论文总字数：24108字

摘 要

环氧树脂（EP）由于具有优异的粘接、机械、电绝缘性能等而广泛应用于各个领域。然而EP高度易燃，提高了火灾危害的可能性，这极大地限制了它在高阻燃要求领域的使用。为了避免卤系阻燃剂对人体健康及环境带来的负面影响，设计开发无卤阻燃剂成为业界研究者关注的焦点。

本文研究一种以9，10-二氢-9-氧杂-10-磷杂菲-10-氧化物（DOPO）为主要分子结构，在其中引入硼元素，设计一种新型高磷硼含量阻燃剂的合成方案。方案采用DOPO，甲醛，硼酸为反应物进行加成和酯化反应合成高磷硼含量阻燃剂（ODOPM-B），拟定合成配方摩尔比为DOPO：甲醛：硼酸=1.2：1.2：1。拟采用傅里叶红外光谱和核磁共振氢谱来表征其分子结构。按照提前拟定的配方将阻燃剂与双酚A型环氧树脂（E-51）加热共混后加入化学计量4，4二氨基二苯砜（DDS）固化得到阻燃环氧树脂，拟定固化制度：160℃/2h，180℃/4h。拟采用差示扫描量热分析（DSC）、动态热机械分析（DMA）、极限氧指数（LOI）等测试技术对阻燃环氧树脂固化行为，热性能和阻燃性进行测试。

最后，通过理论分析，并结合前人已经成功开展的研究工作来探究本设计方案的可行性。

关键词：DOPO；高效阻燃剂；环氧树脂；硼酸

Abstract

Epoxy resin (EP) is widely used in various fields due to its excellent adhesion, mechanical and electrical insulation properties.However, EP is highly flammable and increases the likelihood of fire hazards, which greatly limits its use in areas requiring high flame retardancy.In order to avoid the negative effects of halogenated flame retardants on human health and the environment, the design and development of halogen-free flame retardants have become the focus of the industry.

In this paper, a new type of high phosphorous boron flame retardant was designed by introducing boron into 9, 10-dihydro-9-oxyhetero-10-phosphorous hetero-10-oxide (DOPO) as the main molecular structure.DOPO, formaldehyde and boric acid were used as reactants for addition and esterification reaction to synthesize flame retardant with high phosphorus boron content (ODOPM-B). The molar ratio of the prepared formula was DOPO: formaldehyde: boric acid = 1.2:1.2:1.The molecular structure is characterized by FTIR and H NMR.The flame retardant and bisphenol A type epoxy resin (E-51) were heated and blended according to the formula prepared in advance, and then stoichiometrics (4,4 diaminodiphenyl sulfoxide (DDS) was added to solidification to obtain the flame retardant epoxy resin. The proposed curing system was: 160℃/2h, 180℃/4h.Different scanning calorimetry (DSC), dynamic thermomechanical analysis (DMA), limited oxygen index (LOI) and other testing techniques are proposed to test the curing behavior, thermal performance and flame retardation of flame-retardant epoxy resin.

Finally, through theoretical analysis and combining with previous successful research work to explore the feasibility of the design scheme.

Key Words：DOPO；Flame retardant；Epoxy resin；Boric acid

目 录

第1章 绪论.................................................................................................................................1

1.1阻燃剂的起源与发展.....................................................................................................1

1.2聚合物的燃烧过程.........................................................................................................1

1.3阻燃机理.........................................................................................................................2

1.3.1气相阻燃机理.....................................................................................................2

1.3.2凝聚相阻燃机理.................................................................................................3

1.3.3中断热交换机理.................................................................................................3

1.4阻燃剂种类.....................................................................................................................3

1.5环氧树脂阻燃的必要性.................................................................................................6

1.6常用的环氧树脂阻燃剂.................................................................................................7

1.7 DOPO衍生物阻燃剂的研究进展.................................................................................8

1.8本论文研究目的及意义.................................................................................................9

1.9本论文研究内容.............................................................................................................9

第2章 方案设计.........................................................................................................................11

2.1引言.................................................................................................................................11

2.2实验原料.........................................................................................................................11

2.3实验仪器.........................................................................................................................12

2.4阻燃剂ODOPM-B的合成方案设计.............................................................................12

2.5阻燃环氧树脂的制备方案设计.....................................................................................14

2.6本章小结.........................................................................................................................16

第3章 可行性分析.....................................................................................................................18

3.1前言.................................................................................................................................18

3.2合成原理分析.................................................................................................................18

3.3前人研究分析.................................................................................................................19

第4章 总结.................................................................................................................................20

参考文献.......................................................................................................................................21

致谢...............................................................................................................................................23

第1章 绪论

1.1阻燃剂的起源与发展

火自古时候诞生以来便给人类社会带来了许多便利，但与此同时，也给人们带来了很多火灾问题。人们从古时候便一直与火灾进行对抗，阻燃技术便在人类历史上开始出现。最早的阻燃技术起源于公元前450年古希腊人Herodotus用硫酸铝钾溶液浸泡木材，赋予木材一定的阻燃能力。往后很长时间，人们不停在阻燃技术领域进行创新，开始使用不同的阻燃剂，应用在不同的领域，阻燃技术开始了长久的发展。

到了19世纪，随着社会的发展，越来越多用于阻燃的无机物被发现，应用在木材，棉织物等^[1]领域甚至于在军事领域也有所应用。随着石油化工提炼技术的出现，人工合成高分子出现在人们生活的领域。它们以自身优异的物理和化学性能，逐渐被人们接受使用。但渐渐人工高分子的缺点开始出现，大多人工高分子都是容易燃烧的。自此人们将目光主要放在了有机高分子的阻燃方面。

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