改性β-CD的制备及其阻燃环氧树脂研究

doi:10.16265/j.cnki.issn1003-3033.2020.07.016

中国安全科学学报 ›› 2020, Vol. 30 ›› Issue (7): 107-113.doi: 10.16265/j.cnki.issn1003-3033.2020.07.016

改性β-CD的制备及其阻燃环氧树脂研究

韩骥¹, 单雪影^**1 讲师, 邵辉¹ 教授, 郭辉¹, 李锦春² 教授

1 常州大学环境与安全工程学院,江苏常州 213164;
2 常州大学材料科学与工程学院,江苏常州 213164

收稿日期:2020-04-27 修回日期:2020-06-13 出版日期:2020-07-28 发布日期:2021-07-15
通讯作者: ** 单雪影(1986—),女,安徽宿州人,博士,讲师,主要从事聚合物的火灾安全方面的研究。E-mail: xyshan@cczu.edu.cn。
作者简介:韩骥 (1994—),男,江苏淮安人,硕士研究生,主要研究方向为阻燃材料制备及在环氧树脂中的应用。E-mail:15189730617@163.com。
基金资助:
中国科学技术大学火灾科学国家重点实验室开放课题(HZ2018-KF02);常州市科技项目(CJ20190047);江苏省研究生培养创新工程项目(KYCX19_1790)。

Preparation of modified β-CD and flame retardancy of EP

HAN Ji¹, SHAN Xueying¹, SHAO Hui¹, GUO Hui¹, LI Jinchun²

1 School of Environmental and Safety Engineering, Changzhou University, Changzhou Jiangsu 213164, China;
2 School of Materials Science and Engineering, Changzhou University, Changzhou Jiangsu 213164, China

Received:2020-04-27 Revised:2020-06-13 Online:2020-07-28 Published:2021-07-15

摘要/Abstract

摘要： 为了制备单分子阻燃剂,以提高环氧树脂(EP)的阻燃性能,首先使用季戊四醇(PER)与三氯氧磷(POCl₃)反应得到磷酸酯二酰氯(SPDPC),然后用不同量的SPDPC改性β-环糊精(β-CD);将制备的改性环糊精(mβ-CD)应用于EP(添加量为EP质量的25%)中,制备EP/mβ-CD复合材料。结果表明:β-CD与SPDPC的摩尔比例为1∶8时制备的mβ-CD与EP基体相容性较好,此mβ-CD使EP材料在N₂氛围的炭渣量从15.3%提高到26.7%;EP氧指数从19.5%提高到28.2%;复合材料的垂直燃烧等级达到V-0级别,热释放总量(THR)、热释放速率峰值(PHRR)相较于纯EP分别降低了50.4%、47.9%,烟生成速率峰值(PSPR)和总生烟量(TSP)相较于纯EP分别降低了12.5%、52.8%;添加此mβ-CD的EP/mβ-CD复合材料形成了强度更高的炭层。

关键词: β-环糊精(β-CD), 环氧树脂(EP), 热降解, 阻燃性能, 炭渣量

Abstract: In order to develop single molecule flame retardant to improve flame retardancy of EP, phosphate diacid chloride (SPDPC) was prepared by using pentaerythritol (PER) and phosphorus oxychloride (POCl₃). Then different amounts of SPDPC was applied to modify β-CD. Finally, EP/mβ-CD composite was made by adding modified β-CD (mβ-CD) into EP (amount of addition was 25% based on EP quality). The results show that the mβ-CD prepared with 1∶8 molar ratio of β-CD to SPDPC has good compatibility in EP matrix, and it increases amount of char residue of EP in nitrogen atmosphere to 26.7% from 15.3%. EP oxygen index also rises from 19.5% to 28.2%. Vertical combustion of EP/mβ-CD composite reaches V-0 level, and its total heat release (THR) and peak of heat release rate (PHRR) are reduced by 50.4% and 47.9% respectively comparing to pure EP while peak of smoke production rate (PSPR) and total smoke production (TSP) reduced by 12.5% and 52.8%. Moreover, such composite with above mβ-CD could form a stronger char layer.

Key words: β-cyclodextrin(β-CD), epoxy resin(EP), thermal degradation, flame retardancy, amount of char residue

中图分类号:

X937

韩骥, 单雪影, 邵辉, 郭辉, 李锦春. 改性β-CD的制备及其阻燃环氧树脂研究[J]. 中国安全科学学报, 2020, 30(7): 107-113.

HAN Ji, SHAN Xueying, SHAO Hui, GUO Hui, LI Jinchun. Preparation of modified β-CD and flame retardancy of EP[J]. China Safety Science Journal, 2020, 30(7): 107-113.

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改性β-CD的制备及其阻燃环氧树脂研究

Preparation of modified β-CD and flame retardancy of EP

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