| Literature DB >> 31795522 |
Zhongying Yao1,2, Xinxin Liu3, Lijun Qian1,2, Yajun Chen1,2, Bo Xu1,2, Yong Qiu1,2.
Abstract
A flame retardant aluminum 2-carboxyethyl-phenyl-phosphinate (CPA-Al) was synthesized through the salification reaction. The molecular structure of CPA-Al and thermal stability were characterized by solid nuclear magnetic resonance, Fourier transform infrared spectroscopy, and thermogravimetric analysis. Subsequently, CPA-Al mixed in polyurethane was coated on polyester textile to obtain flame-retardant samples. The addition of 14.7 wt.% CPA-Al in textile sample can bring a limited oxygen index (LOI) value of 24.5%, 0 s after flame time, and the vertical burning B1 rating. Meanwhile, the incorporated CPA-Al reduced the peak heat release rate, total heat release, average effective heat of combustion, and increased the charring capacity of polyester textiles in contrast to the samples without CPA-Al. CPA-Al exerted not only its flame inhibition effect in gas phase, but also the charring and barrier effect in the condensed phase. Besides, with an increasing CPA-Al ratio in polyester textile, the contact angle gradually decreased from 123.6° to 75.6°, indicating that the surficial property of coating from hydrophobic to hydrophilic, thereby increasing the moisture permeability of polyester textile.Entities:
Keywords: coating; flame retardant; phosphinate; polyester textile
Year: 2019 PMID: 31795522 PMCID: PMC6960942 DOI: 10.3390/polym11121969
Source DB: PubMed Journal: Polymers (Basel) ISSN: 2073-4360 Impact factor: 4.329
Scheme 1Synthesis route of 2-carboxyethyl-phenyl-phosphinate (CPA-Al).
Formulas of the different textile samples.
| Samples | Polyester Textile (g) | PU (g) | CPA-Al | |
|---|---|---|---|---|
| g | wt % | |||
| PU/T | 139 | 18 | 0 | 0 |
| 7.1%CPA-Al/PU/T | 139 | 18 | 12 | 7.1 |
| 10.3%CPA-Al/PU/T | 139 | 18 | 18 | 10.3 |
| 14.7%CPA-Al/PU/T | 139 | 18 | 27 | 14.7 |
Figure 1Solid-state NMR spectra of CPA-Al. (a) 1H NMR; (b) 13C NMR; (c) 31P NMR; and (d) 27Al NMR of CPA-Al.
Figure 2The chemical structure of CPA-Al main by-product.
Figure 3FTTR spectra of CPA-Al and 3-Hydroxyphenylphosphinyl-propanoic acid (CPA).
Figure 4TGA curves of CPA-Al and CPA.
Thermogravimetric analysis (TGA) parameters of CPA-Al and CPA.
| Samples | Td,1% (°C) | Td,5% (°C) | Residuals at 600 °C (wt %) | Residuals at 700 °C (wt %) |
|---|---|---|---|---|
| CPA | 214 | 248 | 0 | -- |
| CPA-Al | 300 | 324 | 40.1 | 30.1 |
Limited oxygen index (LOI) value and vertical burning test of textile samples.
| Samples | LOI (%) | Vertical Burning Test | |||
|---|---|---|---|---|---|
| After Flame Time (s) | The Length of Combustion/cm | Dripping | Rating | ||
| PU/T | 20.0 | 32.5 | 30.0 | Yes | NR |
| 7.1%CPA-Al/PU/T | 23.6 | 30.0 | 16.2 | Yes | NR |
| 10.3%CPA-Al/PU/T | 23.8 | 8.8 | 9.8 | Yes | B2 |
| 14.7%CPA-Al/PU/T | 24.5 | 0 | 7.4 | No | B1 |
Figure 5Digital photos of 14.7%CPA-Al/PU/T during combustion of vertical burning test. (a) 5 s; (b) 10 s; (c) 15 s; and (d) Partial digital photo.
Figure 6Heat release rate (HRR) curves of CPA-Al polyester textiles.
Figure 7Mass loss rate (MLR) curves of CPA-Al polyester textiles.
Cone calorimeter data of CPA-Al polyester samples.
| Samples | PHRR (kW/m2) | av-EHC (MJ/m2) | THR (MJ/m2) | TSR (m2/m2) | av-COY (kg/kg) | av-CO2Y (kg/kg) | Residue (wt %) |
|---|---|---|---|---|---|---|---|
| 7.1%CPA-Al/PU/T | 375 | 22.6 | 29.8 | 1323 | 0.11 | 2.48 | 11.2 |
| 10.3%CPA-Al/PU/T | 342 | 19.4 | 26.6 | 1395 | 0.15 | 2.69 | 18.9 |
| 14.7%CPA-Al/PU/T | 267 | 16.8 | 25.2 | 1438 | 0.14 | 2.20 | 24.0 |
| PU/T | 930 | 25.5 | 38.2 | 989 | 0.07 | 2.80 | 11.9 |
Figure 8TGA curves of polyester textiles.
TGA parameters of polyester textiles.
| Samples | Td, 1% (°C) | Td, 5% (°C) | Residuals at 600 °C (wt %) |
|---|---|---|---|
| PU/T | 286 | 375 | 9.2 |
| 7.1%CPA-Al/PU/T | 315 | 388 | 17.2 |
| 10.3%CPA-Al/PU/T | 321 | 388 | 17.5 |
| 14.7%CPA-Al/PU/T | 317 | 384 | 19.0 |
Figure 9(a) Three-dimensional (3D) FTIR spectrum of the pyrolysis gas products of CPA-Al from TGA; (b) FTIR spectra of pyrolysis gas products of CPA-Al at the maximum gas release rate.
Figure 10Digital photos of polyester residues from cone calorimeter.
Figure 11SEM photos of 14.7%CPA-Al/PU/T residue from cone calorimeter. (a) 500×; (b) 3000×.
Element contents of residues from the cone calorimeter test.
| Samples | Element Content (wt %) | ||||
|---|---|---|---|---|---|
| C | N | O | Al | P | |
| 7.1%CPA-Al/PU/T | 77.64 | 2.07 | 15.98 | 1.74 | 2.57 |
| 10.3%CPA-Al/PU/T | 70.67 | 1.88 | 19.17 | 3.36 | 4.92 |
| 14.7%CPA-Al/PU/T | 69.55 | 3.01 | 19.34 | 2.81 | 5.29 |
| PU/T | 75.84 | 2.98 | 21.18 | -- | -- |
Water vapor permeation and contact angles of CPA-Al/PU/T.
| Samples | Water Vapor Permeation (g/m2·day) | Contact Angle (°) |
|---|---|---|
| PU/T | 690.3 | 123.6 |
| 7.1%CPA-Al/PU/T | 1091.2 | 99.8 |
| 10.3%CPA-Al/PU/T | 1280.4 | 92.5 |
| 14.7%CPA-Al/PU/T | 1648.6 | 75.6 |
Figure 12Digital images of the contact angle experiment. (a) PU/T; (b) 7.1%CPA-Al/PU/T; (c) 10.3%CPA-Al/PU/T; and, (d) 14.7%CPA-Al/PU/T.