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《工程塑料应用》 2021年第08期
DOI:10.3969/j.issn.1001-3539.2021.08.007
含膦固化剂的制备及其阻燃环氧树脂的性能
冯才敏1,姜佳丽1,农彦彦1,练翠霞1,黄健光1,黄志鑫1,刘云香1,谢荣华2,李景汉3
1.顺德职业技术学院轻化与材料学院,广东佛山 528333; 2.东莞弘科新材料科技有限公司,广东东莞 523000; 3.广东金科新材料有限公司,广州 510000 
Preparation of Curing Agent Containing Phosphine and Properties of It Flame Retardant Epoxy Resin
Feng Caimin1, Jiang Jiali1, Nong Yanyan1, Lian Cuixia1, Huang Jianguang1, Huang Zhixin1, Liu Yunxiang1, Xie Ronghua2, Li Jinghan3
1. College of Light Chemical Industry and Materials Engineering, Shunde Polytechnic, Foshan 528333, China; 2. Dongguan Hongke New Material Technology Co., Ltd., Dongguan 523000, China; 3. Guangdong Jinke New Materials Co., Ltd., Guangzhou 510000, China 
摘要:选用乙基膦酰二氯和乙二胺制备了乙基含膦二胺固化剂(EDE),采用傅立叶变换红外光谱(FTIR)表征了EDE的结构,并跟踪了9,10-二氢-9-氧杂-10-磷杂菲-10氧化物(DOPO)改性环氧树脂(DOPO-EP)与EDE的固化反应过程,制备了EDE固化的DOPO改性环氧树脂(EDE-DOPO-EP)。分析比较了纯环氧树脂、DOPO-EP和EDE-DOPO-EP固化物的阻燃性能、透明性、力学性能和热稳定性能,采用FTIR和扫描电子显微镜(SEM)对残炭的结构和形貌进行分析。结果表明,在80℃固化2 h可以完成EDE-DOPO-EP的固化;当EDE的用量为23.04份(磷质量分数为3.07%)时,EDE-DOPO-EP极限氧指数达到30.5%,垂直燃烧阻燃等级达到UL 94 V-0级;EDE-DOPO-EP具有良好的透明性,在波长200~800 nm内保持了纯环氧树脂固化物透光率的80%~90%;与纯环氧树脂固化物相比,EDE-DOPO-EP的力学性能下降幅度相对较小,初始分解温度虽下降明显,但600℃和800℃的残炭率分别从2.1%和0.9%提高到23.4%和12.0%;FTIR和SEM对残炭的分析表明,EDE-DOPO-EP残炭中形成了更多的P—O—C和P=O的结构,形成了更致密的炭层,从而提高了阻燃性能。 
Abstract:The ethyl diamine curing agent containing phosphine (EDE) was prepared by ethylphosphonous dichloride and ethylenediamine, and the structure of EDE was characterized by Fourier transform infrared spectroscopy (FTIR), the reaction routine of EDE and 9, 10-Dihydro-9-oxa-10-phosphaphenanthrene-10-oxide (DOPO) modified epoxy resin (DOPO-EP) was tracked by FTIR. The DOPO-EP cured by EDE (EDE-DOPO-EP) was prepared. The flame retardant properties, transparency, mechanical properties and thermal stability of cured pure epoxy resin, DOPO-EP and EDE-DOPO-EP were characterized. The molecular structure and morphology of residual char were analyzed by FTIR and scanning electron microscopy (SEM). It is found that it cured completely after heated at 80℃ for 2 hours for EDE-DOPO-EP. The limit oxygen index value of EDE-DOPO-EP is 30.5%, and the flame retardant grade of vertical combustion reaches UL 94 V-0, when the content of EDE is 23.04 phr (mass fraction of P is 3.07%). EDE-DOPO-EP has good transparence and it can keep 80%-90% of the transmittance of cured pure epoxy resin at the wavelength of 200-800 nm. Compared with cured pure epoxy resin, the decrease of the mechanical properties of EDE-DOPO-EP are relatively little, the initial degradation temperature decreases obviously but the carbon residue rate at 600℃ and 800℃ increase from 2.1% and 0.9% to 23.4% and 12.0% respectively. The analysis of residual char characterized by FTIR and SEM illustrates that more P—O—C and P=O bonds during combustion are formed in the residual char of EDE-DOPO-EP, and more compact char layer is formed to improve the flame retardant properties. 
关键词:环氧树脂;9,10-二氢-9-氧杂-10-磷杂菲-10氧化物;含膦固化剂;本征阻燃;阻燃机理 
Keywords:epoxy resin; 9,10-Dihydro-9-oxa-10-phosphaphenanthrene-10-oxide; curing agent containing phosphine; intrinsic flame retardant; flame retardant mechanism 
基金:广东省自然科学基金项目(2021A1515012274),2021年攀登计划(pdjh2021) 
本文引用格式:
冯才敏,姜佳丽,农彦彦,等.含膦固化剂的制备及其阻燃环氧树脂的性能[J].工程塑料应用,2021,49(8):37-42.
Feng Caimin,Jiang Jiali,Nong Yanyan,et al. Preparation of curing agent containing phosphine and properties of it flame retardant epoxy resin[J]. Engineering Plastics Application,2021,49(8):37-42. 

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