本文選題：羥乙基雙環(huán)戊烯基醚甲基丙烯酸酯 + 酯化反應　； 參考：《武漢理工大學》2014年碩士論文

【摘要】：羥乙基雙環(huán)戊烯基醚甲基丙烯酸酯分子具有不飽和雙鍵，廣泛應用于接著劑、丙烯酸涂料、活性稀釋劑等領域。用該單體制備的接著劑具有固化收縮率低、氣味小、揮發(fā)性低、空氣干燥性、耐熱、耐濕、耐化學藥性等特點。鑒于眾多特征，羥乙基雙環(huán)戊烯基醚甲基丙烯酸酯具有很大的國內市場發(fā)展?jié)摿�。對其進行質量標準的研究有助于推進工業(yè)規(guī)�；a，能得到廣泛應用并取得非常好的經濟效益。本課題針對其合成工藝、質量標準研究、穩(wěn)定性試驗分別做出了相關的實驗研究。 一、合成工藝的優(yōu)化本課題采用兩步酯化法，合成過程中分別考察了阻聚劑的用量及其比例、催化劑的確定、帶水劑的確定、最佳反應溫度、最適宜反應時間、最合適的反應配比等條件因素對反應產率及酯化率的影響。經由優(yōu)化之后取得最佳的反應條件，從而最終獲得高純度以及高酯化率的產物。 第一步最佳工藝條件：n (雙環(huán)戊二烯):n (乙二醇)=1.2：1；以對苯二酚和對羥基苯甲醚為混合阻聚劑(對苯二酚質量分數(shù)0.6%、對羥基苯甲醚質量分數(shù)0.2%)；反應溫度為120℃；反應時間為15h。 第二步最佳工藝條件: n (甲基丙烯酸):n (乙二醇基雙環(huán)戊烯基醚)=1.2：1；催化劑對羥基苯磺酸的質量分數(shù)(以以醇酸總質量為基準)3.0%；以正庚烷為混合帶水劑；阻聚劑為對苯二酚的質量分數(shù)0.8%、對羥基苯甲醚質量分數(shù)0.2%)；反應溫度為110℃；反應時間為8h。 二、質量標準的制定本文按照各項指標的國家標準對實驗室自制的羥乙基雙環(huán)戊烯基醚甲基丙烯酸酯進行了質量標準的研究。羥乙基雙環(huán)戊烯基醚甲基丙烯酸酯的性狀指標包括色度、溶解度、相對密度、粘度、折光率、酸度、皂化值、溴值等。鑒別項目分別采用官能團鑒別方法、紫外光譜法以及紅外光譜法。另外還有各項檢查項目包括含水率、高聚合物含量、阻聚劑含量等。本文分別采用氣相色譜法和高效液相色譜法測定羥乙基雙環(huán)戊烯基醚甲基丙烯酸酯的含量，通過方法學驗證最終確定了最適合的測定方法為氣相色譜法，其測定的含量可以達到98.5%以上。 三、穩(wěn)定性考察試驗一批產品在室溫條件下放置6個月，另一批產品進行加速試驗，在溫度55～65℃、相對濕度75%下放置3個月，證明產品的每項考察質量項目，在室溫試驗和加速試驗下都符合要求，在考察期內的自制品和對照品的穩(wěn)定性良好，因此預測本產品的有效期為6個月。
[Abstract]:Hydroxyethyl dicyclopentenyl ether methacrylate has unsaturated double bonds and is widely used in many fields such as adhesives, acrylic coatings, active diluents and so on. The adhesive prepared by this monomer has the characteristics of low curing shrinkage, low smell, low volatility, air dryness, heat resistance, moisture resistance, chemical resistance and so on. In view of many characteristics, hydroxyethyl dicyclopentenyl ether methacrylate has great domestic market potential. The research of quality standard is helpful to promote industrial scale production, and it can be widely used and obtain very good economic benefits. In this paper, the synthesis process, quality standard research and stability test were studied respectively. 1. Optimization of synthetic process. In the course of synthesis, the amount and proportion of polymerization inhibitor, catalyst, water carrying agent, optimum reaction temperature and optimum reaction time were investigated. The most suitable reaction ratio and other factors on the reaction yield and esterification rate. The optimum reaction conditions were obtained after optimization, and the products with high purity and high esterification rate were obtained. In the first step, the optimum reaction conditions were as follows: 1: n (dicyclopentadiene): n (ethylene glycol 1.2: 1); using hydroquinone and p-hydroxyphenylmethyl ether as mixed polymerization inhibitor (hydroquinone mass fraction 0.6, p hydroxy phenyl methyl ether 0.2wt%); reaction temperature 120 鈩，

本文編號：1899538