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微波诱导催化合成四乙酰乙二胺的初步研究
Study on synthesis of tetraacetylenediamine under microwave irradiation
【摘要】 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 ) =1∶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 5 80W ,加热 1 80min ,用磷酸为催化剂。优化再现实验表明 ,DAED、TAED产率分别在 96%、5 6.1 4%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
【Abstract】 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.
【Key words】 ethylenediamine; acetic acid; acetic anhydride; microwave; tetraacetylenediamine; synthesis;
- 【文献出处】 石化技术与应用 ,Pebrochemical Technology & Application , 编辑部邮箱 ,2003年04期
- 【分类号】TQ649.65
- 【被引频次】1
- 【下载频次】95