纳米TiO2溶胶对环氧树脂固化反应的影响毕业论文

 2021-04-08 09:04

摘 要

环氧树脂的应用非常广泛,在我国具有广阔的市场前景,根据不同的需要,经改性后的环氧树脂可用作胶粘剂、涂料、固化剂、土建材料等。

论文主要研究了纳米TiO2对环氧树脂固化的影响,通过制备不同粒径,以及向环氧树脂预聚物中添加不同比例的纳米TiO2颗粒,研究纳米TiO2的粒径和添加量对环氧树脂固化的影响。对纳米TiO2改性环氧树脂预聚物进行DSC测试,观察其在固化时的放热情况,并测试固化完成后环氧树脂的Tg。测试环氧树脂在最佳固化温度下的胶凝化时间,观察纳米TiO2粒径及添加量对环氧树脂预聚物胶凝化速度的影响。对环氧树脂以及加入纳米TiO2改性的环氧树脂预聚物进行红外光谱测试。

研究结果表明:纳米TiO2的粒径及添加量均对环氧树脂的固化产生了影响,其趋势是随着纳米TiO2粒径的减小以及添加量的增多,固化放热峰的峰始温度和峰顶温度降低,尤其以峰始温度降低最为显著,可见在低温区域纳米TiO2对环氧树脂固化反应的促进作用更强;此外,经纳米TiO2改性的环氧树脂的Tg降低,其中添加量对改性环氧树脂Tg的影响更为明显,纳米TiO2添加量为1.5wt%的改性环氧树脂的Tg较未改性环氧树脂低14.45℃;纳米TiO2将会延长环氧树脂的胶凝化时间,添加量为1wt%的粒径为8.91nm的纳米TiO2的改性环氧树脂的胶凝化时间是未经改性的环氧树脂的1.34倍。

本文的特色:当前多数研究纳米TiO2改性环氧树脂的文章,多采用粉体纳米TiO2,相较于通过溶胶-凝胶法制备得到的纳米TiO2,粉体纳米TiO2的添加比例较高、分散不易且长时间存放后易产生团聚。溶胶-凝胶法制备的纳米TiO2则有粒径可控、分散性较好,表面能高,制备完成后可存储一段时间再使用,且具有微量高效的特点。

关键词:纳米TiO2;环氧树脂;固化;

Abstract

The application of epoxy resin is very extensive, and it has broad market prospects in China. According to different needs, the modified epoxy resin can be used as adhesive, coating, curing agent and civil construction material.

The paper mainly studied the effect of nano-TiO2 on the curing of epoxy resin. By preparing different particle sizes and adding different proportions of nano-TiO2 particles to the epoxy resin prepolymer, the particle size and the amount of nano-TiO2 were studied. The effect of curing. The nano-TiO2 modified epoxy resin prepolymer was subjected to DSC test, and the exothermic state during curing was observed, and the Tg of the epoxy resin after curing was tested. The gelation time of the epoxy resin at the optimum curing temperature was tested. The effect of the particle size and the amount of nano-TiO2 on the gelation rate of the epoxy resin prepolymer was observed. Infrared spectroscopy was performed on epoxy resin and nano-TiO2 modified epoxy resin prepolymer.

The results show that the particle size and the addition amount of nano-TiO2 have an effect on the curing of epoxy resin. The trend is that as the particle size of nano-TiO2 decreases and the amount of addition increases, the peak temperature of the exothermic peak of curing increases. The peak temperature decreased, especially the peak temperature decreased most obviously. It can be seen that the nano-TiO2 promoted the curing reaction of epoxy resin in the low temperature region. In addition, the Tg of the epoxy resin modified by nano-TiO2 decreased, and the addition amount thereof The effect of modified epoxy resin Tg is more obvious. The Tg of modified epoxy resin with 1.5wt% nano-TiO2 added is 14.45°C lower than that of unmodified epoxy resin; nano-TiO2 will extend the adhesive of epoxy resin. The gelation time of the modified epoxy resin of nano-TiO2 having a particle diameter of 8.91 nm added in an amount of 1 wt% was 1.34 times that of the unmodified epoxy resin.

The characteristics of this paper: Most of the current research on nano-TiO2 modified epoxy resin, powder nano-TiO2, compared with nano-TiO2 prepared by sol-gel method, the addition ratio of powder nano-TiO2 is higher and dispersed. It is not easy to produce agglomeration after long-term storage. The nano-TiO2 prepared by the sol-gel method has the advantages of controllable particle size, good dispersibility and high surface energy. It can be stored for a period of time after preparation, and has the characteristics of micro-efficiency.

Key Words:nano -TiO2; epoxy resin; curing;

目 录

摘 要 I

Abstract II

第1章 绪论 1

1.1 研究背景 1

1.2 环氧树脂简介 1

1.2.1 环氧树脂的种类 1

1.2.2 环氧树脂的固化 2

1.3 无机纳米颗粒简介 3

1.3.1 无机纳米颗粒的性质 3

1.3.2 无机纳米颗粒的制备 4

1.4 溶胶-凝胶法简介 5

1.4.1 溶胶-凝胶法的特点 5

1.4.2 溶胶-凝胶法在制备纳米TiO2方面的应用 5

1.5 本文研究目的及主要内容 6

第2章 实验过程及内容 8

2.1 引言 8

2.2 实验部分 8

2.2.1 实验仪器及试剂 8

2.2.2 实验过程 9

2.2.3 测试与表征 10

第3章 结果及分析 12

3.1 钛溶胶制备工艺对溶胶性能的影响 12

3.2 纳米TiO2添加量对环氧树脂固化的影响 13

3.2.1 纳米TiO2添加量对环氧树脂固化温度的影响 13

3.2.2 纳米TiO2添加量对环氧树脂Tg的影响 15

3.3 纳米TiO2粒度对环氧树脂固化的影响 16

3.3.1 纳米TiO2粒度对环氧树脂固化温度的影响 16

3.3.2 纳米TiO2粒度对环氧树脂Tg的影响 18

3.4 纳米TiO2对环氧树脂胶凝化时间的影响 20

3.4.1 纳米TiO2添加量对环氧树脂胶凝化时间的影响 20

3.4.2 纳米TiO2粒度对环氧树脂胶凝化时间的影响 21

3.5 红外光谱图的分析 21

第4章 结论 24

致 谢 25

参考文献 26

第1章 绪论

1.1 研究背景

环氧树脂与咪唑、酸酐、树脂类固化剂交联固化时,大都要加热固化,而纳米TiO2粒子因具有纳米效应,可降低环氧树脂的固化反应温度、延长凝胶化时间即降低固化反应速度。本课题采用溶胶-凝胶法制备纳米TiO2溶胶,研究纳米TiO2溶胶添加量对环氧树脂固化行为的影响。

摘 要

环氧树脂的应用非常广泛,在我国具有广阔的市场前景,根据不同的需要,经改性后的环氧树脂可用作胶粘剂、涂料、固化剂、土建材料等。

论文主要研究了纳米TiO2对环氧树脂固化的影响,通过制备不同粒径,以及向环氧树脂预聚物中添加不同比例的纳米TiO2颗粒,研究纳米TiO2的粒径和添加量对环氧树脂固化的影响。对纳米TiO2改性环氧树脂预聚物进行DSC测试,观察其在固化时的放热情况,并测试固化完成后环氧树脂的Tg。测试环氧树脂在最佳固化温度下的胶凝化时间,观察纳米TiO2粒径及添加量对环氧树脂预聚物胶凝化速度的影响。对环氧树脂以及加入纳米TiO2改性的环氧树脂预聚物进行红外光谱测试。

研究结果表明:纳米TiO2的粒径及添加量均对环氧树脂的固化产生了影响,其趋势是随着纳米TiO2粒径的减小以及添加量的增多,固化放热峰的峰始温度和峰顶温度降低,尤其以峰始温度降低最为显著,可见在低温区域纳米TiO2对环氧树脂固化反应的促进作用更强;此外,经纳米TiO2改性的环氧树脂的Tg降低,其中添加量对改性环氧树脂Tg的影响更为明显,纳米TiO2添加量为1.5wt%的改性环氧树脂的Tg较未改性环氧树脂低14.45℃;纳米TiO2将会延长环氧树脂的胶凝化时间,添加量为1wt%的粒径为8.91nm的纳米TiO2的改性环氧树脂的胶凝化时间是未经改性的环氧树脂的1.34倍。

本文的特色:当前多数研究纳米TiO2改性环氧树脂的文章,多采用粉体纳米TiO2,相较于通过溶胶-凝胶法制备得到的纳米TiO2,粉体纳米TiO2的添加比例较高、分散不易且长时间存放后易产生团聚。溶胶-凝胶法制备的纳米TiO2则有粒径可控、分散性较好,表面能高,制备完成后可存储一段时间再使用,且具有微量高效的特点。

关键词:纳米TiO2;环氧树脂;固化;

Abstract

The application of epoxy resin is very extensive, and it has broad market prospects in China. According to different needs, the modified epoxy resin can be used as adhesive, coating, curing agent and civil construction material.

The paper mainly studied the effect of nano-TiO2 on the curing of epoxy resin. By preparing different particle sizes and adding different proportions of nano-TiO2 particles to the epoxy resin prepolymer, the particle size and the amount of nano-TiO2 were studied. The effect of curing. The nano-TiO2 modified epoxy resin prepolymer was subjected to DSC test, and the exothermic state during curing was observed, and the Tg of the epoxy resin after curing was tested. The gelation time of the epoxy resin at the optimum curing temperature was tested. The effect of the particle size and the amount of nano-TiO2 on the gelation rate of the epoxy resin prepolymer was observed. Infrared spectroscopy was performed on epoxy resin and nano-TiO2 modified epoxy resin prepolymer.

The results show that the particle size and the addition amount of nano-TiO2 have an effect on the curing of epoxy resin. The trend is that as the particle size of nano-TiO2 decreases and the amount of addition increases, the peak temperature of the exothermic peak of curing increases. The peak temperature decreased, especially the peak temperature decreased most obviously. It can be seen that the nano-TiO2 promoted the curing reaction of epoxy resin in the low temperature region. In addition, the Tg of the epoxy resin modified by nano-TiO2 decreased, and the addition amount thereof The effect of modified epoxy resin Tg is more obvious. The Tg of modified epoxy resin with 1.5wt% nano-TiO2 added is 14.45°C lower than that of unmodified epoxy resin; nano-TiO2 will extend the adhesive of epoxy resin. The gelation time of the modified epoxy resin of nano-TiO2 having a particle diameter of 8.91 nm added in an amount of 1 wt% was 1.34 times that of the unmodified epoxy resin.

The characteristics of this paper: Most of the current research on nano-TiO2 modified epoxy resin, powder nano-TiO2, compared with nano-TiO2 prepared by sol-gel method, the addition ratio of powder nano-TiO2 is higher and dispersed. It is not easy to produce agglomeration after long-term storage. The nano-TiO2 prepared by the sol-gel method has the advantages of controllable particle size, good dispersibility and high surface energy. It can be stored for a period of time after preparation, and has the characteristics of micro-efficiency.

Key Words:nano -TiO2; epoxy resin; curing;

目 录

摘 要 I

Abstract II

第1章 绪论 1

1.1 研究背景 1

1.2 环氧树脂简介 1

1.2.1 环氧树脂的种类 1

1.2.2 环氧树脂的固化 2

1.3 无机纳米颗粒简介 3

1.3.1 无机纳米颗粒的性质 3

1.3.2 无机纳米颗粒的制备 4

1.4 溶胶-凝胶法简介 5

1.4.1 溶胶-凝胶法的特点 5

1.4.2 溶胶-凝胶法在制备纳米TiO2方面的应用 5

1.5 本文研究目的及主要内容 6

第2章 实验过程及内容 8

2.1 引言 8

2.2 实验部分 8

2.2.1 实验仪器及试剂 8

2.2.2 实验过程 9

2.2.3 测试与表征 10

第3章 结果及分析 12

3.1 钛溶胶制备工艺对溶胶性能的影响 12

3.2 纳米TiO2添加量对环氧树脂固化的影响 13

3.2.1 纳米TiO2添加量对环氧树脂固化温度的影响 13

3.2.2 纳米TiO2添加量对环氧树脂Tg的影响 15

3.3 纳米TiO2粒度对环氧树脂固化的影响 16

3.3.1 纳米TiO2粒度对环氧树脂固化温度的影响 16

3.3.2 纳米TiO2粒度对环氧树脂Tg的影响 18

3.4 纳米TiO2对环氧树脂胶凝化时间的影响 20

3.4.1 纳米TiO2添加量对环氧树脂胶凝化时间的影响 20

3.4.2 纳米TiO2粒度对环氧树脂胶凝化时间的影响 21

3.5 红外光谱图的分析 21

第4章 结论 24

致 谢 25

参考文献 26

第1章 绪论

1.1 研究背景

环氧树脂与咪唑、酸酐、树脂类固化剂交联固化时,大都要加热固化,而纳米TiO2粒子因具有纳米效应,可降低环氧树脂的固化反应温度、延长凝胶化时间即降低固化反应速度。本课题采用溶胶-凝胶法制备纳米TiO2溶胶,研究纳米TiO2溶胶添加量对环氧树脂固化行为的影响。

1.2 环氧树脂简介

环氧树脂由Prileschajew于1909年发现。环氧树脂定义为含有一种以上形式的环氧基团的低分子量预聚物。环氧树脂是热固性树脂,其通过固化反应使用各种固化剂固化。它们的性质取决于所用环氧树脂和固化剂类型的具体组合由于其优异的机械性能,对许多基材的高粘合性以及良好的耐热性和耐化学性,目前环氧树脂应用于广泛的领域,其中它们充当纤维增强材料,通用粘合剂,高性能涂料和包封材料[1]

1.2.1 环氧树脂的种类

1.2.1.1 双酚A环氧树脂

双酚-A的二缩水甘油醚(DGEBA)通过在碱性催化剂存在下使表氯醇与双酚-A反应制备的。周雪艳等[2]以以异佛尔酮二胺(IPDA)为固化剂,与具有不同分子量比的氢化双酚A型环氧树脂 (AL-3040) 、聚丙二醇二缩水甘油醚 (JH-230) 共混,制备出来一种具有形状记忆功能的新型环氧树脂。实验表明随着JH-230含量的增高,体系玻璃态模量及玻璃化转变温度降低,并且在回复温度一致的条件下(Tg,Tg 10℃,Tg 20℃),达到同一水平的形变回复率的形变回复时间变长。

1.2.1.2 脂环族环氧树脂

3',4'-环氧环己基甲基3,4-环氧环己烷羧酸酯通过使3'-环己烯基甲基3-环己烯羧酸酯与过乙酸反应来合成。该环氧树脂具有脂肪 族主链和完全饱和的分子结构,这有助于其优异的UV稳定性,良好的耐候性,良好的热稳定性和优异的电性能。这些性能对于用于制造需要在高温环境中应用的结构部件的树脂是至关重要的。

1.2.2 环氧树脂的固化

1.2.2.1环氧树脂的固化剂

环氧固化剂促进或控制环氧树脂的固化反应。通过添加固化剂来实现环氧树脂固化。在固化过程中发生环氧树脂的不可逆变化。环氧树脂的固化动力学和Tg取决于固化剂的分子结构[3]。根据化学组成,固化剂可分为胺类固化剂,碱固化剂,酸酐和催化固化剂。其中胺类固化剂的使用最为广泛,本次实验亦采用胺类固化剂,因此主要介绍胺类固化剂。

胺类固化剂是环氧树脂的基本固化剂之一,它们可分为三大类:脂族、芳族或脂环族胺。胺类固化剂通过亲核加成与环氧环反应。

1.2.2.2环氧树脂固化剂的特点

以胺类环氧树脂固化剂为例。

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