Tetraacetylenediamine was synthesized using diacetylenediamine (DAED) with the untreated or pretreated acetic acid anhydride. The effect of reaction temperature, time and the molar ratio of acetic acid anhydride and DAED on the absorbency of product were investigated. The results showed that reaction temperature and time had obvious effect on the generation of black by-product, but the effect of materials ratio was little. Under the condition of temperature 130 °C, 6:1 of molar ratio of acetic acid anhydride and DAED, over 360 min of reaction time, the absorbency of product synthesized by pretreated acetic acid anhydride, which was pretreated by sulfur trioxide, was less than one fifth of the un-pretreated. Pretreating acetic acid anhydride was a good method to evidently depress the black by-product.%分别采用预处理前后的醋酸酐与二乙酰乙二胺(DAED)反应制备四乙酰乙二胺.研究了反应温度、反应时间、n(醋酸酐)∶n(DAED)等工艺条件对产物吸光度的影响.结果表明:反应温度和反应时间对黑色副产物的产生影响较大,n(醋酸酐)∶n(DAED)的影响较小.在反应温度130 ℃,n(醋酸酐)∶n(DAED)=6∶1,反应时间360 min以上的条件下,醋酸酐经预处理(以三氧化硫为处理剂)后合成产物的吸光度不到未预处理时的1/5,醋酸酐预处理对降低黑色副产物具有显著的效果.
展开▼
