羟乙基双环戊烯基醚甲基丙烯酸酯的合成及质量标准研究

发布时间：2018-05-17 02:34

  本文选题：羟乙基双环戊烯基醚甲基丙烯酸酯 + 酯化反应　； 参考：《武汉理工大学》2014年硕士论文

【摘要】：羟乙基双环戊烯基醚甲基丙烯酸酯分子具有不饱和双键，广泛应用于接着剂、丙烯酸涂料、活性稀释剂等领域。用该单体制备的接着剂具有固化收缩率低、气味小、挥发性低、空气干燥性、耐热、耐湿、耐化学药性等特点。鉴于众多特征，羟乙基双环戊烯基醚甲基丙烯酸酯具有很大的国内市场发展潜力。对其进行质量标准的研究有助于推进工业规模化生产，能得到广泛应用并取得非常好的经济效益。本课题针对其合成工艺、质量标准研究、稳定性试验分别做出了相关的实验研究。 一、合成工艺的优化本课题采用两步酯化法，合成过程中分别考察了阻聚剂的用量及其比例、催化剂的确定、带水剂的确定、最佳反应温度、最适宜反应时间、最合适的反应配比等条件因素对反应产率及酯化率的影响。经由优化之后取得最佳的反应条件，从而最终获得高纯度以及高酯化率的产物。 第一步最佳工艺条件：n (双环戊二烯):n (乙二醇)=1.2：1；以对苯二酚和对羟基苯甲醚为混合阻聚剂(对苯二酚质量分数0.6%、对羟基苯甲醚质量分数0.2%)；反应温度为120℃；反应时间为15h。 第二步最佳工艺条件: n (甲基丙烯酸):n (乙二醇基双环戊烯基醚)=1.2：1；催化剂对羟基苯磺酸的质量分数(以以醇酸总质量为基准)3.0%；以正庚烷为混合带水剂；阻聚剂为对苯二酚的质量分数0.8%、对羟基苯甲醚质量分数0.2%)；反应温度为110℃；反应时间为8h。 二、质量标准的制定本文按照各项指标的国家标准对实验室自制的羟乙基双环戊烯基醚甲基丙烯酸酯进行了质量标准的研究。羟乙基双环戊烯基醚甲基丙烯酸酯的性状指标包括色度、溶解度、相对密度、粘度、折光率、酸度、皂化值、溴值等。鉴别项目分别采用官能团鉴别方法、紫外光谱法以及红外光谱法。另外还有各项检查项目包括含水率、高聚合物含量、阻聚剂含量等。本文分别采用气相色谱法和高效液相色谱法测定羟乙基双环戊烯基醚甲基丙烯酸酯的含量，通过方法学验证最终确定了最适合的测定方法为气相色谱法，其测定的含量可以达到98.5%以上。 三、稳定性考察试验一批产品在室温条件下放置6个月，另一批产品进行加速试验，在温度55～65℃、相对湿度75%下放置3个月，证明产品的每项考察质量项目，在室温试验和加速试验下都符合要求，在考察期内的自制品和对照品的稳定性良好，因此预测本产品的有效期为6个月。
[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，

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