| 溶解-沉淀法分离纯化去氢枞酸丙烯酸乙二醇酯 |
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| 引用本文： | 常艳红,赵治巨,韩海威,覃柳妹,李光华,段文贵.溶解-沉淀法分离纯化去氢枞酸丙烯酸乙二醇酯[J].广西科学,2016,23(1):47-50. |
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| 作者姓名： | 常艳红 赵治巨 韩海威 覃柳妹 李光华 段文贵 |
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| 作者单位： | 广西大学化学化工学院,广西石化资源加工及过程强化技术重点实验室,广西南宁530004 |
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| 基金项目： | 国家自然科学基金项目(21064001)，广西自然科学基金项目(2014GXNSFAA118042) |
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| 摘 要： | 【目的】考察溶解-沉淀法分离纯化去氢枞酸丙烯酸乙二醇酯(DAEA)的可行性。【方法】从歧化松香中提取去氢枞酸(dehydroabietic acid,DHAA),经酰氯化、与丙烯酸(2-羟基)乙酯(HEA)反应得到DAEA粗产物,再分别通过硅胶柱层析法和溶解-沉淀法进行分离纯化,并利用1 H-NMR、熔点仪、GC-MS和元素分析法对所得产物进行表征和测试。【结果】硅胶柱层析法和溶解-沉淀法得到的DAEA的纯度分别为97.19%和98.73%,收率分别为48.37%和46.18%。【结论】与硅胶柱层析法比较,溶解-沉淀法减少洗脱剂的使用量,缩短处理时间,为松香乙烯基单体的分离纯化提供一个更简便的方法。
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| 关 键 词： | 去氢枞酸丙烯酸乙二醇酯 溶解-沉淀法 柱层析法 纯化 |
| 收稿时间： | 2015/12/3 0:00:00 |
| 修稿时间： | 2015/12/21 0:00:00 |
Separation and Purification of Dehydroabietic Ethyl Acrylate by Dissolving-precipitating Method |
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| CHANG Yanhong,ZHAO Zhiju,HAN Haiwei,QIN Liumei,LI Guanghua and DUAN Wengui.Separation and Purification of Dehydroabietic Ethyl Acrylate by Dissolving-precipitating Method[J].Guangxi Sciences,2016,23(1):47-50. |
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| Authors: | CHANG Yanhong ZHAO Zhiju HAN Haiwei QIN Liumei LI Guanghua and DUAN Wengui |
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| Institution: | Guangxi Key Laboratory of Petrochemical Resource Processing & Process Intensification Technology, School of Chemistry and Chemical Engineering, Guangxi University, Nanning, Guangxi, 530004, China,Guangxi Key Laboratory of Petrochemical Resource Processing & Process Intensification Technology, School of Chemistry and Chemical Engineering, Guangxi University, Nanning, Guangxi, 530004, China,Guangxi Key Laboratory of Petrochemical Resource Processing & Process Intensification Technology, School of Chemistry and Chemical Engineering, Guangxi University, Nanning, Guangxi, 530004, China,Guangxi Key Laboratory of Petrochemical Resource Processing & Process Intensification Technology, School of Chemistry and Chemical Engineering, Guangxi University, Nanning, Guangxi, 530004, China,Guangxi Key Laboratory of Petrochemical Resource Processing & Process Intensification Technology, School of Chemistry and Chemical Engineering, Guangxi University, Nanning, Guangxi, 530004, China and Guangxi Key Laboratory of Petrochemical Resource Processing & Process Intensification Technology, School of Chemistry and Chemical Engineering, Guangxi University, Nanning, Guangxi, 530004, China |
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| Abstract: | Objective] The feasibility of dissolving-precipitating method was examined in the purification of dehydroabietic ethyl acrylate (DAEA).Methods] DAEA crude product was obtained by the reaction of 2-hydroxyethyl acrylate (HEA)and dehydroabietic acid chloride starting from dehydroabietic acid (DHAA), which extracted from disproportionated rosin.The obtained crude product was purified by silica gel column chromatography and dissolving-precipitating method, respectively, and then DAEA product was characterized and examined by 1H-NMR, melting point instrument, GC-MS and element analysis.Results] The purity of DAEA was 97.19% and 98.73%, and the yield was 48.37% and 46.18%, by means of silica gel column chromatography and dissolving-precipitating method, respectively.Conclusion] Comparedwith silica gel column chromatography, dissolving-precipitating method reduced the amount of eluent, and shortened the processing time, and therefore it provided a more convenient method for the separation and purification of rosin vinyl monomers. |
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| Keywords: | DAEA column chromatography dissolving-precipitating purification |
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