本文選題：羥乙基雙環(huán)戊烯基醚甲基丙烯酸酯 + 酯化反應(yīng)　； 參考：《武漢理工大學(xué)》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(yīng)用于接著劑、丙烯酸涂料、活性稀釋劑等領(lǐng)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(xué)藥性等特點(diǎn)。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(nèi)市場發(fā)展?jié)摿�。對其進(jìn)行質(zhì)量標(biāo)準(zhǔn)的研究有助于推進(jìn)工業(yè)規(guī)�；a(chǎn)，能得到廣泛應(yīng)用并取得非常好的經(jīng)濟(jì)效益。本課題針對其合成工藝、質(zhì)量標(biāo)準(zhǔn)研究、穩(wěn)定性試驗(yàn)分別做出了相關(guān)的實(shí)驗(yàn)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(yīng)溫度、最適宜反應(yīng)時(shí)間、最合適的反應(yīng)配比等條件因素對反應(yīng)產(chǎn)率及酯化率的影響。經(jīng)由優(yōu)化之后取得最佳的反應(yīng)條件，從而最終獲得高純度以及高酯化率的產(chǎn)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(zhì)量分?jǐn)?shù)0.6%、對羥基苯甲醚質(zhì)量分?jǐn)?shù)0.2%)；反應(yīng)溫度為120℃；反應(yīng)時(shí)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(zhì)量分?jǐn)?shù)(以以醇酸總質(zhì)量為基準(zhǔn))3.0%；以正庚烷為混合帶水劑；阻聚劑為對苯二酚的質(zhì)量分?jǐn)?shù)0.8%、對羥基苯甲醚質(zhì)量分?jǐn)?shù)0.2%)；反應(yīng)溫度為110℃；反應(yīng)時(shí)間為8h。 二、質(zhì)量標(biāo)準(zhǔn)的制定本文按照各項(xiàng)指標(biāo)的國家標(biāo)準(zhǔn)對實(shí)驗(yàn)室自制的羥乙基雙環(huán)戊烯基醚甲基丙烯酸酯進(jìn)行了質(zhì)量標(biāo)準(zhǔn)的研究。羥乙基雙環(huán)戊烯基醚甲基丙烯酸酯的性狀指標(biāo)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(xiàng)目分別采用官能團(tuán)鑒別方法、紫外光譜法以及紅外光譜法。另外還有各項(xiàng)檢查項(xiàng)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(xué)驗(yàn)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(dá)到98.5%以上。 三、穩(wěn)定性考察試驗(yàn)一批產(chǎn)品在室溫條件下放置6個(gè)月，另一批產(chǎn)品進(jìn)行加速試驗(yàn)，在溫度55～65℃、相對濕度75%下放置3個(gè)月，證明產(chǎn)品的每項(xiàng)考察質(zhì)量項(xiàng)目，在室溫試驗(yàn)和加速試驗(yàn)下都符合要求，在考察期內(nèi)的自制品和對照品的穩(wěn)定性良好，因此預(yù)測本產(chǎn)品的有效期為6個(gè)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(hào)：1899538