Co., Ltd. , リカシツド MH, hereinafter referred to as acid anhydride H-1), reacted at 40°C for 3 hours, and then heated and stirred at 70°C for 1 hour, thus (confirming the disappearance of tricyclodecane dimethanol (less than 1 area %) by GPC) to obtain 120 parts of curing agent composition (T-1) containing polycarboxylic acid (B-1) and acid anhydride (H-1).The gain is a colorless liquid resin, and the purity is measured by GPC, polycarboxylic acid (B-1; The following formula (9)) is 55 area %, and methyl hexahydrophthalic anhydride is 45 area %. In addition, the functional group equivalent is 201 g / eq.
[0228]
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