Δ22-Stigmasten-3β-ol-5, 6α-oxidewas obtained from stigmasterol by the epoxidation with one equivalent of perbenzoic acid, and 5, 6 α- and 5, 6β-oxide acetate were obtained from stigmasteryl acetate. Melting point (142 143) and specific optical rotation ([α]11.5D -13.5° (dioxane)) of 5, 6-oxide acetate were different from the data of Fernholz. 5, 6α -Oxide was converted to 6β -chloro-Δ22-stigm-asten-3β, 5α-diol-3-monoacetate by hydrochloric acid in chloroform and glacial acetic acid, further it was converted to 22, 23-oxide, and to dichlorohydrine-3-monoacetate. By the epoxidation with excess perbenzoic acid for 5 days, a stigmastan-3β, 5α, 6β -triol-22, 23-oxide was obtained from stigmasterol.
Various kinds of chlorinated stearic acid esters were prepared to test properties with PVC compounds. As a result the PVC compounds showed marked increase in tensile strength, electrical resistivity and improved properties in oil extraction and volatility tests, as the chlorine content increased. On the other hand, increase in chlorine content tended the compounds less flexible and higher in brittle point temperatures. Increase in carbon number of the alcohols bound to the esters improved the properties of PVC compounds such as in flexibility, in lower brittle point temperature and in less volatility on heating, but other properties of the compounds became inferior such as inn their strength, oil extraction and electrical resistivity as well. From the above results, methyl pentachloro stearate was found to be most suitable as the plasticizer for PVC.
The method of preparing high purity granular soybean lecithin from powdered products was investigated. Every conditions that simultaneous extruding and cutting the powdered lecithin by using extruder followed by separating off the chains of granulated lecithins, then shifting them, extracting glyceride by aceton as solvent, removing miscella and desolventizing and drying under vacuum were studied. From the results of both basic and bench scale experiments, we could have a prospect for the industrial development of manufacturing granular soybean lecithin.
As authors mentioned in the previous reports, the pilled copper-chromium-manganese oxide Catalyst had the superior activity and selectivity against those of the nickel catalyst for hydrogenation of nitrobenzene to aniline, crotonaldehyde to butylaldehyde and butanol in the vapor phase, and the selective hydrogenation of acetylene contained in a small amount in the mixture gas of ethylene and hydrogen and of carbon monoxide and hydrogen. An investigation was made to confirm the reproducibility of the hydrogenation of the unsaturated organic compound mentioned above by using the same catalyst on a pilot plant scale, and also to determine the very small amount of by-products coming from hydrogenation of the raw materials which could not decode in the laboratory scale. As a result, it was found that the catalyst has good reproducibility for the hydrogenation of unsaturated organic compounds, especially in the produced ethylene-hydrogen gas mixture the amount of acetylene was 1 ppm or less.
In Japan, the analytical method of the melting point of cocoa butter has not been studied enough, the capillarv-tube method used in Japan was discussed to make reference to the international methods, in this paper. 1) The melting point by capillary-tube method is measured with pre-treatment as follows. The cocoa butter is melted at 5060°C. It is then filtered and transfered to the capillary-tube at the same temperature. The molten fat is solidified at 16-18 for one hour and then transferred to an incubator at 2324°C to set there for one day (24 hours). The stabillized fat is cooled again at 16-18°C for one hour. 2) The diameter of the capillary-tube causes error of the measurement, therefore it is necessary to keep the range of inside diameter at 1.0±0.1 mm.
For the analysis of total active materials (AM) and individual surfactants in the cationics-ampholytics-nonionics ternary mixtures, the determination of total AM in the mixtures by “n-Butanol Liq.-Liq. Extraction” method has been investigated and a new method determining the individual surfactants in the mixtures has been developed. The method consists of four steps as follows : (1) determination of total AM by n-butanol EKieselbach Eliq.-liq. extraction method, (2) direct titration of cationics by “Semimicro BPB-DCE” method, (3) determination of nonionics by “Semimicro Cation-exchange UV Absorption Spectrophotometry”, and (4) ampholytics=total AM-(cationics+nonionics). The results with various ternary mixtures showed that the total AM in the mixtures were extracted quantitatively by n-butanol Eliq.-liq. extraction method, and that the individual surfactants could be accurately determined by our method.
In the previous report, authors reported that higher aliphatic amine salt of inorganic acid reacts with ethylene oxide to produce the quaternary ammonium compound when treated in the presence of water and the reaction has two reaction mechanisms. Higher aliphatic amine salt of organic acid also readily reacts with ethylene oxide. This reaction involves the quaternization by ester produced from organic acid and ethanol used as the solvent, and water is necessary to promote the main reaction. Their properties on surface tension, wettability and antistatic effect were tested. As the result, it was recognized that the quaternary ammonium laurate particularly showed good surface activity in low concentration.
Interactions between sodium dodecyl sulfate (SDS) and polymers including polyvinylpyrrolidone (PVP), polyacrylamide (PAA), polvinylalcohol (88% saponified, PVA), polyvinylacetate (PVAc) were studied by measuring the viscosity and the solubilization of an oil-soluble dye, Orange OT at 40°C. The viscosity of PVP was markedly raised by SDS addition and the solubilizing power of SDS was greatly increased by PVP, but PAA with similar polar group had very little effect both on viscosity and on solubilization; PVA and PVAc showed relatively little solubilization effect in spite of their much increased viscosity due to adsorption-complex formation. In SDS-PVP system, where the molar ratio of the two components was kept constant, the solubilization curve showed a linear relation with concentration above about CMC. This was interpreted by considering an equilibrium between free and adsorbed SDS molecules and assuming the linearity of the solubilizing power of the adsorption-complex with the concentration of the adsorbed SDS. In contrast with the reported Yellow OB solubilization, an internal CMC was observed and the solubilizing power of the complex to Orange OT was not so striking. These results were explained on the basis of the different solubilizing-sites for these dyes.
An investigation was made to determine the effect of structure of surface active agents on their azopigment dispersion power by “Semimicro Azopigment Method”. The dispersing powerr becomes higher with increasing carbon numbers in anionics such as sodium alkyl sulfates, sodium alkyl sulfonates, and disodium salts of α-sulfo fatty acid, and with increasing ethylene oxide moles in nonionics such as POE nonyl phenyl ethers, POE lauryl ethers and POE oleic esters. Thermal stability of azopigment dispersion was most excellent when sodium methyl naphthalene sulfonate formalin condensate was used as a dispersing agent.