Epichlorohydrin → Diglycidyl ether

Glycidyl ether of novolak type substituted phenolic resin was produced from the novolak type phenolic resin synthesized in Example 1, using a 1-liter flask equipped with a thermometer, dropping funnel, stirrer, and separating tube with cooler. In the flask were placed 1.0 mol (as phenolic hydroxyl group) of novolak type phenolic resin, 7.0 mols of epichlorohydrin, and 0.4 times (by weight) as much dioxane as epichlorohydrin. Then, 48% NaOH (1.0 mol as NaOH) was added dropwise over 4 hours. During this time, epichlorohydrin, dioxane, and water were azeotropically boiled at 58° to 60° C. under reduced pressure (150 mmHg) and cooled in the separating tube, whereby the organic layer containing major amounts of epichlorohydrin and dioxane were returned to the reaction system whereas the water layer was discharged from the reaction system. After the reaction was completed, epichlorohydrin and dioxane were distilled away, and the reaction product was dissolved in methyl isobutyl ketone. Then the salt formed as a by-product was filtered out, and then methyl isobutyl ketone was distilled away. Thus, there was obtained a glycidyl ether of the novolak type substituted phenolic resin. This product was found to contain 0.029% (290 ppm) of hydrolyzable chlorine and to have an epoxy equivalent of 203, a softening point of 62° C., and a density of 1.19 g/cm3.

1. customequipped with a thermometer
2. customseparating tube with cooler
3. temperaturecooled in the separating tube, whereby the organic layer
4. distillationepichlorohydrin and dioxane were distilled away
5. dissolutionthe reaction product was dissolved in methyl isobutyl ketone
6. customThen the salt formed as a by-product
7. filtrationwas filtered out
8. distillationmethyl isobutyl ketone was distilled away

ORD record

ord-91b78bbfe2fb487a993aa49a0bf34074

Source dataset

uspto-grants-1984_08

DOI

10.6084/m9.figshare.5104873.v1

Patent number

US04468508