| 引用本文： |
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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. [点击复制]
- CHANG Yanhong,ZHAO Zhiju,HAN Haiwei,QIN Liumei,LI Guanghua,DUAN Wengui.Separation and Purification of Dehydroabietic Ethyl Acrylate by Dissolving-precipitating Method[J].Guangxi Sciences,2016,23(1):47-50. [点击复制]
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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1H-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。 |
| 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 |
| DOI：10.13656/j.cnki.gxkx.20160315.002 |
| 投稿时间：2015-12-03修订日期：2015-12-21 |
| 基金项目:国家自然科学基金项目(21064001)和广西自然科学基金项目(2014GXNSFAA118042)资助。 |
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| 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, DUAN Wengui
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| (Guangxi Key Laboratory of Petrochemical Resource Processing & Process Intensification Technology, School of Chemistry and Chemical Engineering, Guangxi University, Nanning, Guangxi, 530004, China) |
| 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. |
| Key words: DAEA column chromatography dissolving-precipitating purification |
