| abstract |
1493538 Glycide ethers INVENTA AG 28 April 1975 [24 May 1974] 17472/75 Heading C2C Glycine ethers are prepared by (stage 1) so heating a mixture comprising a phenol, an epihalohydrin, an aqueous alkali metal hydroxide solution (e.g. 5-70% NaOH) and an at least partially water-miscible reaction aid which is a substantially inert organic solvent (e.g. nbutanol) as to cause etherification and partial dehydrohalogenation, less than one mol. of alkali metal hydroxide being employed per equivalent of phenolic hydroxide groups, separating from the reaction mixture the salt solution formed, distilling off excess epihalohydrin and the reaction aid from the reaction mixture, and (stage 2) treating the remaining reaction product with an alkali metal hydroxide solution in excess with respect to the molar amount of halogen present in the remaining reaction product, thereby removing saponifiable halogen and forming an alkali metal halide solution, and separating off the alkali metal halide solution. The epihalohydrin exemplified is epichlorohydrin, and the phenols are 2,2-bis-(4-hydroxyphenyl)-propane from which is obtained the bisglycidyl ether and p-cresol. The alkali used in the first stage may be added in portions, while an inert solvent, e.g. a mixture of xylenes or toluene with n-butanol, may be present in the second stage; residual water may be removed from the final product by azeotropic distillation. The product is preferably neutralized before separating glycide ether from it, e.g. by distillation. A reaction temperature of 40‹-90‹ C. may be used for both stages. |