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Solubilities, Separation and Purification of DSD Acid Intermediate Series

Author: ChenYing
Tutor: ZhangGuoLiang
School: Tianjin University
Course: Biomedical Engineering
Keywords: DSD DSD acid intermediate series DNS ANSD solubility
CLC: TQ460.1
Type: Master's thesis
Year: 2010
Downloads: 76
Quote: 0
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Abstract


4,4’-Diaminostilbene-2,2’-disulfonic acid (DSD Acid)is an important dye inter- mediate. The preparation of DSD Acid includes three steps namely,sulfonation of p-nitrotoluene (PNT) to p-nitrotoluene-o-sulfonic acid (NTS),oxidation of PNTSA to 4,4’-dinitrostilbene-2,2’-disulfonic acid (DNS), and reduction of DNS to DSD with iron powder. 4-Amino-4’-nitrostilbene-2,2’-disulfonic acid (ANSD) is another inter- mediate that can be further reduced to DSD, and is thus usually regarded as a minor byproduct of DSD,ANSD is also widely used in the dye industry. The three subst- ances (DNS, ANSD and DSD) are known as DSD acid intermediate series in this paper.In the oxidation process, some DNS dissolve in the oxidation wastewater, which make a decrease in the yield of DSD; in the reduction section, the compeletly recycling of DSD acid in the solution has gone unfulfilled; and in the pre- paration of ANSD, small amount of DNS and ANSD exist in the target product because of the unmanageable reactive conditins. Therefore, the separation and purificaitin of DSD acid intermediate series are of great significance. The separation can be achieved in a number of methods, the gravity separation is the simplest, and the study of the solubilities of the three subtances is necessarily to precipitation separation, which are the research directions of this paper.This work measured the aqueous sollubility data of DSD acid intermediate series by equilibrium method and the author also inspected the effect of a change in pH (in the range of 0.5-7),temperature (from 293 to 323 K) and iornic strength (from 0 to 0.5 mol/L) on the solubility of the three subtances. The thus aims were to find the isoelectric point of the solutes by S-pH data, fit the solubility data of the solutes at different temperature and iornic strength by Apelblat and Cohn Empirical equations. And the ultimate objective was the selection of the optimal condition for the gravity separation and purification.According to the results of the measurement, Apelblat and Cohn Empirical equations can successfully described the solubility of this system. At the same time we found most of DNS precipitated from the saturation by adding potassium chloride; the recycling of DSD was perfect when pH value equaled 2.5; and the solubility of ANSD slightly incresed(while the other two solutes decreased) by adding ammonium sulfate which is useful for the purification of ANSD. Therefore, we made use of the conditions above to separate and purificate DSD acid intermediate series by the analysis of high performance liquid chramatography. The result showed that the precipitation method is suitable for the separation and purification of DSD acid interm- ediate series.

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