凝胶色谱与紫外分析桐油甲酯D-A反应的研究

doi:10.16085/j.issn.1000-6613.2017.01.005

化工进展 ›› 2017, Vol. 36 ›› Issue (01): 40-46.DOI: 10.16085/j.issn.1000-6613.2017.01.005

凝胶色谱与紫外分析桐油甲酯D-A反应的研究

李科¹, 蒋剑春^1,2, 聂小安^1,2, 陈洁¹, 黄金瑞¹, 陈水根¹

1 中国林业科学研究院林产化学工业研究所;生物质化学利用国家工程实验室;国家林业局林产化学工程重点开放性实验室;江苏省生物质能源与材料重点实验室, 江苏南京 210042;
2 中国林业科学研究院林业新技术研究所, 北京 100091

收稿日期:2016-05-27 修回日期:2016-07-26 出版日期:2017-01-05 发布日期:2017-01-05
通讯作者: 李科(1985-),男,博士研究生,助理研究员,主要从事生物质资源利用及精细化学品开发研究。E-mail:liketaiping@163.com。
作者简介:李科(1985-),男,博士研究生,助理研究员,主要从事生物质资源利用及精细化学品开发研究。E-mail:liketaiping@163.com。
基金资助:
中央级公益性科研院所基本科研业务费专项（CAFYBB2014MA011）及江苏省生物质绿色燃料与化学品重点实验室项目（JSBGFU14007）。

Study on conversion rate of methyl ester D-A reaction by gel chromatography and UV analysis

LI Ke¹, JIANG Jianchun^1,2, NIE Xiao'an^1,2, CHEN Jie¹, HUANG Jinrui¹, CHEN Shuigen¹

1 Institute of Chemical Industry of Forestry Products, CAF;National Engineering Laboratory for Biomass Chemical Utilization;Key and Open Laboratory on Forest Chemical Engineering, SFA, Nanjing 210042, Jiangsu, China;
2 Institute of New Technology of Forest, CAF, Beijing 100091, China

Received:2016-05-27 Revised:2016-07-26 Online:2017-01-05 Published:2017-01-05

摘要/Abstract

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C22-三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%。

关键词: D-A反应, 凝胶色谱, 紫外, 桐油, 增塑剂

Abstract: Tung oil with conjugated fatty acids and diisooctyl maleate were employed as raw materials to study the synthetic process of C₂₂-tricarboxylic diisooctyl-monomethyl ester and conversion rate calculation of D-A reaction of methyl eleostearate and diisooctyl maleate. Three test methods were used including analysis of yield,gel chromatography,and ultraviolet. The test results showed that all three methods can be used to evaluate the progress of D-A reaction. However,the yield measurement was least accurate. The gel chromatography was the most precise to calculate conversion rate. The UV method could calculate the 270nm absorption reaction progress but the calculation results was too high. The UV method was able to use the band absorption characteristics to judge the reaction type effectively. Combining the analytical results from the gel chromatography and UV concluded that the optimum technological conditions were:the molar ratio of tung oil methyl ester to diisooctyl maleate is 1:1,the reaction temperature is 220℃,reaction time is 5h,and the conversion of tung oil methyl ester can be up to 97.4%.

Key words: D-A reaction, gel chromatography, UV, tung oil, plasticize

中图分类号:

TQ645.1
O657

李科, 蒋剑春, 聂小安, 陈洁, 黄金瑞, 陈水根. 凝胶色谱与紫外分析桐油甲酯D-A反应的研究[J]. 化工进展, 2017, 36(01): 40-46.

LI Ke, JIANG Jianchun, NIE Xiao'an, CHEN Jie, HUANG Jinrui, CHEN Shuigen. Study on conversion rate of methyl ester D-A reaction by gel chromatography and UV analysis[J]. Chemical Industry and Engineering Progree, 2017, 36(01): 40-46.

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凝胶色谱与紫外分析桐油甲酯D-A反应的研究

Study on conversion rate of methyl ester D-A reaction by gel chromatography and UV analysis

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