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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。
Using 2-chloro-4,6-dinitroresorcin as raw material and Pd / C as catalyst, hydrogenation was carried out in a phosphoric acid aqueous solution to directly generate 4,6-diamino resorcinol (DAR) Salt formation, after a series of separation and purification to give 4,6-diamino resorcinol diphosphate (DAR.2H3PO4). The product was identified as DAR.2H3PO4 by FT-IR, elemental analysis and HPLC. The highest yield was 98.21% and the HPLC purity was 97.25%. It was found that the catalyst prepared with activated carbon treated with 3% H2O2 had the best activity and stability comparable to commercial catalysts of the same type. It was scrubbed and regenerated after use, and the catalytic activity was not reduced more than 10 cycles.