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    • 10. 发明授权
    • Process for producing 1,5-dinitroanthraquinone and
1,8-dinitroanthraquinone
    • 1,5-二硝基蒽醌和1,8-二硝基蒽醌的制备方法
    • US3963762A
    • 1976-06-15
    • US513907
    • 1974-10-10
    • Walter Hohmann
    • Walter Hohmann
    • C07C205/47C07C20060101C07C67/00C07C201/00C07C49/68
    • Substantially pure 1,5- and/or 1,8-dinitroanthraquinone is recovered from dinitration mixtures which may contain sulfuric acid or a perfluoralkane sulfonic acid by adjusting the nitric acid concentration in the nitration mixture to a value of 91 to 96% for a ratio by weight of nitric acid to solids of from 2.5 : 1 to 10 : 1; separating off the insoluble crude 1,5-dinitroanthranthraquinone at 15.degree. to 50.degree.C; taking up the 1,5-dinitroanthraquinone with 90 to 100% nitric acid in a ratio by weight of nitric acid to solids of from 0.5 : 1 to 3.5 : 1; stirring at 15.degree. to 80.degree. C; separating off the insoluble pure 1,5-dinitroanthraquinone thus obtained; adjusting the mother liquid left following separation of the crude 1,5-dinitroanthraquinone to a nitric acid concentration of from 88 to 94% for a ratio by weight of nitric acid to solids of from 3.0 : 1 to 12 : 1, with the proviso that the nitric acid concentration is at least 1.5% lower than in the preceding separation of crude 1,5-dinitroanthraquinone; and separating off the pure 1,8-dinitroanthraquinone obtained in this way at a temperature in the range of from 20.degree. to 50.degree.C and freeing it from the nitric acid adhering thereto.
    • 通过将硝化混合物中的硝酸浓度调节至91至96%的比例,从可能含有硫酸或全氟烷基磺酸的二硝化混合物回收基本上纯的1,5-和/或1,8-二硝基蒽醌 的硝酸至2.5:1至10:1的固体; 在15〜50℃下分离不溶性粗制1,5-二硝基蒽醌; 以0.5:1至3.5:1的比例将硝酸与固体的重量比为90至100%硝酸1,5-二硝基蒽醌; 在15℃至80℃下搅拌; 分离得到的不溶性纯1,5-二硝基蒽醌; 在将粗制的1,5-二硝基蒽醌分离出硝酸浓度为88至94%,硝酸与固体的重量比为3.0:1至12:1之后留下的母体液体,条件是 硝酸浓度比原来的1,5-二硝基蒽醌分离低至少1.5%; 并将这样获得的纯的1,8-二硝基蒽醌分离出在20℃至50℃的温度范围内,并将其从附着于其上的硝酸释放出来。