Influence of a novel P/N-containing oligomer on flame retardancy and thermal degradation of intumescent flame-retardant epoxy resin

In this work, a novel P/N-containing oligomer poly(piperazine phenylphosphamide) (BPOPA) was synthesized via the polymerization reaction of phenylphosphonic dichloride with piperazine. Its structure was characterized by Fourier transformation infrared spectroscopy (FT-IR), nuclear magnetic resonance...

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Published inPolymer degradation and stability Vol. 162; pp. 129 - 137
Main Authors Zhu, Zong-Min, Wang, Luo-Xin, Dong, Liang-Ping
Format Journal Article
LanguageEnglish
Published London Elsevier Ltd 01.04.2019
Elsevier BV
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Abstract In this work, a novel P/N-containing oligomer poly(piperazine phenylphosphamide) (BPOPA) was synthesized via the polymerization reaction of phenylphosphonic dichloride with piperazine. Its structure was characterized by Fourier transformation infrared spectroscopy (FT-IR), nuclear magnetic resonance (NMR), elemental analysis (EA) and gel permeation chromatography (GPC). It was used to enhance the flame retardancy of epoxy resin/ammonium polyphosphate (APP). As expected, improvement in flame retardancy of EP/APP was observed. In detail, EP containing 10 wt% APP alone possessed a LOI value of 30.2% but UL-94 no rating. When both 7.5 wt% APP and 2.5 wt% BPOPA were added into EP, EP/7.5APP/2.5BPOPA passed a UL-94 V-0 rating with a LOI value of 33.1%. Moreover, EP/7.5APP/2.5BPOPA presented much lower values of the peak of heat release rate (PHRR) and total smoke production (TSP) compared with EP/10APP. The flame-retardant mechanism was analyzed by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and thermogravimetric analysis/infrared spectrometry (TG-IR). Results illustrated that EP/7.5APP/2.5BPOPA mainly functioned in condensed phase which was associated with the formation of more compact char layer. •A novel P/N-containing oligomer (BPOPA) was synthesized and characterized successfully.•Adding BPOPA significantly improved flame retardancy of EP/APP.•Incorporation of BPOPA improved compactness degree of char for EP/APP during combustion.
AbstractList In this work, a novel P/N-containing oligomer poly(piperazine phenylphosphamide) (BPOPA) was synthesized via the polymerization reaction of phenylphosphonic dichloride with piperazine. Its structure was characterized by Fourier transformation infrared spectroscopy (FT-IR), nuclear magnetic resonance (NMR), elemental analysis (EA) and gel permeation chromatography (GPC). It was used to enhance the flame retardancy of epoxy resin/ammonium polyphosphate (APP). As expected, improvement in flame retardancy of EP/APP was observed. In detail, EP containing 10 wt% APP alone possessed a LOI value of 30.2% but UL-94 no rating. When both 7.5 wt% APP and 2.5 wt% BPOPA were added into EP, EP/7.5APP/2.5BPOPA passed a UL-94 V-0 rating with a LOI value of 33.1%. Moreover, EP/7.5APP/2.5BPOPA presented much lower values of the peak of heat release rate (PHRR) and total smoke production (TSP) compared with EP/10APP. The flame-retardant mechanism was analyzed by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and thermogravimetric analysis/infrared spectrometry (TG-IR). Results illustrated that EP/7.5APP/2.5BPOPA mainly functioned in condensed phase which was associated with the formation of more compact char layer.
In this work, a novel P/N-containing oligomer poly(piperazine phenylphosphamide) (BPOPA) was synthesized via the polymerization reaction of phenylphosphonic dichloride with piperazine. Its structure was characterized by Fourier transformation infrared spectroscopy (FT-IR), nuclear magnetic resonance (NMR), elemental analysis (EA) and gel permeation chromatography (GPC). It was used to enhance the flame retardancy of epoxy resin/ammonium polyphosphate (APP). As expected, improvement in flame retardancy of EP/APP was observed. In detail, EP containing 10 wt% APP alone possessed a LOI value of 30.2% but UL-94 no rating. When both 7.5 wt% APP and 2.5 wt% BPOPA were added into EP, EP/7.5APP/2.5BPOPA passed a UL-94 V-0 rating with a LOI value of 33.1%. Moreover, EP/7.5APP/2.5BPOPA presented much lower values of the peak of heat release rate (PHRR) and total smoke production (TSP) compared with EP/10APP. The flame-retardant mechanism was analyzed by scanning electron microscopy (SEM), X-ray photoelectron spectroscopy (XPS) and thermogravimetric analysis/infrared spectrometry (TG-IR). Results illustrated that EP/7.5APP/2.5BPOPA mainly functioned in condensed phase which was associated with the formation of more compact char layer. •A novel P/N-containing oligomer (BPOPA) was synthesized and characterized successfully.•Adding BPOPA significantly improved flame retardancy of EP/APP.•Incorporation of BPOPA improved compactness degree of char for EP/APP during combustion.
Author Zhu, Zong-Min
Wang, Luo-Xin
Dong, Liang-Ping
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  surname: Zhu
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– sequence: 2
  givenname: Luo-Xin
  surname: Wang
  fullname: Wang, Luo-Xin
  organization: State Key Laboratory of New Textile Materials and Advanced Processing Technology, College of Materials Science and Engineering, Wuhan Textile University, Wuhan, 430200, Hubei, PR China
– sequence: 3
  givenname: Liang-Ping
  surname: Dong
  fullname: Dong, Liang-Ping
  email: dlpscu@163.com
  organization: Institute of Electronic Engineering, China Academy of Engineering Physics, Mianyang, 621000, Sichuan, PR China
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Keywords Epoxy resin
Flame retardancy
Flame-retardant mechanism
P/N-containing oligomer
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Snippet In this work, a novel P/N-containing oligomer poly(piperazine phenylphosphamide) (BPOPA) was synthesized via the polymerization reaction of phenylphosphonic...
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SubjectTerms ammonium polyphosphates
Chemical analysis
Dichlorides
epoxides
Epoxy resin
Epoxy resins
Flame retardancy
Flame retardants
Flame-retardant mechanism
Fourier transform infrared spectroscopy
Fourier transforms
gel chromatography
heat
Heat release rate
Infrared analysis
Infrared spectroscopy
Liquid chromatography
NMR
Nuclear magnetic resonance
nuclear magnetic resonance spectroscopy
P/N-containing oligomer
Photoelectrons
piperazine
polymerization
Scanning electron microscopy
Smoke
Thermal degradation
Thermogravimetric analysis
thermogravimetry
X ray photoelectron spectroscopy
Title Influence of a novel P/N-containing oligomer on flame retardancy and thermal degradation of intumescent flame-retardant epoxy resin
URI https://dx.doi.org/10.1016/j.polymdegradstab.2019.02.021
https://www.proquest.com/docview/2222922028
https://www.proquest.com/docview/2221022653
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