Effects of Fluorenyl Polyphosphazene Microspheres on the Flame Retardant Properties of Polybenzoxazine Resins

Chun-xia Zhao; Ling Zhao; Xiao-jia He; Hao-lan Gou; Yun-tao Li

doi:10.11777/j.issn1000-3304.2018.18042

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Effects of Fluorenyl Polyphosphazene Microspheres on the Flame Retardant Properties of Polybenzoxazine Resins

Research Article | 更新时间：2021-01-26

- Effects of Fluorenyl Polyphosphazene Microspheres on the Flame Retardant Properties of Polybenzoxazine Resins
- Acta Polymerica Sinica Vol. 0, Issue 10, Pages: 1336-1344(2018)
- 作者机构：
  
  西南石油大学材料科学与工程学院　成都 610500
- 作者简介：
- 基金信息：
- DOI：10.11777/j.issn1000-3304.2018.18042
  CLC：
- Published：2018-10，
  
  Received：2 February 2018，
  
  Revised：29 March 2018，
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Chun-xia Zhao, Ling Zhao, Xiao-jia He, Hao-lan Gou, Yun-tao Li. Effects of Fluorenyl Polyphosphazene Microspheres on the Flame Retardant Properties of Polybenzoxazine Resins. [J]. Acta Polymerica Sinica 0(10):1336-1344(2018)
DOI：

Chun-xia Zhao, Ling Zhao, Xiao-jia He, Hao-lan Gou, Yun-tao Li. Effects of Fluorenyl Polyphosphazene Microspheres on the Flame Retardant Properties of Polybenzoxazine Resins. [J]. Acta Polymerica Sinica 0(10):1336-1344(2018) DOI： 10.11777/j.issn1000-3304.2018.18042.

摘要

以六氯环三磷腈(HCCP)和4

4′-(9-芴)二苯酚为原料，通过超声辅助沉淀聚合制备芴基聚磷腈(PZFP)微球，并将其用于双酚A型苯并噁嗪树脂(PBa)的阻燃改性. 热重分析仪(TGA)、锥型量热仪(CONE)和动态热机械分析仪(DMA)测试结果表明，PZFP可提高PBa热降解后残留量，并能显著降低热释放速率(HRR)，延长点燃时间(TTI)，提高火灾性能指数(FPI)，起到良好的阻燃作用. 其中，PBa/PZFP-10%具有最佳阻燃性能. 与纯PBa相比，PBa/PZFP-10%的HRR值由566 kW/m

降低到214 kW/m

，玻璃化转变温度(

)和储能模量略有提高. 纯PBa和PBa/PZFP-10%的

分别为222 和226 °C. PBa/PZFP-10%复合材料的CONE测试后炭层扫描电镜(SEM)和热重-红外联用(TG-FTIR)结果显示，PZFP在PBa燃烧过程中，可以促进PBa主链和侧基交联成炭，形成外表面致密和内部多孔结构的凝聚相；PZFP本身热解产物部分参与凝聚相形成过程，仍有少量逸到气相中阻碍或终止气相燃烧循环. PZFP在PBa基体中起到凝聚相和气相阻燃机理协同作用.

Abstract

Fluorenyl polyphosphazene (PZFP) microspheres were facilely prepared through a one-step precipitation copolymerization of hexachlorocyclotriphosphazene (HCCP) and 4

4′-(9-fluorenylidene)diphenol under ultrasonic. PZFP microspheres were incorporated into polybenzoxazine resins to improve the flame properties of the polymers. The results of thermogravimetric analysis (TGA)

cone calorimeter (CONE) and dynamic thermal mechanical analysis (DMA) showed that incorporation of PZFP microspheres enhanced the char residues amount of PBa during thermal degradation process

reduced the heat release rate (HRR)

delayed the time to ignition (TTI) and increased the fire performance index (FPI) of PBa in fire. Interestingly

PBa/PZFP-10% showed the relatively best flame retardant properties among a series of PBa/PZFP composites with different PZFP contents. In comparison to pure PBa

the HRR value in the composite PBa/PZFP-10% was reduced to 214 kW·m

−2

from 566 kW·m

−2

for pure PBa

and FPI value was enhanced to 0.243 from 0.087. The glass transition temperature (

) and storage modules of PBa/PZFP-10% were increased slightly

with the introduction of 10% PZFP microspheres. The

of PBa and PBa/PZFP-10% was 222 and 226 °C

respectively. It is believed that PZFP microspheres offered PBa resins good flame retardant properties

without affecting the application temperature of PBa. The char residue analysis using scanning electron microscopy (SEM) suggested the formation of high-quality char layer with compact outer surfaces and polyphorous inner structure. The volatile products formed in the thermal degradation process of PBa and PBa/PZFP composites were detected by a TGA-Fourier transform infrared spectrometer (TGA-FTIR). The improved flame retardancy of PBa/PZFP composites was mainly attributed to a combination of the greatly increased melt viscosity of PBa and matrix fast swelling due to the pyrolytic gases. Additionally

PZFP microspheres was found to greatly reduce the amount of pyrolytic gases containing N―H and ―C＝C＝C― groups. Instead

it released phosphorous-containing species to achieve flame retardancy in the gas phase. PZFP microspheres contributed a synergistic condensed phase and gas phase flame retardant mechanism for PBa resins.

关键词

芴基聚磷腈微球阻燃苯并噁嗪树脂锥型量热分析

Keywords

Fluorenyl polyphosphazene microspheresFlame retardancyPolybenzoxazine resinsCone calorimeter

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Related Institution

The Collaborative Innovation Center for Eco-Friendly and Fire-Safety Polymeric Materials (MOE), National Engineering Laboratory of Eco-Friendly Polymeric Materials (Sichuan), State Key Laboratory of Polymer Materials Engineering, College of Chemistry, Sichuan University

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