凝胶色谱与紫外分析桐油甲酯D-A反应的研究
发布时间:2018-04-10 17:16
本文选题:D-A反应 + 凝胶色谱 ; 参考:《化工进展》2017年01期
【摘要】:选用具有高共轭脂肪酸含量的桐油与马来酸二异辛酯作为二烯体与亲二烯体,研究了合成C_22-三元酸一甲二辛酯增塑剂的工艺并探讨了酮油甲酯与马来酸二异辛酯D-A反应转化率的计算问题。通过对比分析得率、凝胶色谱、紫外3种测试方法,结果表明得率、凝胶色谱、紫外都可作为检测手段评估D-A反应的进行程度。其中得率误差较大,凝胶色谱计算转化率较为准确,紫外可利用270nm处的吸收判断反应程度,可是计算结果偏大,但可利用各波段吸收特征有效判断反应类型;综合分析凝胶色谱与紫外的结果得出桐油甲酯与马来酸二异辛酯的D-A反应最佳合成条件为桐油甲酯与马来酸二异辛酯在摩尔比为1∶1时,在220℃下反应5h,转化率为97.4%。
[Abstract]:Tung oil and diisooctyl maleate with high conjugated fatty acid content were selected as dienes and dienophiles.The synthesis process of C22- trimethylidene dioctyl ester plasticizer and the calculation of the conversion of methyl ketone oil with diisooctyl maleate D-A were studied.The results showed that yield, gel chromatography and UV could be used as detection methods to evaluate the degree of D-A reaction.Among them, the error of yield is large, the conversion rate calculated by gel chromatography is more accurate, the degree of reaction can be judged by UV absorption at 270nm, but the calculation result is on the high side, but it can be used to judge the reaction type effectively by using the absorption characteristics of each band.The synthetic conditions of D-A reaction of tung oil methyl ester with diisooctyl maleate were obtained by comprehensive analysis of gel chromatography and UV. The optimum conditions were as follows: when the molar ratio of tung oil methyl ester and diisooctyl maleate was 1:1, at 220 鈩,
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