Please wait a minute...
Table of Content
25 October 1951, Volume 2 Issue 3
    化工学报
    THE PREPARATION OF, CHLOROBENZENE
    1951, 2(3):  71-79. 
    Abstract ( 1773 )   PDF (552KB) ( 439 )  
    Related Articles | Metrics
    Although voluminous literature can be found in regard to the production of Chlorobenzene from benzene and chlorine, it is considered necessary to make some further investigations. The major variables studied in the present work are temperature, concentrations of the reactants, kinds of catalysts, and the effect of air admixed in the chlorine gas. It is known from the experimental results that the yield of chlorobenzene decreases while that of dichlorobenzene incroases with inerease in temperature. The temperature between 25?and 30℃ can be considered as most suitable for industrial production as regards the catalysts, anhydrous alumminum chloride and the residue remained after distillation of the reaction mixture are the best. Anhydrous ferric chloride is a little worse than the two just mentioned but slightly better than metallic iron. Any air mixed in the chlorine gas has only very little effect on the chemical reactions. If one desires to obtain as little dichlorobenzene as possible in comparison with the amount of chlorobenzene obtained, it is suggested to use 0.8 mol chlorine per mol of benzene when the temperature is 30℃ and iron is used as catalyst. Under these conditions, the highest ratio of the amount of chloro-benzene to that of dichlorobenzene will obtained.
    A STUDY OF SULFUR BLACK
    C. C. YIN, W. H. YUAN, H. H. ChANG
    1951, 2(3):  80-85. 
    Abstract ( 820 )   PDF (375KB) ( 324 )  
    Related Articles | Metrics
    The demand for sulfur black with a red shade has far Surpassed that for the blue tinted ones. The current opinion seems to recognize that pieric acid is a necessary ingredient in producing the red tint. On aocount of the present shortage of picric acid, which is also an expensive chemical and dangerous to handle, its omission from the manufacturing procedure would solve an acute problem of the sulfur black dye industry. In this investigation, the authors at- tempted and succeeded in obtaining the red shade without using picric acid by a mere variation Of the proportion of the three components, namely dinitro-chl-orobenzene, sodium sulfide and sulfur. The experiment was carried out with similar equipment used by factories of the local district except on a miniature scale. In some factory practice, the preliminary hydrolysis of the dinitro-chlorobenzene is performed in an iron reactor containing all the caustie soda solution with the dinitro-chlorobenzene added subsequently in one portion. When so operated, there is a period of vigorous chemical reaction, which renders temperature control very difficult. To avoid this, the caustic soda soiution was added dropwise to the warm din-itro-chlorobenzene suspension instead, which procedure has already been adopted by some local factories. This is a point worth mentioning, as the authors be-lieve that any careless operation would eventually affect the quality of the dye produced. Two series of experiments were performed. In the first series, the poly-sulfide index was fixed while changing the mole ratio of dinitro-chlorobenzene to sodium polysulfide, and in the other the polysulfide index was varied. The following conclusions were obtained: (1) Fixing the polysulfide index at 3.6 but varying the mole ratio of D.N.C.B. to polysulfide, the effective range of color formation is found to be between l:1.59 and 1:1.72. If the ratio is less than 1:1.59, it fails to give a dye; while on the other hand, when the ratio exceeds 1:1.72, the color intensity may be decreased. Within this range, increasing the ratio increases the rate of thionation without any apparent affect on the color intensity. However, the shade is substantially modified. The red shade is produced only when the ratio is kept ithin an even narrower range of 1:1.63 to 1:1.64. This rather indicates that the control of composition is exceedingly important and should be strictly adhered to. (2) With a fixed ratio of D.N.C.B. to polysulfide at 1:1.58, which showed no tendency of dye-formation at a polysulfide index of 3.6, the index was in- creased up to 3.9. (The highest polysulfide index used in the sulfur black in-dustry is usually 4.0). In all these cases, dyes were obtained with a higher in-tensity accompanying a larger index. The shades, however, are all greenish. When the fixed ratio was increased to 1:1.62 and the polysulfide index gradually lowered from 3.9, the color intensity of each dye produced was less than that of the corresponding one with a smaller D.N.C.B. to polysulfide ratio, although the shade was also an invariable green one. The lower limit, where the dye-forming ability of the composition disappears, is found to be at a polysulfide index of 3.1. It is thus believed that with 3.9 as the upper limit of the poly-sulfide index, the lower limit would progressively shift upward by decreasing the D.N.C.B. to polysulfide ratio, until a point is ultimately reached where the two limits would coincide. This would give a dye of maximum intensity. Further research is required to verify this fact. (3) It is also logical to conclude from the results of this experiment that the intensity and the red shade of sulfur black are antagonistic. It thus neces-sitates a certain degree of compromise in actual factory practice.
    ETHANOL AS A SOLVENT IN THE EXTRACTION OF SOYBEAN OIL
    BY SHU-KAI LIu
    1951, 2(3):  86-92. 
    Abstract ( 1114 )   PDF (419KB) ( 397 )  
    Related Articles | Metrics
    From the standpoint of oil production, solvent extraction is the most efficient method known for processing oil seeds. Ethyl alcohol ia one of the most common organic solvents and has a relatively lower price than others. The oil and meal yield from the alcohol extraction of soybean have considerab-ly better flavor and color than those from extraction with petroleum products or other solvents. On the basis of the data obtained, several important points may be mentioned as follows in connection with the use of ethyl alcohol as a solvent for soybean oil extraction: a. A comparison of the alcohol extraction of the whole sample with that of the ground sample shows that on the average, the rate of extraction of the ground sample is almost twenty times as fast as that of the whole sample. b. The smaller the particle size is, the higher will be the yield of the oil. obtained. If the sample is grounded to pass 40 mesh screen, the highest yield will be obtained. c. Extraction temperature: Soybean oil is insoluble in the alcohol at room temperature. Its solubility increase with increase in temperature. It is better to extract the oil at boiling point of the alcohol solution. d. The concentration of ethyl alcohol: Since soybean oil is insoluble in water, higher concentration of alcohol will give higher yield. As shown by this experiment, poor result will be obtained if the concentration of alcohol is less than 89%.