Preparation of Poly(phosphoric acid piperazine) and Its Application as an Effective Flame Retardant for Epoxy Resin

Miao-Jun Xu; Si-Yu Xia; Chuan Liu; Bin Li

doi:10.1007/s10118-018-2036-8

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Preparation of Poly(phosphoric acid piperazine) and Its Application as an Effective Flame Retardant for Epoxy Resin

Articles | Updated：2021-02-18

- Preparation of Poly(phosphoric acid piperazine) and Its Application as an Effective Flame Retardant for Epoxy Resin
- Chinese Journal of Polymer Science Vol. 36, Issue 5, Pages: 655-664(2018)
- Affiliations：
  
  Heilongjiang Key Laboratory of Molecular Design and Preparation of Flame Retarded Materials, College of Science, Northeast Forestry University, Harbin 150040, China
- Author bio：
  
  Bin Li, E-mail libinzh62@163.com
- Funds：
- DOI：10.1007/s10118-018-2036-8
  CLC：
- Received：03 August 2017，
  
  Accepted：06 September 2017，
  
  Online First：18 January 2018，
  
  Published：05 May 2018
- Accepted：
Scan QR Code
Miao-Jun Xu, Si-Yu Xia, Chuan Liu, et al. Preparation of Poly(phosphoric acid piperazine) and Its Application as an Effective Flame Retardant for Epoxy Resin[J]. Chinese Journal of Polymer Science, 2018, 36(5): 655-664.
DOI：

Miao-Jun Xu, Si-Yu Xia, Chuan Liu, et al. Preparation of Poly(phosphoric acid piperazine) and Its Application as an Effective Flame Retardant for Epoxy Resin[J]. Chinese Journal of Polymer Science, 2018, 36(5): 655-664. DOI： 10.1007/s10118-018-2036-8.

摘要

Abstract

A phosphorus-nitrogen containing flame retardant additive of poly(phosphoric acid piperazine)

defined as PPAP

was synthesized by the salt-forming reaction between anhydrous piperazine and phosphoric acid

and the dehydration polymerization under heating in nitrogen atmosphere. Its chemical structure was well characterized by Fourier transform infrared (FTIR) spectroscopy

C and

P solid-state nuclear magnetic resonance measurements. The synthesized PPAP and curing agent

-phenylenediamine were blended into epoxy resin (EP) to prepare flame retardant EP thermosets. The effects of PPAP on the fire retardancy and thermal degradation behavior of cured EP/PPAP composites were investigated by limiting oxygen index (LOI)

vertical burning (UL-94)

thermogravimetric analysis/infrared spectrometry (TG-IR) and cone calorimeter tests. The morphologies and chemical compositions of char residues for cured epoxy resin were investigated by scanning electron microscopy (SEM) and X-ray photoelectron spectroscopy (XPS)

respectively. The results demonstrated that the flame retardant EP thermosets successfully passed UL-94 Ⅴ-0 flammability rating and the LOI value was as high as 30.8% when incorporating 5wt% PPAP into the EP thermosets. The TGA results indicated that the synthesized PPAP flame retardant additive possessed high thermal stability and excellent charring capability. Meanwhile

the incorporation of PPAP stimulated the epoxy resin matrix to decompose and charring ahead of time due to its catalytic decomposition effect

which led to a higher char yield at high temperature. The morphological structures and the analysis results of XPS for char residues of EP thermosets revealed that the introduction of PPAP benefited the formation of a sufficient

more compact and homogeneous char layer containing phosphorus-nitrogen flame retardant elements on the material surface during combustion. The formed char layer with high quality effectively prevented the heat transmission and diffusion

limited the production of combustible gases

and inhibited the emission of smoke

leading to the reduction of heat and smoke release.

关键词

Keywords

references

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