Epoxy resin composition and cured product thereof
A technology of epoxy resin and composition, which is applied in the direction of epoxy resin glue, synthetic resin layered products, adhesive types, etc., can solve the problems of increased molecular weight, inappropriateness, and reduced operability, and achieve high heat resistance , low dielectric effect
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[0068] Hereinafter, the present invention will be further specifically described based on examples and comparative examples, but the present invention is not limited thereto. In the examples, unless otherwise specified, "parts" means parts by mass, and "%" means % by mass.
[0069] (1) Determination of epoxy equivalent
[0070] Measurement was performed in accordance with JIS K 7236 standard. Specifically, a potentiometric titration device was used, methyl ethyl ketone was used as a solvent, a tetraethylammonium bromide acetic acid solution was added, and a 0.1 mol / L perchloric acid-acetic acid solution was used.
[0071] (2) Determination of phosphorus content
[0072] Sulfuric acid, hydrochloric acid, and perchloric acid are added to the sample, and heated to carry out wet ashing, so that all the phosphorus atoms become orthophosphoric acid. React metavanadate and molybdate in sulfuric acid acidic solution, measure the absorbance of the generated vanadium phosphomolybdate...
Synthetic example 1
[0089] Synthesis Example 1 (Synthesis of Phenol Compound (B1))
[0090] 806 parts of methanol and 201.7 parts of potassium hydroxide were put into a 4-mouth separable glass flask equipped with a stirring device, a thermometer, a cooling pipe, and a nitrogen gas introduction device, and stirred, and 550 parts of dihydroxy compound (a) were added thereto. Bis(4-hydroxy-3,5-dimethylphenyl) sulfone (hereinafter referred to as TMBPS) to make alkali metal salt. After that, 4.5 parts of 4,4'-bischloromethylbiphenyl (hereinafter referred to as BCMB) as a halomethyl-containing compound (b) and 488 parts of bis(2-methoxyethyl) as a solvent were charged. Ether, heated to 75°C while stirring, and reacted for 2 hours.
[0091] After the reaction was completed, the generated salt was removed by filtration, and the temperature was raised to 100°C under a reduced pressure of 50 mmHg. After distilling off the entire amount of methanol and bis(2-methoxyethyl) ether, 1,290 parts of toluene was ...
Synthetic example 2
[0092] Synthesis Example 2 (Synthesis of Phenol Compound (B2))
[0093] 367 parts of methanol and 91.7 parts of potassium hydroxide were put into a 4-mouth separable glass flask equipped with a stirring device, a thermometer, a cooling pipe, and a nitrogen gas introduction device, and stirred, and 250 parts of dihydroxy compound (a) were put into it. TMBPS, prepared as an alkali metal salt. Thereafter, 61.5 parts of BCMB as a halomethyl-containing compound (b) and 360 parts of bis(2-methoxyethyl)ether as a solvent were charged, heated to 75°C while stirring, and reacted for 2 hours.
[0094] After the reaction was completed, the generated salt was removed by filtration, and the temperature was raised to 100°C under a reduced pressure of 50 mmHg. After distilling off the entire amount of methanol and bis(2-methoxyethyl) ether, 685 parts of toluene was added and dissolved. . After neutralizing and liquid-separating with phosphoric acid, washing and liquid-separating with water...
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