歧化松香(丙烯酸-2-羥基乙基酯)酯的合成

林明濤1， 儲富祥1*， 馬 麗1，2， 周道兵1，王基夫1， 王春鵬1

（1．中國林業(yè)科學(xué)研究院林產(chǎn)化學(xué)工業(yè)研究所；國家林業(yè)局林產(chǎn)化學(xué)工程重點開放性實驗室，江蘇南京210042； 2．南京林業(yè)大學(xué)化學(xué)工程學(xué)院，江蘇南京210037）

摘 要： 通過對歧化松香（DPR）分別進(jìn)行酰氯化和酯化反應(yīng)成功制備了DPR（丙烯酸-2-羥基乙基酯）酯?？疾炝朔磻?yīng)過程中反應(yīng)溫度、反應(yīng)時間以及原料物質(zhì)的量之比對DPR酰氯化反應(yīng)的影響，確定了DPR酰氯化反應(yīng)的最佳條件（DPR與三氯化磷（PCl3）的物質(zhì)的量比為1∶0.33，反應(yīng)溫度50℃，反應(yīng)時間3h)，并對DPR酰氯的酯化反應(yīng)進(jìn)行了研究。實驗結(jié)果表明：溫度對于DPR酰氯化反應(yīng)的影響較??；而原料物質(zhì)的量之比對反應(yīng)程度的影響較大，PCl3用量的增加有利于反應(yīng)程度的增加。實驗結(jié)果還顯示IR、13C NMR和GC-MS聯(lián)用分析技術(shù)可有效地對反應(yīng)過程進(jìn)行跟蹤。
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關(guān)鍵詞： 歧化松香；丙烯酸-2-羥基乙基酯；酰氯；酯化

中圖分類號：TQ351.471      文獻(xiàn)標(biāo)識碼：A      文章編號：0253-2417(2006)04-0043-05

Study on the Synthesis of Disproportionated Rosin (2­Hydroxyethyl Acrylate) Ester

LIN Ming­tao1, CHU Fu­xiang1, MA Li1,2, ZHOU Dao­bing1, WANG Ji­fu1, WANG Chun­peng1

(1. Institute of Chemical Industry of Forest Products,CAF; Key and Open Lab. on Forest Chemical Engineering,SFA,  Nanjing 210042, China；2.College of Chemical Engineering,Nanjing Forestry University, Nanjing 210037, China)

Abstract: Disproportionated rosin (DPR) (2­hydroxyethyl acrylate) ester was synthesized by acyl chlorination and esterification of DPR acid. The influences of temperature, reaction time and molar ratio of the reaction were studied by monitoring the course of reaction.The optimum conditions of acyl chlorination and esterification were investigated as follows: molar ratio of DPR to PCl3 1∶0.33, reaction temperature  50℃ and reaction time 3 h. It was found that  temperature had no significant effect on acylation of DPR, and the increase of molar ratio of PCl33 had a positive impact on the reaction degree. The results also showed that IR,13C NMR and GC­MS were effective methods for tracking the course of acylation and esterification reaction.
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Key words: disproportionated rosin;2­hydroxyethyl acrylate;acyl chlorination;
esterification