環氧樹脂阻燃劑的合成及表征

化工論文編號:HG040  論文字數:15032,頁數:41

目  錄
摘  要 I
Abstract II
1  緒 論 1
1.1 阻燃問題的提出 1
1.2阻燃技術發展概述 1
1.3磷系阻燃劑概述 2
1.4磷系阻燃劑阻燃機理 3
1.5磷系阻燃劑的研究 4
1.6前人的工作成果 5
1.7本論文的可行性研究 7
1.8本論文研究的主要內容 7
2  DOPO-HB的合成 8
2.1 前言 8
2.2 合成方法 8
2.3 實驗部分 8
2.3.1 實驗試劑 8
2.3.2 實驗儀器 8
2.3.3 實驗步驟 9
2.3.4實驗流程圖 10
2.4 DOPO-HB的表征 10
2.4.1 TGA 10
2.4.2 DSC 11
2.4.3 熔點 12
2.4.4 紅外光譜 12
2.5 小結 13
3  DOPO-HB溶解度的測定 14
3.1概述 14
3.2實驗部分 14
3.2.1.溶解度測定實驗儀器 14
3.2.2實驗步驟 14
3.2.3.實驗裝置 14
3.2.4.實驗結果和數據處理 15
3.2.5 溶解度數據與溫度的關聯 20
3.2.6 小結 25
4  DOPO-ITA的合成 26
4.1 概述 26
4.2 合成原理 26
4.3 實驗部分 26
4.3.1 實驗試劑 26
4.3.2 實驗儀器 26
4.3.3 實驗步驟 27
4.3.4實驗流程圖 27
4.4 DOPO-ITA的表征 28
4.4.1 TGA 28
4.4.2 DSC 28
4.4.3 紅外光譜 29
4.5小結 29
5  結 論 30
5.1 本論文的主要研究成果 30
5.2 存在的不足與研究展望 30
參考文獻 31
致  謝 34

摘  要
 
 DOPO（9，10-2氫-9-氧-10磷雜菲-10-氧化物）和4HBA（4-羥基苯甲醛）通過加成反應合成DOPO-HB(2-6-氧-6-氫-二苯并磷氧雜-6-酮-4-羥基苯甲醇)，同時優化了DOPO-HB的合成條件。DOPO（9，10-2氫-9-氧-10磷雜菲-10-氧化物）和ITA（衣康酸）在甲苯溶劑中反應合成DOPO-ITA({（6-氧-（6H）-二苯并-（CE）（1,2）-氧磷雜己環-6-酮）甲基}-丁二酸)，并通過紅外檢測（FIIR）和熔點檢測法確定所得到的DOPO-HB和DOPO-ITA的化學結構。通過示差掃描熱量計（DSC）和熱重量分析法(TGA)測得這些固化型環氧樹脂的熱力學特征和熱降解行為。本論文還重點研究了DOPO-HB在不同溶劑中的溶解度，結果表明，DOPO-HB在苯，甲苯，二甲苯和水中的溶解度都隨溫度的增加呈上升趨勢，且溶解度的大小順序為：S苯＞S二甲苯＞S甲苯 ＞S水。
 
 關鍵詞：環氧樹脂  固化劑 阻燃劑 溶解度

 Synthesis and Characterization of Epoxy Resin Flame
 Retardant
Abstract
 
 A novel phosphorus-containing hydroxyl benzoaldehyde (DOPO-HB) from 9,10-dihydro-9-oxa-10– phosphaphenanthrene -10-oxide (DOPO) and 4-hydroxyl benzoaldehyde was obtained via simple addition reactions.The synthesis conditions of DOPO-HB were also optimized A novel phosphorous -containing flame retardants 10-(2,5-dicarbonylpropyl) 9,10-dihydro-9-oxa-10-phospha- phenanthrene-10- oxide (DOPO-ITA) was synthesized using 9,10-dihydro-9-oxa-10-phospha-phenanthrene-10-oxide (DOPO) and itaconic acid(ITA) as starting materials.The chemical structure of the obtained DOPO-HB and DOPO-ITA were characterized with FTIR, 1H and 31P NMR and elemental analysis. The DOPO-HB, with multi-phenol groups in the molecular chain, was used as a poly functional curing agent for epoxies. The activity and activation energies of the DOPO-HB curing reactions with epoxies were investigated with differential scanning calorimetry (DSC). The thermal properties and thermal degradation behaviors of the DOPO-HB-cured epoxy resins were also studied with DSC and thermo gravimetric analysis(TGA). The paper also focuses on the solubility of DOPO-HB in different solvents with the temperature trend, the results show that, the solubility of DOPO-HB in benzene, toluene and xylene, and water increases with the temperature rising. Moreover, the benzene> xylene> toluene> Water

 Keywords: Epoxy resin  Curing agent  Flame retardant  solubility