The reaction factors for the formation of bisphenol A and B, or the raw materials for polycarbonate resin, have been investigated. Bisphenol A was prepared with Hasen No, 70 and 91% yield of the theory by reaction of 3 moles of phenol, 1 mole of acetone, 0-0.02 mole of mercaptoacetic acid, and 0.36 mole of hydrogen chloride gas for 8 hours, and washing with hot water, distillation in vacuum and recrystallization. Similarly, bisphenol B with Hasen No. 100 was prepared with 76% yield of the theory.
The refining methods and purities of bisphenol A, methylene chloride and phosgene as the raw materials for polycarbonate have been investigated in relation to condensation-polymerization reaction. For obtaining the colorless, transparent high polymer easy for washing after the completion of the reaction with good yield, the following procedures are necessary:1) Bisphenol A should be recrystallized from solvent, such as xylene, to white and, highly pure form.2) Methylene chloride should not contain large amount of molecular weight modifier such as methanol.3) Highly pure phosgene must be used with the lesat amount of chlorine and hydrochloric acid.
In the formation of a monomer and a olygomer by the reaction of bisphenol A andphosgene, the effects of the rate of passing of phosgene, the concentration of caustic soda, the amount of phosgene and catalyst have been investigated. When a part of bisphenol A remained unreacted after the completion of introduction of phosgene, it was recognized that molecular weight of polymer obtained in the condensation polymerization reaction increased but its yield and the reproducibility of the reaction decreasd. Also, an increase in the rate of passing of phosgene retarded the next condensation-polymerization reaction and made the molecular weight distribution range narrow. By the addition of catalyst in the phosgenation period or a stepwise addition of sodium hydroxide during the introduction of phosgene, the consumption of phosgene and sodium hydroxide can be decreased to a considerable extent.
Several kinds of reactive dyes having chloromethylbenzenesulfonyl group or chloromethylbenzoyl group were synthesized, by the reaction of water-soluble dye containing amino group with p-chloromethylbenzenesulfonly chloride or p- or ο-chloromethylbenzoyl chloride. These dyes give fast-dyed products when heated with cellulose fibers in the presence of alkali by the formation of ether-like linkage between the dye and the fiber. The fixing strength of dyes to the fiber were in order of p-chloromethylben-zenesulfonyl >p-chloromethylbenzoyl> ο-chloromethlbenzoyl.