The conditions for condensation-polymerization of olygomer which was prepared from Bisphenol A and phosgene by the addition of caustic soda have been investigated. The results indicated that the molecular weight of polymer can be adjusted to any desired extent by addition of a small amount of monohydric alcohols or phenols. Also, the rate of formation of polymer was increased by vigorous agitation, raising temperature and increasing concentrations of olygomer and caustic soda. Addition of methanol and catalyst was effective to complete condensationpolymerization reaction, and separation into two layers after the reaction and the removal of salt as the by-product be came easy . Vigorous stirring and increasing the concentration of catalyst resulted in the increase of the molecular weight of the polymer .
In order to make a simultaneous synthesis of α-and γ-picolines, the above reaction was carried out by use of silica-alumina catalyst. The products, besides the above expected compounds, contained a small amount of pyridine with traces of A-picoline and ethylamine. It was also recognized the formation of large amount of big hboiling pyridines, aldehyde condensation products, carbon aceous sudstances and gaseous decomposition products. The reacting conditions were investigated. It was found that the recycling of aldehyde raw material was not favorable, and that the deposition of carbonaceous substance on the catalyst caused rapid decrease in its selectivity to make it necessary to be regenerated frequently. The theoretical yield from aldehyde was 20 mol% of α-picoline, 23 mol % of γ-picoline, 10 mol % of high boiling pyridines at the reacting temperature of 450°c for 7 hr with space velocity 0 .19 g, ald./ml, cat?hr and ammonia 200% excess (against paraldehyde)
In the thermal decomposition of nickel Formate in a mixed solvent of diphenyl ether and diphenyl for manufacturing of nickel catalyst, the relation between the conditions for deconposition and the activity of catalyst has been investigated. The determination of its activity was made by measuring the velocity constant of hydrogenation of dinitrotoluene under pressure. Repeated use of solvent was not only simple for operation but also gave catalyst of high activity than using it after recovering it with distillation. Its higher activity partly depends on effect of phenol formed from hydrogenolysis of Biphenyl ether during the decomposition. The amount of solvent used for catalyst preparation had no relation with its activity above a certain amount. The greater the velocity of raising temperature at the time of decomposition, the higher was the activity of catalyst. As to the method of decomposition, heating of a suspension of nickel formate in the solvent gave stronger activity of catalyst rather than the addition of slurry of nickel formate in the heated solvent. Glass and zinc were found to be suitable for the material of the vessel for decomposition.
Reactive dyes with a general formula, or -SO2 CH3 were synthesized (D=dye component, D-NHSO2 and -CF3 or -SO2CH3 are in o- or p-position to fluorine atom) by condensation of azo, anthraquinone or phtha-locyanine type dyes having amino group capable of acylation with 3 kinds of following sulfonyl chlorides : These dyes can be combined chemically with cotton, nylon, silk, wool, etc., by heating with alkali to make fast dyeing against washing, but the reactivity of fluorine of these dyes was weaker than that of D-NHSO2type dyes and the dyeing ability was poorer. However the light-fastness of dyed product was better than that with the above nitro type dyes.