Preparation method of low-chlorine 1, 6-dihydroxy naphthalene type epoxy resin
A technology of dihydroxynaphthalene and epoxy resin, which is applied in the direction of semiconductor devices, circuits, electrical components, etc., and can solve problems such as failure to meet the use requirements in the field of semiconductor packaging, corrosion of metal parts, etc.
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[0032] A first aspect of the present invention provides a preparation method of 1,6-dihydroxynaphthalene type epoxy resin, and the preparation method comprises the following steps:
[0033] 1) Mix and dissolve 1,6-dihydroxynaphthalene and epichlorohydrin under an inert gas atmosphere; then add an alkaline aqueous solution to carry out the reaction, and carry out filtration and vacuum distillation after the reaction to provide a crude product.
[0034] 2) dissolving the crude product provided in step 1) in an organic solvent, after filtration, at a certain temperature, add an alkaline aqueous solution to the filtrate to react with a cosolvent, and the reaction is washed with water and then distilled under reduced pressure to provide 1,6 - Dihydroxynaphthalene type epoxy resin; the hydrolyzable chlorine content of the 1,6-dihydroxynaphthalene type epoxy resin is less than 100 ppm.
[0035] In the preparation method of 1,6-dihydroxynaphthalene type epoxy resin provided by the pre...
Embodiment 1
[0062] To the four-necked flask equipped with a stirrer, a thermometer, a nitrogen inlet tube, a dropping funnel, and a condenser, add 2026 g of epichlorohydrin, 350 g of 1,6-dihydroxynaphthalene, and under nitrogen protection, turn on and stir until all the solids are Dissolve, stir and heat to 50°C, start to drop 437.5g of 40wt% sodium hydroxide aqueous solution, and maintain the reaction for 4 hours. After the reaction is completed, after the temperature of the system drops to room temperature, the insoluble matter is removed by filtration, and the obtained filtrate is removed by distillation under reduced pressure. Dissolved (distillation temperature 75°C, vacuum degree -0.080MPa) to obtain 564 g of crude product.
[0063] To the crude product, add 1692 g of methyl isobutyl ketone solvent to fully dissolve it, remove insoluble inorganic salts by filtration, transfer the remaining filtrate to another four-necked flask, set the reaction temperature to 90 ° C, and then add 35...
Embodiment 2
[0066] To the four-necked flask equipped with a stirrer, a thermometer, a nitrogen inlet tube, a dropping funnel, and a condenser, add 2776 g of epichlorohydrin, 400 g of 1,6-dihydroxynaphthalene, and under nitrogen protection, turn on and stir until the solids are all Dissolve, stir and heat to 50°C, start to drop 525 g of 40wt% sodium hydroxide aqueous solution, and maintain the reaction for 4 hours. After the reaction is completed, after the temperature of the system drops to room temperature, the insoluble matter is removed by filtration, and the obtained filtrate is desolubilized by distillation under reduced pressure. (temperature 75°C, vacuum degree -0.080MPa) to obtain 646.03 g of a crude product.
[0067] To the crude product, add 2584g of methyl isobutyl ketone solvent to fully dissolve it, filter to remove insoluble inorganic salts, transfer the remaining filtrate to another four-necked flask, set the reaction temperature to be 80°C, and then add 40wt 437.5g of % so...
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