论文总字数：19640字

摘 要

随着半导体制造业和微电子技术的快速进步，环氧树脂因其具有较好的电绝缘的功能和可以很大程度地耐酸碱腐蚀而被大量用来包装一些与电子有关的产品。针对环氧模塑料贮存需冷藏的特点，本实验对其组成成分中的固化促进剂咪唑进行改性，在不影响其力学性能的前提下，利用α，β-不饱和二酯与咪唑环中的仲胺反应，在室温下使咪唑变得不再活泼，实现能提高环氧树脂固化体系的室温贮存性的目的。反应得到的产物可以通过复合迈克尔加成反应热分解成咪唑和不饱和二酯，咪唑的迅速参与环氧树脂的固化，得到固化产物。

本次实验的主要工作：用富马酸二乙酯与2-苯基咪唑反应制得产物改性咪唑（PZDF），验证高温下产物PZDF发生热分解，得到富马酸二乙酯与2-苯基咪唑，然后以邻甲酚醛环氧树脂为固化剂，环氧树脂为原料，按相同的配比分别与2-苯基咪唑和PZDF混合形成环氧固化体系。对PZDF进行红外光谱测试，核磁共振来表征分子结构，用差示扫描量热法（DSC）来验证PZDF的热分解反应，对环氧树脂固化体系进行力学性能测试以及DSC测试研究室温贮存性能，得到以下结论：

得到的产物在170℃下发生热分解反应，生成富马酸二乙酯和2-苯基咪唑。PZDF对环氧固化体系的力学性能没有影响，并延长了环氧固化体系在室温下的贮存期。

关键词：环氧模塑料 固化促进剂 2-苯基咪唑 力学性能 贮存期

The Preparation and Study of Latent Epoxy Curing Agent

Abstract

The epoxy molding compound(EMC)which is one of the IC three main package materials has become the mainstream for domestic and VLSI package.In view of the characteristics of storage of epoxy molding materials to be refrigerated,the curing accelerator imidazole in the composition of the epoxy resin is used to modify the curing agent imidazole.Under the premise of not affecting its mechanical properties,α,β-unsaturated diester is used in the imidazole ring to reduce the reactivity of the imidazole.The product can be decomposed into imidazole and unsaturated diester by complex Michael addition reaction,so that the activity of releasing the imidazole is involved in the curing of the epoxy resin to improve the storage time at room temperature.

The main work of this experiment: the reaction of diethyl fumarate with 2-phenylimidazole to produce the product PZDF, and then verify the high temperature of the product PZDF thermal decomposition, to be diethyl fumarate and 2-phenyl imidazole, The epoxy curing system was prepared by mixing o-cresol-formaldehyde epoxy resin as curing agent and epoxy resin as raw materials in the same ratio with 2-phenylimidazole and modified imidazole respectively. By infrared spectroscopy, nuclear magnetic resonance spectroscopy, DSC and mechanical properties of the test, the following conclusions:

The resulting product was subjected to a thermal decomposition reaction at 170 ° C to give diethyl fumarate and 2-phenylimidazole. PZDF has no effect on the mechanical properties of the epoxy curing system and extends the shelf life of the epoxy curing system at room temperature.

Key words: Epoxy molding compound; Curing accelerator; 2-phenylimidazole; mechanical properties; shelf life

目 录

摘要 I

Abstract II

第一章 绪论 1

1.1 环氧模塑料概述 1

1.1.1 背景 1

1.1.2 定义及组成 1

1.2 环氧树脂简介 2

1.2.1背景及发展状况 2

1.3环氧树脂固化剂简介 2

1.3.1普通固化剂 3

1.3.2潜伏性固化剂 3

1.4 环氧树脂固化促进剂简介 5

1.5咪唑作为固化剂、促进剂概述 5

1.5.1咪唑固化机理 5

1.5.2咪唑类固化剂促进剂的特征 5

1.6本文研究内容与意义 6

第二章 实验部分 7

2.1 实验原料 7

2.2 实验仪器设备 7

2.3 实验样品设备 8

2.3.1改性固化促进剂的制备 8

2.3.2改性固化促进剂的分离提纯 8

2.3.3测试样品的制备 9

2.4性能测试 10

2.4.1产物表征 10

2.4.2核磁测试 10

2.4.3DSC测试 10

2.4.4力学性能测试 11

第三章 实验结果与讨论 12

3.1产物表征 12

3.2产物分解反应的验证 13

3.3环氧固化体系力学性能测试 15

3.4环氧固化体系贮存性能测试 15

第四章 结论与展望 19

4.1结论 19

4.2展望 19

参考文献 20

致谢 22

第一章 绪论

1.1 环氧模塑料概述

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