【摘要】 对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 ,常压合成四乙酰乙二胺进行了初步研究。主要设备为经改造的家用微波炉。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 =1:2 .5 :4 ,第一步合成二乙酰乙二胺 ,微波功率 6 80W、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 5 80W、加热 180min ,用磷酸为催化剂。经优化再现实验 ,DAED、TAED产率分别在 96 %、5 6 .14 %左右。与传统工艺相比反应时间缩短 ,产品色泽气味较好。更多还原

【Abstract】 Tetraacetylethylenediamine was synthesized from ethylenediamine, acetic acid and acetic anhydride with sulphuric acid, phosphoric acid, aluminiumchloride as catalysts under microwave irradiation, using a reconstructed home microwave oven as the main equipment, was studied in this paper. The effect of radiation time, microwave power, kinds of catalysts were discussed in orthogonal experiments. Data illustrated that the optimum reaction conditions were as follows: ethylenediamine: acetic acid :acetic anhydride =1:2.5:4(molar ratio). The microwave power, time and catalyst were 680 w, 8 min, aluminum chloride (in the first step) and 580 w, 180 min, phosphoric acid (in the second step). The yield is 96%, 56.14% . Compared with the traditional heating ways, the microwave irradiation is a rapid method with good color and aroma.更多还原