The
nitration process as one step in 2-amino-5-chloro-4-methylbenzenesulfonic
acid synthesis was improved by optimizing nitration reaction conditions,
improving product separation method to eliminate salty scrap acid
and cycle use of the concentrated sulfuric acid. The effect of various
parameters such as temperature, quality of fuming sulfuric acid, quality
of fuming nitric acid, and reaction time was studied for optimization
of the nitration reaction condition. In the optimum conditions, the
mass ratio of fuming sulfuric acid to sodium 2-chlorotoluene-4-sulfonate
and molar ratio of fuming nitric acid to sodium 2-chlorotoluene-4-sulfonate
were 4 and 1.05, respectively. The reaction temperature was −5
°C, and the time of reaction was 3 h. By applying the optimum
reaction conditions, the yield of nitration reaction was increased
to 91%, larger than that of the current industrial process whose yield
is only 65.7%. The solubilities of sodium 2-chloro-5-nitrotoluene-4-sulfonate
in aqueous sulfuric acid solutions were determined by a dynamic method,
and the results showed that the lowest sodium 2-chloro-5-nitrotoluene-4-sulfonate
solubility was exhibited in 0.7 mass fraction aqueous sulfuric acid
solutions. So the product sodium 2-chloro-5-nitrotoluene-4-sulfonate
of nitration reaction was separated by filtration from 0.7 mass fraction
aqueous sulfuric acid solutions, and the obtained concentrated aqueous
sulfuric acid solution was reused.