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8415616 
Journal Article 
Synthesis of 1, 2, 4, 5-tetraaminobenzene and its hydrochloride 
Jin, N; Liu, W; Jin, T; Chen, H; He, B 
2012 
63 
2092-2099 
Chinese 
Based on the current worldwide trend of using 1, 2, 4, 5-tetraaminobenzene (TAB)and its hydrochloride (TAB·4HCl) in new materials and absence of relevant study in China, a new method of synthesizing polymer grade monomer TAB·4HCl was studied, systematic analysis and optimization was made for the synthesis process, and the relationship of the ammonolysis selectivity with pressure and temperature were clarified. The results showed that 4, 6-dinitro-1, 3-phenylenediamine (DADNB) was prepared by double ammonolysis reaction at 1.0 MPa pressure in 1, 4-dioxane solvent from 1, 3-dichloro-4, 6-dinitrobenzene (DCDNB) ammonia as ammonolysis agent, and then hydrogenated in methanol solvent, the solution containing TAB was obtained after the hydrogenation liquid was decolored with active carbon, then TAB·4HCl was obtained by adding hydrochloric acid and concentrating under reduced pressure and filtering, with 99.3% purity and 79.7% total yield. Finally, with synthesis reliability of 99% and good practical value, a plan for solvent recovery and recycling was proposed for commercialization of TAB·4HCl production. © 2012 All Rights Reserved. 
1, 2, 4, 5-tetraaminobenzene tetrahydrochloride; 1, 3-dichloro-4, 6-dinitrobenzene; 4, 6-dinitro-1, 3-phenylenediamine; Ammonolysis selectivity