微波诱导催化合成四乙酰乙二胺的初步研究

在微波辐射下，以乙二胺、乙酸、乙酸酐为原料，用不同催化剂(硫酸、磷酸、氯化铝)，常压合成出了四乙酰乙二胺。对微波功率、辐射时间、催化剂种类进行了正交实验，数据表明最佳反应条件为：n(乙二胺)：n(乙酸)：n(乙酸酐)=l：2．5：4，第一步合成二乙酰乙二胺，微波功率680W、加热8min，用氯化铝为催化剂；第二步合成四乙酰乙二胺，微波功率580W，加热180min，用磷酸为催化剂。优化再现实验表明，DAED、TAED产率分别在96％、56．14％左右。与传统工艺相比，反应时间缩短，产率有所提高，产品色泽较好。

Study on synthesis of tetraacetylenediamine under microwave irradiation

Tetraacetylenediamine was synthesized from ethylenediamine,acetic acid and acetic anhydride with sulphuric acid,phosphoric acid and aluminum chloride as catalysts under microwave irradiation.The effect of radiation time,microwave power and kind of catalyst were discussed.The optimum conditions were molar ratio ethylenediamine/acetic acid/acetic anhydride 1/2.5/4,microwave power 680 W,heating time 8 min with aluminum chloride as catalyst in the first step,and 580 W,180 min with phosphoric acid as catalyst in the second step.