Patent ID: 8143450

Claim:
A process for preparing a complex that comprises 1,2,4,5-tetraminobenzene and the aromatic diacid XYTA [which is represented by the structure of the following Formula (I)]: wherein X and Y are each independently selected from the group consisting of H, OH, SH, methyl, ethyl, F, Cl and Br; comprising (a) nitrating 1,3-dihalobenzene, which is represented by the structure of the following Formula (II): wherein each Z is independently Cl or Br, to produce 1,3-dihalo-4,6-dinitrobenzene; (b) heating a suspension of the 1,3-dihalo-4,6-dinitrobenzene, and contacting it with NH 3 to aminate the 1,3-dihalo-4,6-dinitrobenzene and convert it to 1,3-diamino-4,6-dinitrobenzene; (c) forming a slurry of the 1,3-diamino-4,6-dinitrobenzene with water, and contacting the slurry with hydrogen and a hydrogenation catalyst to hydrogenate the 1,3-diamino-4,6-dinitrobenzene and produce 1,2,4,5-tetraminobenzene; (d) contacting the 1,2,4,5-tetraminobenzene produced in (c) with an aqueous solution comprising 1 to 6 equivalents of acid per mol of 1,2,4,5-tetraminobenzene, and, optionally, heating the solution to dissolve the 1,2,4,5-tetraminobenzene; and (e) combining the dissolved 1,2,4,5-tetraminobenzene with (i) 0 to 5 equivalents of an acid; (ii) 0 to 5 equivalents of a base; (iii) optionally, a buffer solution; and (iv) an XYTA source selected from XYTA and M 2 XYTA as represented by the structure of the following Formula (III): wherein M is K or Na, and wherein the molar ratio of XYTA to the 1,2,4,5-tetraminobenzene salt is from 1:1 to 1:1.1; to adjust the pH of the mixture to between about 3 and about 10, and to produce and precipitate a Formula (I) complex.