CIESC Journal

• 化工学报 • 上一篇    下一篇

硫化青之研究

尹敬执,袁万熊,张含骧   

  1. 山东大学化学系 ,山东大学化学系 ,山东大学化学系
  • 出版日期:1951-10-25 发布日期:1951-10-25

A STUDY OF SULFUR BLACK

C. C. YIN, W. H. YUAN, H. H. ChANG   

  • Online:1951-10-25 Published:1951-10-25

摘要: <正> 张,柯二氏会系统的研究硫化青深度与原料比例之关系,但对于染料光头,未多加考虑.目前染厂所最喜购者为红光硫化青,故一般厂家,皆加用苦味酸以制造红光成品.查该项药品,不但成本较昂,且在制造时,极易发生危险.由于上海大中染料厂之爆炸,停止使用苦味酸之建议,应为各厂家所采纳.本实验之目的为不用苦味酸或其他代替品,试制红光硫化青.实验结果,经青岛市建新化工厂大规模试验,认为可以使用,如此则不但减低成本,免除不必要之危险,且可符合染厂之需要.特将结果发表,望染化界加以指正.

Abstract: 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.