含哒嗪酮结构生物基环氧树脂本征阻燃机制研究

doi:10.12422/j.issn.1006-396X.2023.01.001

摘要/Abstract

摘要：

通过树脂烧蚀实验和扫描电子显微镜、X射线光电子能谱仪、热重?红外同步热分析仪等表征手段探究了含哒嗪酮结构的生物基环氧树脂的本征阻燃机制。结果表明，相对于目前最常用的石油基双酚A型环氧树脂，所制备的生物基环氧树脂在燃烧时更易形成大量膨胀型的炭层结构，同时释放出大量CO₂和NH₃等不可燃性气体和更少的可燃性气体；含哒嗪酮结构的本征阻燃生物基环氧树脂呈现出凝聚相?气相协同阻燃机理。本研究为构筑高性能的本征阻燃环氧树脂提供了新的思路。

关键词: 生物基, 环氧树脂, 本征阻燃, 哒嗪酮结构, 高性能

Abstract:

The intrinsic flame retardant mechanism of bio?based epoxy resin containing pyridazinone structure was explored through resin ablation experiment, scanning electron microscope,X?ray photoelectron spectrometer,thermogravimetry?infrared simultaneous thermal analyzer,and other characterization methods.The results show that compared with the most commonly used petroleum?based bisphenol A epoxy resin, the resultant bio?based epoxy resin is more likely to form a large amount of intumescent carbon layer structure during combustion and release a large amount of non?combustible gases such as CO₂ and NH₃ with less combustible gases.The intrinsic flame retardant bio?based epoxy resin containing pyridazinone structure exhibits a condensed phase?gas phase synergistic flame retardant mechanism. This study provides new ideas for constructing high?performance intrinsic flame retardant epoxy resin.

Key words: Bio?based, Epoxy resin, Intrinsic flame retardant, Pyridazinone, High?performance

中图分类号:

TQ323.5

戚裕, 曹旗, 李佳惠, 蹇锡高, 翁志焕. 含哒嗪酮结构生物基环氧树脂本征阻燃机制研究[J]. 石油化工高等学校学报, 2023, 36(1): 1-7.

Yu Qi, Qi Cao, Jiahui Li, Xigao Jian, Zhihuan Weng. Intrinsic Flame Retardant Mechanism of Bio⁃Based Epoxy Resin Containing Pyridazinone Structure[J]. Journal of Petrochemical Universities, 2023, 36(1): 1-7.

图/表 7

图1 环氧树脂前驱体及固化剂的化学结构式

Fig.1 Chemical structures of epoxy precursors and curing agent

图2 环氧树脂烧蚀前后的形貌变化

Fig.2 Morphological changes of epoxy before and after calcination

图3 环氧树脂的内外层炭在不同放大倍数下的SEM照片

Fig.3 SEM images of the outer and inner layers of carbon in the epoxy with different magnification

图4 环氧树脂经UL?94测试后形成残炭的XPS谱图

Fig.4 XPS spectrum of char residues formed from eposy after UL?94 test

表1 环氧树脂残炭中各元素的质量分数

Table 1 The mass fraction of each element in the char residues of epoxy

元素	质量分数/%
元素	GSPZ⁃EP/DDM	DGEBA/DDM
C	78.93	88.18
N	8.71	3.80
O	12.36	8.02

图5 环氧树脂在整个热解过程中的气相3D红外谱图及最大热解速率处的FT?IR谱图（a） GSPZ?EP/DDM气相3D红外谱图（b） DGEBA/DDM气相3D红外谱图（c）最大热解速率处的FT?IR谱图

Fig.5 Meteorological 3D infrared spetrum of eposy during the whole degradation process and FT?IR spectrum of maximum pyrolysis rate

图6 环氧树脂体系的阻燃机理

Fig.6 The flame retardancy mechanism of eposy system

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