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对于制造硫化蓝染料的中间体,磷-甲基靛苯胺Ⅰ的合成过程,研究了应用光度计的控制方法.经确定试样以多量82%硫酸稀释后,反应实际上立刻停止进行,而Ⅰ在82%的硫酸中又非常稳定.随后测定了Ⅰ在82%硫酸溶液中对波长574和428毫微米的克分子消光系数分别为2.44×10~4和2.27×10~3(公升-克分子~(-1)-厘米~(-1)),而对亚硝基苯酚的则分别为0和5.40×10~3;并证明可以利用光度计法来分析两者在混合溶液中的各别含量.应用本法测定的反应速率常数与文献上发表过的数字相符,因此肯定在控制Ⅰ的合成过程上就用光度计法的可靠性.试用本法观察实际生产情况的结果,发现靛苯胺在反应混合物中的存在量往往随着反应时间而上升至一个最高值,接着再下降.由此推测,采用本法来控制生产是具有实际意义的.
For the production of sulfur blue dye intermediates, phosphorus-methyl indoaniline Ⅰ synthesis process, the application of photometric control method was determined after the sample was diluted with a large amount of 82% sulfuric acid, the reaction actually stopped immediately, and Ⅰ Was very stable in 82% sulfuric acid.It was then determined that the molar extinction coefficients of Ⅰ for 574 and 428 nm in wavelength of 82% sulfuric acid solutions were 2.44 × 10 ~ 4 and 2.27 × 10 ~ 3, respectively ~ -1 -1 cm -1), while that of p-nitrosophenol was 0 and 5.40 × 10 -3, respectively. It was also demonstrated that the photometric method can be used to analyze the difference between the two in the mixed solution Content. The reaction rate constant determined by this method is consistent with the number published in the literature, so it is certain that the photometric method will be used in the control of the synthesis of I. The results of the actual production were tested by this method. It was found that indoaniline The amount present in the reaction mixture tends to rise to a maximum with the reaction time and then drops again, suggesting that it is of practical interest to control production with this method.