塔式连续氯化合成1-氯蒽醌的方法研究

Study on the synthesis method of 1-Chloroanthraquinone by consecutive chlorination in the tower

以1-硝基蒽醌为原料,在内置分布器的塔式反应器中,通过氯气直接氯化反应生成1-氯蒽醌。在原料中加入10%的助溶剂和0.2%的复合引发剂;在其作用下使自由基氯代反应在170℃以下稳定地进行,所得粗品含量90%左右。经过磺基转化和重结晶两步提纯可得到含量≥99%的高纯度1-氯蒽醌。

1-nitroanthraquinone as raw materials,in the reaction tower within a distributor,was directly chlorinated by chlorine gas to generated 1-chloroanthraquinone.10% of cosolvent and 0.2%of composite initiator were added to raw materials;so as a free radical chlorinated reaction was stably proceeding under 170 ℃.After that,about 90% crude product of 1-chloroanthraquinone was obtained. 99% of 1-chloroanthraquinone can be obtained after sulfonation reaction and recrystallization.