4,6-二氨基-1,3-苯二磺酸水解工艺及其动力学研究

Study on Hydrolysis Process of 4,6-diamino-1,3-benzenedisulfonic Acid and Its Kinetics

以间苯二胺磺化反应得到的4，6-二氨基-1，3-苯二磺酸和2，4-二氨基苯磺酸的混合产物为原料，通过对4，6-二氨基-1，3-苯二磺酸进行水解得到产物2，4-二氨基苯磺酸；并采用Fr—IR和。HNMR等手段对产物进行了表征。利用单因素实验确定了适宜的水解工艺条件：水解时间2．5h，水解温度130℃，滴加水量W（水）：W（间苯二胺）=0．75：1，在此条件下，2，4-二氨基苯磺酸得率为98．16％（间苯二胺为基准）。温度在393—408K，4，6-二氨基-1，3-苯二磺酸水解反应符合1—1级可逆反应模型，且随着温度的升高正、逆反应的水解速率常数都增加；通过拟合不同温度下的正、逆反应的水解速率常数，得4，6-二氨基-1，3-苯二磺酸水解反应正反应活化能为48．83kJ／mol，逆反应活化能为47．62kJ／mol。

The mixed products of 4,6-diamino- 1,3-benzenedisulfonic acid and 2,4-diaminobenzenesulfonic acid as raw material were prepared by m-phenylenediamine sulfonation. 2,4-Diaminobenzenesulfonic acid was obtained through 4,6-diamino-1,3-benzenedisulfonic acid hydrolysis, and the product was characterized by FT-IR and 1H NMR. The favorable conditions of hydrolysis process obtained by single factor experiments were as follows： 2. 5 h as the hydrolysis time, 130 ~C as the hydrolysis temperature, w（water） ： w（m-phenylenediamine） = 0. 75 ： 1 as the amount of dropping water. Under these conditions, the yield of 2,4-diaminobenzenesulfonic acid could reach 98.16% （ m-phenylenediamine as datum）. Temperature at 393 - 408 K, the hydrolysis reaction of 4,6 - diamino - 1,3 - benzenedisulfonic acid corresponded with the model of 1-1 reversible reaction, otherwise the hydrolysis rate constants of positive and reverse reaction had increased as temperature rose. Hydrolysis rate constants of positive and reverse reaction at different temperatures were fitted knew that 4,6 - diamino - 1,3 - benzenedisulfonic acid hydrolysis activation energy of positive reaction was 48.83 kJ/mol, and the hydrolysis activation energy of reverse reaction was 47.62 kJ/mol.