Epoxy resin composition, method for producing the same, and cured product thereof
A technology of epoxy resin and composition, which is applied in the field of epoxy resin composition, can solve the problems of no hygroscopicity, etc., and achieve the effects of low hygroscopicity, high glass transition temperature, and good handling
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[0114]The following examples will be given to describe the present invention in detail. In addition, this invention is not limited to these Examples. In addition, the evaluation method of the resin composition obtained by this invention is shown below.
[0115] (1) epoxy equivalent
[0116] Measurement was performed according to the method of JIS K-7236.
[0117] (2) 150° C. melt viscosity: The melt viscosity of the epoxy resin composition at 150° C. was measured using an ICI melt viscometer.
[0118] The measuring method of ICI viscosity is as follows.
[0119] ICI Cone and Plate Viscometer Model CV-1S TOA Industry Co., Ltd.
[0120] The plate temperature of the ICI viscometer was set at 150° C., and a predetermined amount of sample was weighed.
[0121] The weighed resin composition was placed on the plate, pressurized with a cone from above, and left to stand for 90 seconds. Rotate the cone and read its torque value as the ICI viscosity.
[0122] (3) Gel Time (Gel Ti...
Synthetic example 1
[0152] Add 564 g (6.00 moles) of phenol and 4,4'-bis(methoxymethyl)biphenyl (hereinafter abbreviated as 4.4'-BMMB) to a glass reactor equipped with a stirring device, a condenser, and a nitrogen gas introduction pipe. 202.60 g (0.84 mol), 40.0 g (0.56 mol) of 42% formalin aqueous solution, and 0.28 g of 50% sulfuric acid aqueous solution were reacted at 100° C. for 3 hours.
[0153] Then, it was made to react for 2 hours, keeping reaction temperature at 125 degreeC, and it heated up to 165 degreeC after that, and performed reaction for 3 hours. During this time, generated methanol was distilled off. After completion of the reaction, the resulting reaction solution was cooled and washed with water three times. The oil layer was separated, and unreacted phenol was removed by distillation under reduced pressure to obtain 330 g of a phenolic resin composition.
[0154] The ICI viscosity of the obtained phenolic resin composition was 39 mPa·s, and the OH equivalent measured by th...
Synthetic example 2
[0156] Add 470 g (5.00 moles) of phenol, 233.44 g (0.96 moles) of 4,4'-BMMB, 45.71 g (0.64 moles) of 42% formalin aqueous solution in a glass reaction kettle equipped with a stirring device, a condenser and a nitrogen inlet pipe ), 0.26 g of 50% sulfuric acid aqueous solution, and reacted at 100° C. for 3 hours.
[0157] Then, it was made to react for 2 hours, keeping reaction temperature at 125 degreeC, and it heated up to 165 degreeC after that, and performed reaction for 3 hours. During this time, generated methanol was distilled off. After completion of the reaction, the resulting reaction solution was cooled and washed with water three times. The oil layer was separated, and unreacted phenol was removed by vacuum distillation to obtain 360 g of a phenolic resin composition.
[0158] The ICI viscosity of the obtained phenolic resin composition was 70 mPa·s, and the OH equivalent measured by the acetylation method was 164 g / eq.
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