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一种新型含磷氮酚醛固化剂的制备及其对环氧树脂的固化与阻燃性能研究

Preparation of a Novel Phosphorus-Nitrogen Containing Novolac Curing Agent for Epoxy Resin and flame-retardancy of its cured epoxy resin.

作者信息

Qiao Hui, Liang Yun, Xu Guilong, Zhang Yanchong, Wang Yi, Hu Jian

机构信息

State Key Lab of Pulp & Paper Engineering, South China University of Technology, Guangzhou, PR China.

South China University of Technology, National Engineering Research Center of Papermaking and Pollution Control, Guangzhou, PR China.

出版信息

Des Monomers Polym. 2019 Oct 23;22(1):171-179. doi: 10.1080/15685551.2019.1678224. eCollection 2019.

DOI:10.1080/15685551.2019.1678224
PMID:31692991
原文链接:https://pmc.ncbi.nlm.nih.gov/articles/PMC6818113/
Abstract

In this study, DICY (dicyandiamide)-containing novolac (NN) was first prepared, and then DOPO (9,10-Dihydro-9-oxa-10-phosphaphenanthrene-10-oxide) was introduced to react with the unsaturated bonds from DICY to obtain a novel phosphorus-nitrogen-containing novolac resin (PNN), which was used as a curing agent for epoxy resins. The curing condition was confirmed by a non-isothermal curing kinetics study. The thermal stability and flame retardancy of the cured epoxy resin system were studied by thermogravimetric analysis (TGA), limited oxygen index (LOI) measurement, UL-94 test and cone calorimeter. The morphology of the burned chard residues was observed by Scanning electron microscopy (SEM). The results show that epoxy resin cured by the prepared PNN curing system presents excellent flame retardancy. The cured resin system, which contains only 1.31wt% phosphorus and 2.48wt% nitrogen, can achieve UL 94 V-0 rating.

摘要

在本研究中,首先制备了含双氰胺(DICY)的线型酚醛清漆(NN),然后引入9,10-二氢-9-氧杂-10-磷杂菲-10-氧化物(DOPO)与双氰胺中的不饱和键反应,得到一种新型含磷氮线型酚醛清漆树脂(PNN),并将其用作环氧树脂的固化剂。通过非等温固化动力学研究确定了固化条件。采用热重分析(TGA)、极限氧指数(LOI)测定、UL-94测试和锥形量热仪对固化环氧树脂体系的热稳定性和阻燃性进行了研究。通过扫描电子显微镜(SEM)观察了燃烧后炭渣的形态。结果表明,由制备的PNN固化体系固化的环氧树脂具有优异的阻燃性。该固化树脂体系仅含1.31wt%的磷和2.48wt%的氮,即可达到UL 94 V-0等级。

https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/3a9d0ca66157/TDMP_A_1678224_F0011_B.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/a7aa1f26050e/TDMP_A_1678224_F0001_B.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/710bf5d4e2b5/TDMP_A_1678224_F0002_OC.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/1b9e4c8c3e9c/TDMP_A_1678224_F0003_OC.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/7468757a5945/TDMP_A_1678224_F0004_OC.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/96fec04112d8/TDMP_A_1678224_F0005_OC.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/ad026b29a091/TDMP_A_1678224_F0006_OC.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/1b80853e07f6/TDMP_A_1678224_F0007_OC.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/d601f02d149f/TDMP_A_1678224_F0008_OC.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/8bd0584911db/TDMP_A_1678224_F0009_OC.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/01d7a6915932/TDMP_A_1678224_F0010_OC.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/3a9d0ca66157/TDMP_A_1678224_F0011_B.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/a7aa1f26050e/TDMP_A_1678224_F0001_B.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/710bf5d4e2b5/TDMP_A_1678224_F0002_OC.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/1b9e4c8c3e9c/TDMP_A_1678224_F0003_OC.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/7468757a5945/TDMP_A_1678224_F0004_OC.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/96fec04112d8/TDMP_A_1678224_F0005_OC.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/ad026b29a091/TDMP_A_1678224_F0006_OC.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/1b80853e07f6/TDMP_A_1678224_F0007_OC.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/d601f02d149f/TDMP_A_1678224_F0008_OC.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/8bd0584911db/TDMP_A_1678224_F0009_OC.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/01d7a6915932/TDMP_A_1678224_F0010_OC.jpg
https://cdn.ncbi.nlm.nih.gov/pmc/blobs/f09b/6818113/3a9d0ca66157/TDMP_A_1678224_F0011_B.jpg

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Brominated flame retardants and the formation of dioxins and furans in fires and combustion.溴化阻燃剂与火灾和燃烧中二恶英和呋喃的形成。
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