环氧树脂阻燃剂的合成及表征

论文编号:HG040  论文字数:15032,页数:41

摘  要
 
 DOPO（9，10-2氢-9-氧-10磷杂菲-10-氧化物）和4HBA（4-羟基苯甲醛）通过加成反应合成DOPO-HB(2-6-氧-6-氢-二苯并磷氧杂-6-酮-4-羟基苯甲醇)，同时优化了DOPO-HB的合成条件。DOPO（9，10-2氢-9-氧-10磷杂菲-10-氧化物）和ITA（衣康酸）在甲苯溶剂中反应合成DOPO-ITA({（6-氧-（6H）-二苯并-（CE）（1,2）-氧磷杂己环-6-酮）甲基}-丁二酸)，并通过红外检测（FIIR）和熔点检测法确定所得到的DOPO-HB和DOPO-ITA的化学结构。通过示差扫描热量计（DSC）和热重量分析法(TGA)测得这些固化型环氧树脂的热力学特征和热降解行为。本论文还重点研究了DOPO-HB在不同溶剂中的溶解度，结果表明，DOPO-HB在苯，甲苯，二甲苯和水中的溶解度都随温度的增加呈上升趋势，且溶解度的大小顺序为：S苯＞S二甲苯＞S甲苯 ＞S水。
 
 关键词：环氧树脂  固化剂 阻燃剂 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

目  录
摘  要 I
Abstract II
1  绪 论 1
1.1 阻燃问题的提出 1
1.2阻燃技术发展概述 1
1.3磷系阻燃剂概述 2
1.4磷系阻燃剂阻燃机理 3
1.5磷系阻燃剂的研究 4
1.6前人的工作成果 5
1.7本论文的可行性研究 7
1.8本论文研究的主要内容 7
2  DOPO-HB的合成 8
2.1 前言 8
2.2 合成方法 8
2.3 实验部分 8
2.3.1 实验试剂 8
2.3.2 实验仪器 8
2.3.3 实验步骤 9
2.3.4实验流程图 10
2.4 DOPO-HB的表征 10
2.4.1 TGA 10
2.4.2 DSC 11
2.4.3 熔点 12
2.4.4 红外光谱 12
2.5 小结 13
3  DOPO-HB溶解度的测定 14
3.1概述 14
3.2实验部分 14
3.2.1.溶解度测定实验仪器 14
3.2.2实验步骤 14
3.2.3.实验装置 14
3.2.4.实验结果和数据处理 15
3.2.5 溶解度数据与温度的关联 20
3.2.6 小结 25
4  DOPO-ITA的合成 26
4.1 概述 26
4.2 合成原理 26
4.3 实验部分 26
4.3.1 实验试剂 26
4.3.2 实验仪器 26
4.3.3 实验步骤 27
4.3.4实验流程图 27
4.4 DOPO-ITA的表征 28
4.4.1 TGA 28
4.4.2 DSC 28
4.4.3 红外光谱 29
4.5小结 29
5  结 论 30
5.1 本论文的主要研究成果 30
5.2 存在的不足与研究展望 30
参考文献 31
致  谢 34