4,6-二氨基间苯二酚二磷酸盐的合成及其催化剂的研究

Synthesis of 4,6-diaminoresorcinol diphosphate salt and preparation of its catalyst

以2-氯-4,6-二硝基间苯二酚为原料,Pd/C为催化剂,在磷酸水溶液体系中加氢,使生成的4,6-二氨基间苯二酚(DAR)直接成盐,经过一系列的分离提纯得到4,6-二氨基间苯二酚二磷酸盐(DAR.2H3PO4)。通过FT-IR、元素分析、高效液相色谱等分析,确定产品为DAR.2H3PO4,最高收率为98.21%,HPLC纯度为97.25%。且发现用3%H2O2处理后的活性炭制得的催化剂活性和稳定性最好,可媲美同类商业化催化剂,使用后可洗涤再生,循环10以上催化活性未见降低。

A new method to prepare 4,6-diaminoresorcinol（DAR） from 2-chlorine-4,6-dinitroresorcinol in the sys- tem of phosphoric acid solution was studied, where a salt was synthesized directly, and 4,6-diaminoresorcinol diphosphate salt（DAR · 2Ha PO4 ） was obtained after some isolation and purification steps. The product was determined by FT-IR spec- trometry, elemental analysis, HPLC. The yield of the reaction was 98. 21 ~, and the purity was 97.25 %. The activated car- bon was pretreated by different solvents, whose impregnation and reduction were happened in liquid systerm By using differ- ent catalysts in the reaction aforesaid,the catalyst using an activated carbon pretreated by 3% H2O2 （aq） showed the best activity and stability, which didn＇t lose in comparing with congeneric commercial catalyst. Furthermore, the catalyst can be recycled for over ten times by a washing process without weaken in catalytic properties.